WorldWideScience

Sample records for simultaneous transdermal extraction

  1. In vitro transdermal delivery of caffeine, theobromine, theophylline and catechin from extract of Guarana, Paullinia Cupana.

    Science.gov (United States)

    Heard, Charles M; Johnson, Sarah; Moss, Gary; Thomas, Chris P

    2006-07-06

    Extracts of guarana (Paullinia cupana) feature as putatively stimulating ingredients in a number of foods, drinks and dietary/herbal supplements. The objective of this work was to investigate in vitro the transdermal delivery of the major pharmacologically active compounds contained in guarana extract. Saturated solutions of guarana were prepared in polyethylene glycol 400 (PEG400), propylene glycol (PG) and H(2)O at 32 degrees C. Guarana extract was also formulated in Duro-tak 2287 transdermal adhesive in a range of concentrations and the diffusional release was determined in addition to adhesive properties. Transdermal delivery across full thickness pig ear skin was investigated in vitro using Franz-type diffusion cells, with reverse-phase HPLC being used for the quantification of the permeation of theobromine (TB), theophylline (TP), (+)-catechin (C) and caffeine (CF). Based upon a combination of release and adhesive property data a patch containing 5.55 mg guarana extract cm(-2) was deemed optimal. The general trend for the delivery of the 4 analytes was: water >5.55 mg cm(-2) patch approximately PG>PEG400. For CF the greatest steady state flux was obtained from the water vehicle: 19 microg cm(-2)h(-1), with approximately 420 microg cm(-2) permeating after 24h. This was some 6x times more than from the drug-in-adhesive patch and 10x greater than PG, a well-known penetration enhancer, and 50x that of the 'regular' excipient PEG400. A water vehicle also provided the greatest delivery of TB (0.45 microg cm(-2) h(-1)), TP (0.022 microg cm(-2) h(-1)), and C (0.10 microg cm(-2) h(-1)). An inverse relationship was noted between lipophilicity and k(p) in each vehicle. The simultaneous transdermal delivery of the major actives of guarana was established, with permeation rates being highly concentration and vehicle dependent.

  2. Encapsulation of a flavonoid-rich Allium cepa L. var. agrogatum don extract in β-cyclodextrin for transdermal drug delivery.

    Science.gov (United States)

    Ding, Zhiying; Wu, Min; Guo, Qiushi; Yang, Xiaohong; Zhang, Bingren

    2013-05-22

    This work aims to evaluate the encapsulation of a flavonoid-rich Allium cepa L. var. agrogatum Don extract (ACADFE) in β-cyclodextrin (β-CD) by analyzing the percutaneous penetration in vitro and in vivo, leading to an explanation of the physical mechanism during transdermal transport. The optimal inclusion compound containing ACADFE in β-CD was prepared in a 1:3 molar ratio. The physicochemical characterization of the inclusion complex was performed using IR, UV-vis, simultaneous thermogravimetry (TG), and differential thermal analysis (DTA) studies. It was concluded that the inclusion complex could improve the aqueous solubility and bioavailability of ACADFE. The inclusion complex exhibited significant enhancement of percutaneous absorption both in vitro and in vivo. The dorsal skins of hairless mice were photographed using a confocal scanning laser microscope. Confocal scanning laser microscopy shows that penetration of the ACADFE-β-CD inclusion complex proceeds across skin via both follicular and transcellular routes.

  3. A high aspect ratio SU-8 fabrication technique for hollow microneedles for transdermal drug delivery and blood extraction

    Science.gov (United States)

    Chaudhri, Buddhadev Paul; Ceyssens, Frederik; De Moor, Piet; Van Hoof, Chris; Puers, Robert

    2010-06-01

    Protein drugs, e.g. hormonal drugs, cannot be delivered orally to a patient as they get digested in the gastro-intestinal (GI) tract. Thus, it is imperative that these kinds of drugs are delivered transdermally through the skin. To provide for real-time feedback as well as to test independently for various substances in the blood, we also need a blood sampling system. Microneedles can perform both these functions. Further, microneedles made of silicon or metal have the risk of breaking inside the skin thereby leading to complications. SU-8, being approved of as being biocompatible by the Food and Drug Agency (FDA) of the United States, is an attractive alternative because firstly it is a polymer material, thereby reducing the chances of breakages inside the skin, and secondly it is a negative photoresist, thereby leading to ease of fabrication. Thus, here we present very tall (around 1600 µm) SU-8 polymer-based hollow microneedles fabricated by a simple and repeatable process, which are a very good candidate for transdermal drug delivery as well as blood extraction. The paper elaborates on the details that allow the fabrication of such extreme aspect ratios (>100).

  4. Development and validation of a reverse phase liquid chromatography method for the simultaneous quantification of eserine and pralidoxime chloride in drugs-in-adhesive matrix type transdermal patches.

    Science.gov (United States)

    Banerjee, S; Chattopadhyay, P; Ghosh, A; Kaity, S; Veer, V

    2013-09-01

    In the present study, a simple, precise, specific, fast, accurate and reliable reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous determination and quantification of eserine and pralidoxime chloride in drugs-in-adhesive matrix type transdermal patches. The chromatographic separation was achieved by C18 column, using a mobile phase consisting of acetonitrile: 10 mM potassium dihydrogen phosphate, 10 mM heptane-1-sulfonic acid sodium salt monohydrate in water (30:70, v/v) adjusted at pH 3.0 with ortho-phosphoric acid. Flow rate was 1.0 mL/min and UV detection at 238 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines. The calibration curves were linear over the different concentration ranges of 0.5-10 μg/ml for eserine and 5-25 μg/mL for 2PAM. Relative standard deviation for precision was less than 2.0%. Limit of detection values of eserine and 2-PAM were 0.018 µg/mL and 0.008 µg/mL, respectively. The limit of quantification of eserine and 2-PAM were 0.055 µg/mL and 0.026 µg/mL, respectively. The developed method was applied for the routine analysis of these 2 drugs in drugs-in-adhesive matrix type transdermal patches in order to evaluate the drug content of different formulations. It could be also used with reliability for the determination of the drug in other pharmaceutical dosage forms. © Georg Thieme Verlag KG Stuttgart · New York.

  5. A fully validated LC-MS/MS method for simultaneous determination of nicotine and its metabolite cotinine in human serum and its application to a pharmacokinetic study after using nicotine transdermal delivery systems with standard heat application in adult smokers.

    Science.gov (United States)

    Abdallah, Inas A; Hammell, Dana C; Stinchcomb, Audra L; Hassan, Hazem E

    2016-05-01

    A sensitive and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of nicotine and its main metabolite cotinine in human serum samples. Liquid-liquid extraction using ethyl acetate was employed for serum sample extractions. Chromatographic separation was achieved on Phenomenex Luna(®) HILIC column (150 mm x 3.0mm, 5 μm). Isocratic elution was performed using acetonitrile:100mM ammonium formate buffer (pH=3.2) (90:10, v/v) as the mobile phase, at a flow rate of 0.4 mL/min. Tandem mass spectrometric detection was employed at positive electrospray ionization in MRM mode for the determination of both nicotine and cotinine and their stable isotope labeled internal standards. Analysis was carried out in 8 min over a concentration range of 0.26-52.5 ng/mL and 7.0-1500 ng/mL for nicotine and cotinine, respectively. The assay was validated according to FDA guidelines for bioanalytical method validation and satisfactory results were obtained; the accuracy ranged between 93.39% and 105.73% for nicotine and between 93.04% and 107.26% for cotinine. No significant matrix effect was observed. Stability assays indicated both nicotine and cotinine were stable during sample storage, preparation and analytical procedures. The method was successfully applied to biological samples obtained from a pharmacokinetic study conducted in adult smokers to investigate heat effect on nicotine and cotinine serum levels after nicotine transdermal delivery system (TDS) application. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Assay of 6-gingerol in CO2 supercritical fluid extracts of ginger and evaluation of its sustained release from a transdermal delivery system across rat skin.

    Science.gov (United States)

    Chen, Yan; Zhang, Cuiping; Zhang, Mei; Fu, Xiaobing

    2014-07-01

    Ginger has been widely used as healthy food condiment as well as traditional Chinese medicine since antiquity. Multiple potentials of ginger for treatment of various ailments have been revealed. However, the biological half-life of 6-gingerol (a principal pungent ingredient of ginger) is only 7.23 minutes while taken orally. Delivery of ginger compositions by routes other than oral have scarcely been reported. Therefore, we studied a noninvasive transdermal drug delivery system (TDDS) of ginger to bypass hepatic first pass metabolism, avoid gastrointestinal degradation and achieve long persistent release of effective compositions. After establishment of a HPLC analysis method of 6-gingerol, assays of 6-gingerol were performed to compare two kinds of ginger extracts. Then, the characteristics of transdermal delivery of 6-gingerol in TDDS were exhibited. The results showed that the contents of 6-gingerol in two kinds of ginger extracts were significantly different. The maximal delivery percentage of 6-gingerol across rat skin at 20 h was more than 40% in different TDDS formulations. TDDS may provide long-lasting delivery of ginger compounds.

  7. Characterisation of chamomile volatiles by simultaneous distillation solid-phase extraction in comparison to hydrodistillation and simultaneous distillation extraction.

    Science.gov (United States)

    Krüger, Hans

    2010-05-01

    A new method for complete separation of steam-volatile organic compounds is described using the example of chamomile flowers. This method is based on the direct combination of hydrodistillation and solid-phase extraction in a circulation apparatus. In contrast to hydrodistillation and simultaneous distillation extraction (SDE), an RP-18 solid phase as adsorptive material is used rather than a water-insoluble solvent. Therefore, a prompt and complete fixation of all volatiles takes place, and the circulation of water-soluble bisabololoxides as well as water-soluble and thermolabile en-yne-spiroethers is inhibited. This so-called simultaneous distillation solid-phase extraction (SD-SPE) provides extracts that better characterise the real composition of the vapour phase, as well as the composition of inhalation vapours, than do SDE extracts or essential oils obtained by hydrodistillation. The data indicate that during inhalation therapy with chamomile, the bisabololoxides and spiroethers are more strongly involved in the inhaling activity than so far assumed. Georg Thieme Verlag KG Stuttgart New York.

  8. Use of reverse micelles for the simultaneous extraction of oil, proteins, and glucosinolates from cruciferous oilseeds.

    Science.gov (United States)

    Ugolini, Luisa; De Nicola, Gina; Palmieri, Sandro

    2008-03-12

    Cruciferous oilseeds are important sources of oil, proteins, and glucosinolates (GLs), potentially available when biorefinery processes are used. The proposed extraction technology is based on the use of reverse micelles (RMs) made with cetyltrimethylammonium bromide (CTAB) dispersed in organic solvent. The physicochemical properties of this extraction system and the good water solubility of many high value compounds, such as GLs and some proteins, permit the simultaneous extraction of oil, and these products from cruciferous oilseed meals. This procedure is based on three main steps: (i) seed conditioning; (ii) solid-liquid extraction by RM solution; and (iii) back-transfer of the RM solution for recovery of the extracted compounds. The method makes it possible to simultaneously extract almost the same amount of oil as with pure organic solvents used in the current extraction plants and more than 90% of soluble proteins and GLs. It is a promising biorefinery technology alternative to traditional oil extraction processes.

  9. Buprenorphine Transdermal Patch

    Science.gov (United States)

    Buprenorphine patches are used to relieve severe pain in people who are expected to need pain medication ... Transdermal buprenorphine comes as a patch to apply to the skin. The patch is usually applied to the skin ...

  10. Simultaneous extraction of chitin and astaxanthin from waste of ...

    African Journals Online (AJOL)

    From deproteinised exoskeleton, astaxanthin was extracted in methanol, transferred into various vegetable oils, and its concentration measured using spectrophotometry. Maximum stable concentration of astaxanthin in oil was approximately 80 mg ml–1, above which astaxanthin precipitated. Astaxanthin oil prepared from ...

  11. Alghedon Fentanyl Transdermal System.

    Science.gov (United States)

    Romualdi, Patrizia; Santi, Patrizia; Candeletti, Sanzio

    2017-04-01

    The efficacy of transdermal fentanyl for cancer pain and chronic non-cancer pain (chronic lower back pain, rheumatoid arthritis, osteoarthritis, neuropathic pain) is well established. Several formulations of fentanyl transdermal systems have been developed to improve the drug delivery and prevent misuse of the active principle. The addition of a rate controlling membrane to the matrix system represented an important advance. The design and functional features of Alghedon patch are compared with other approved generic fentanyl transdermal systems, emphasizing the distinctiveness of Alghedon patch. Alghedon patch has no liquid component in the finished product, therefore no leakage of active ingredient from the system can occur. A rate-controlling membrane provides controlled release of the active substance from the matrix reservoir, ensuring that fentanyl delivery and entry into the microcirculation is not solely controlled by the skin's permeability to this active substance. Alghedon patch contains part of the drug (approximately 15%) in the skin-contact adhesive: this innovative solution allows to overcome a typical drawback of transdermal patches, i.e. the long lag-time before the drug appears in plasma after the first administration, and provides rapid analgesia during the first hours of administration. Alghedon Fentanyl Transdermal System employs materials commonly used in other transdermal applications and having established safety profiles. For each strength level, the fentanyl content - and, thus, the resulting residual fentanyl remaining in the patch after use - is at the lowest end of the range used in commercially available fentanyl patches, minimizing the potential for abuse and misuse.

  12. Enzymatic aqueous technology for simultaneous coconut protein and oil extraction

    Directory of Open Access Journals (Sweden)

    Coelho, Maria A. Z.

    2003-03-01

    Full Text Available In this study, the following commercial enzymes were evaluated in the enzymatic extraction of oil and protein from coconut: Celluclast, Termamyl, Viscozyme, Neutrase y Protease. Preliminary experiments were carried out for selection of enzymes, enzyme concentration and incubation time. In order to verify the effects of pH and water/substrate ratio, a response surface methodology was applied based in a 32 full factorial experimental design. The pH is the most meaningful parameter on oil and protein extraction yields, with a significance level higher than 90%. The maximal extraction yields of oil and protein emulsion (83% was reached using Viscozyme L and subsequently Neutrase 1.5 MG at concentrations of 0.6% (w/w and 0.3% (w/w, respectively, total incubation time of 60 minutes, substrate/water ratio 1:6 and pH around 7 (no adjustment.En este trabajo diferentes enzimas hidroliticos fueron usados para la extracción de aceite y proteína de coco: Celluclast, Termamyl, Viscozyme, Neutrase y Protease producidos por Novo Nordisk. Experimientos preliminares fueron encaminados a la selección de los extractos enzimaticos, de las concentraciones de las enzimas y de los tiempos de incubación. La técnica de análisis de varianza, mediante un delineamiento factorial en tres niveles, fue usada para la optimización de los procesos con relación a los parámetros pH y razón sustrato/agua. Comparando con la extracción acuosa todos los enzimas hidroliticos incrementan la extracción de aceite y proteína vegetal de coco. Los coeficientes de correlación muestran que el pH fué el parámetro mas significativo (pViscozyme y Neutrase 0.6 % (w/w y 0.3 % (w/w, respectivamente, tiempo de incubación 30 minutos, razón sustrato/agua 1:6 y pH 7.

  13. Comparison and optimization of methods for the simultaneous extraction of DNA, RNA, proteins, and metabolites.

    Science.gov (United States)

    Vorreiter, Fränze; Richter, Silke; Peter, Michel; Baumann, Sven; von Bergen, Martin; Tomm, Janina M

    2016-09-01

    The challenge of performing a time-resolved comprehensive analysis of molecular systems has led to the quest to optimize extraction methods. When the size of a biological sample is limited, there is demand for the simultaneous extraction of molecules representing the four areas of "omics": genomics, transcriptomics, proteomics, and metabolomics. Here we optimized a protocol for the simultaneous extraction of DNA, RNA, proteins, and metabolites and compared it with two existing protocols. Our optimization comprised the addition of a methanol/chloroform metabolite purification before the separation of DNA/RNA and proteins. Extracted DNA, RNA, proteins, and metabolites were quantitatively and/or qualitatively analyzed. Of the three methods, only the newly developed protocol yielded all biomolecule classes of adequate quantity and quality. Copyright © 2016 The Author(s). Published by Elsevier Inc. All rights reserved.

  14. Testosterone Transdermal Patch

    Science.gov (United States)

    ... growth, development, and functioning of the male sexual organs and typical male characteristics. Testosterone transdermal patches work ... Keep this medication in the container it came in, tightly closed, and out of reach of children. Store it at room temperature and away from excess heat ...

  15. Perspectives on Transdermal Electroporation

    Directory of Open Access Journals (Sweden)

    Kevin Ita

    2016-03-01

    Full Text Available Transdermal drug delivery offers several advantages, including avoidance of erratic absorption, absence of gastric irritation, painlessness, noninvasiveness, as well as improvement in patient compliance. With this mode of drug administration, there is no pre-systemic metabolism and it is possible to increase drug bioavailability and half-life. However, only a few molecules can be delivered across the skin in therapeutic quantities. This is because of the hindrance provided by the stratum corneum. Several techniques have been developed and used over the last few decades for transdermal drug delivery enhancement. These include sonophoresis, iontophoresis, microneedles, and electroporation. Electroporation, which refers to the temporary perturbation of the skin following the application of high voltage electric pulses, has been used to increase transcutaneous flux values by several research groups. In this review, transdermal electroporation is discussed and the use of the technique for percutaneous transport of low and high molecular weight compounds described. This review also examines our current knowledge regarding the mechanisms of electroporation and safety concerns arising from the use of this transdermal drug delivery technique. Safety considerations are especially important because electroporation utilizes high voltage pulses which may have deleterious effects in some cases.

  16. Simultaneous distillation-extraction of high-value volatile compounds from Cistus ladanifer L.

    Science.gov (United States)

    Teixeira, Salomé; Mendes, Adélio; Alves, Arminda; Santos, Lúcia

    2007-02-19

    The present paper describes a procedure to isolate volatiles from rock-rose (Cistus ladanifer L.) using simultaneous distillation-extraction (SDE). High-value volatile compounds (HVVC) were selected and the influence of the extraction conditions investigated. The effect of the solvent nature and extraction time on SDE efficiency was studied. The best performance was achieved with pentane in 1 h operation. The extraction efficiencies ranged from 65% to 85% and the repeatability varied between 4% and 6% (as a CV%). The C. ladanifer SDE extracts were analysed by headspace solid phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The HS-SPME sampling conditions such as fiber coating, temperature, ionic strength and exposure time were optimized. The best results were achieved with an 85 microm polyacrylate fiber for a 60 min headspace extraction at 40 degrees C with 20% (w/v) of NaCl. For optimized conditions the recovery was in average higher than 90% for all compounds and the intermediate precision ranged from 4 to 9% (as CV %). The volatiles alpha-pinene (22.2 mg g(-1) of extract), 2,2,6-trimethylcyclohexanone (6.1 mg g(-1) of extract), borneol (3.0 mg g(-1) of extract) and bornyl acetate (3.9 mg g(-1) of extract) were identified in the SDE extracts obtained from the fresh plant material.

  17. Simultaneous cloud point extraction of low levels of Cd, Cr and Hg in ...

    African Journals Online (AJOL)

    A one-step preconcentration cloud point extraction (CPE) method has been developed for the simultaneous determination of Cd, Cr, and Hg using a mixture of 1-(2-pyridylazo)-2-naphthol (PAN) and 1-(2-thiazolylazo)-2-naphthol (TAN) chelating agents and polyoxyethylene nonylphenylether-20 (PONPE-20) surfactant.

  18. Modeling of transdermal drug delivery with a microneedle array

    Science.gov (United States)

    Lv, Y.-G.; Liu, J.; Gao, Y.-H.; Xu, B.

    2006-11-01

    Transdermal drug delivery is generally limited by the extraordinary barrier properties of the stratum corneum, the outer 10-15 µm layer of skin. A conventional needle inserted across this barrier and into deeper tissues could effectively deliver drugs. However, it would lead to infection and cause pain, thereby reducing patient compliance. In order to administer a frequent injection of insulin and other therapeutic agents more efficiently, integrated arrays with very short microneedles were recently proposed as very good candidates for painless injection or extraction. A variety of microneedle designs have thus been made available by employing the fabrication tools of the microelectronics industry and using materials such as silicon, metals, polymers and glass with feature sizes ranging from sub-micron to nanometers. At the same time, experiments were also made to test the capability of the microneedles to inject drugs into tissues. However, due to the difficulty encountered in measurement, a detailed understanding of the spatial and transient drug delivery process still remains unclear up to now. To better grasp the mechanisms involved, quantitative theoretical models were developed in this paper to simultaneously characterize the flow and drug transport, and numerical solutions were performed to predict the kinetics of dispersed drugs injected into the skin from a microneedle array. Calculations indicated that increasing the initial injection velocity and accelerating the blood circulation in skin tissue with high porosity are helpful to enhance the transdermal drug delivery. This study provides the first quantitative simulation of fluid injection through a microneedle array and drug species transport inside the skin. The modeling strategy can also possibly be extended to deal with a wider range of clinical issues such as targeted nanoparticle delivery for therapeutics or molecular imaging.

  19. Transdermal hyoscine induced unilateral mydriasis.

    LENUS (Irish Health Repository)

    Hannon, Breffni

    2012-03-20

    The authors present a case of unilateral mydriasis in a teenager prescribed transdermal hyoscine hydrobromide (scopolamine) for chemotherapy induced nausea and vomiting. The authors discuss the ocular side-effects associated with this particular drug and delivery system and the potential use of transdermal hyoscine as an antiemetic agent in this group.

  20. Encapsulated Curcumin for Transdermal Administration

    African Journals Online (AJOL)

    Purpose: To develop a proniosomal carrier system of curcumin for transdermal delivery. Methods: Proniosomes of curcumin were prepared by encapsulation of the drug in a mixture of Span 80, cholesterol and diethyl ether by ether injection method, and then investigated as a transdermal drug delivery system (TDDS).

  1. Transdermal Spray in Hormone Delivery

    African Journals Online (AJOL)

    market for the delivery system and ongoing development of transdermal sprays for hormone delivery. Keywords: Transdermal, Delivery systems, ... delivery compared with gels, emulsions, patches, and subcutaneous implants. Among .... In a safety announcement, the US Food and. Drug Administration (FDA) warned that ...

  2. Simultaneous extraction and biotransformation process to obtain high bioactivity phenolic compounds from Brazilian citrus residues.

    Science.gov (United States)

    Madeira, Jose Valdo; Macedo, Gabriela Alves

    2015-01-01

    Recent studies have pointed to a reduction in the incidence of some cancers, diabetes, and neuro-degenerative diseases as a result of human health benefits from flavanones. Currently, flavanones are obtained by chemical synthesis or extraction from plants, and these processes are only produced in the glycosylated form. An interesting environmentally friendly alternative that deserves attention regarding phenolic compound production is the simultaneous extraction and biotransformation of these molecules. Orange juice consumption has become a worldwide dietary habit and Brazil is the largest producer of orange juice in the world. Approximately half of the citrus fruit is discarded after the juice is processed, thus generating large amounts of residues (peel and pectinolytic material). Hence, finding an environmentally clean technique to extract natural products and bioactive compounds from different plant materials has presented a challenging task over the last decades. The aim of this study was to obtain phenolics from Brazilian citrus residues with high bioactivity, using simultaneous extraction (cellulase and pectinase) and biotransformation (tannase) by enzymatic process. The highest hesperetin, naringenin and ellagic acid production in the experiment were 120, 80, and 11,250 µg g(-1), respectively, at 5.0 U mL(-1) of cellulase and 7.0 U mL(-1) of tannase at 40°C and 200 rpm. Also, the development of this process generated an increase of 77% in the total antioxidant capacity. These results suggest that the bioprocess obtained innovative results where the simultaneous enzymatic and biotransformatic extracted flavanones from agro-industrial residues was achieved without the use of organic solvents. The methodology can therefore be considered a green technology. © 2015 American Institute of Chemical Engineers.

  3. Ionic liquids based simultaneous ultrasonic and microwave assisted extraction of phenolic compounds from burdock leaves

    Energy Technology Data Exchange (ETDEWEB)

    Lou Zaixiang, E-mail: louzaixiang@126.com [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Wang Hongxin, E-mail: whx200720082009@yahoo.cn [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Zhu Song; Chen Shangwei; Zhang Ming; Wang Zhouping [State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China)

    2012-02-24

    The ionic liquids based simultaneous ultrasonic and microwave assisted extraction (IL-UMAE) technique was first proposed and applied to isolate compounds. The ionic liquids comprising a range of four anions, five 1-alkyl-3-methylimidazolium derivatives were designed and prepared. The results suggested that varying the anion and cation both had apparent effects on the extraction of phenolics. The results also showed that irradiation power, time and solid-liquid ratio significantly affected the yields. The yields of caffeic acid and quercetin obtained by IL-UMAE were higher than those by regular UMAE. Compared with conventional heat-reflux extraction (HRE), the proposed approach exhibited higher efficiency (8-17% enhanced) and shorter extraction time (from 5 h to 30 s). The results indicated ILUMAE to be a fast and efficient extraction technique. Moreover, the proposed method was validated by the reproducibility and recovery experiments. The ILUMAE method provided good recoveries (from 96.1% to 105.3%) with RSD lower than 5.2%, which indicated that the proposed method was credible. Based on the designable nature of ionic liquids, and the rapid and highly efficient performance of the proposed approach, ILUMAE provided a new alternative for preparation of various useful substances from solid samples.

  4. Simultaneous determination of nine phytohormones in seaweed and algae extracts by HPLC-PDA.

    Science.gov (United States)

    Górka, Bogusława; Wieczorek, Piotr P

    2017-07-01

    An RP-HPLC-PDA method for the simultaneous analysis of 9 compounds deriving from the phytohormones class was developed and optimized, namely indoleacetic acid (IAA), indolebutyric acid (IBA), phenyleacetic acid (PAA), naphtyleacetic acid (NAA), trans-zeatin (TZ), kinetin (KA), isopentenyladenine (IA), 6-benzylaminopurine (6-BA) and abscisic acid (ABA). Validation of the method was performed on the SFE-CO2 extract made out of the mixture of Baltic algae. The regression coefficients for plant hormones were in the range from 0.997 to 0.999. The LOD and LOQ were on the levels from 0.05-0.29 and 0.15-0.88mg/L, respectively. Developed method was used for the separation and determination plant hormones in extracts obtained by SFE-CO2 (supercritical fluid extraction) made out of the mixture of Baltic algae, Cladophora glomerata and Spirulina sp. In the extract of Baltic seaweed 2 of tested compounds were present in the concentration of 154,45±20,63μg/g for TZ and 362,47±13,00μg/g for PAA, whereas in Cladophora glomerata extract contained PAA and IAA in the concentration of 229,30±7,90μg/g and 23,91±0,80μg/g, respectively (all values per g of extract). The differences in the hormones levels may occur due to the different scale of extract preparation (laboratory or industrial) and other factors like the place of algae collection, year of collection or the way of biomass preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Ultrasound-assisted extraction method for the simultaneous determination of emerging contaminants in freshwater sediments.

    Science.gov (United States)

    de Sousa, Diana Nara Ribeiro; Grosseli, Guilherme Martins; Mozeto, Antonio Aparecido; Carneiro, Renato Lajarim; Fadini, Pedro Sergio

    2015-10-01

    Sediments are the fate of several emerging organic contaminants, such as pharmaceuticals, personal care products and hormones, and therefore an important subject in environmental monitoring studies. In the present work, a simple and sensitive method was developed, validated and applied for the simultaneous extraction of atenolol, caffeine, carbamazepine, diclofenac, ibuprofen, naproxen, propranolol, triclosan, estrone, 17-β-estradiol and 17-α-ethinylestradiol using ultrasound-assisted extraction from freshwater sediment samples followed by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection. The solvent type and extraction pH were evaluated to obtain the highest recoveries of the compounds. The best method shows absolute recoveries between 54.0 and 94.4% at 50 ng/g concentration. The method exhibits good precision with relative standard deviation ranging from 1.0-16%. The detection and quantification limits ranged from 0.006-0.067 and 0.016-0.336 ng/g, respectively. The developed method was successfully applied to freshwater sediment samples collected from different sites in Jundiaí River basin of São Paulo State, Brazil. The compounds atenolol, caffeine, propranolol and triclosan were detected in all the sampling sites with concentrations of 13.8, 41.0, 28.5 and 176 ng/g, respectively. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Volatile components and key odorants of fennel (Foeniculum vulgare Mill.) and thyme (Thymus vulgaris L.) oil extracts obtained by simultaneous distillation-extraction and supercritical fluid extraction.

    Science.gov (United States)

    Díaz-Maroto, M Consuelo; Díaz-Maroto Hidalgo, Ignacio Javier; Sánchez-Palomo, Eva; Pérez-Coello, M Soledad

    2005-06-29

    Volatile oil extracts of fennel seeds (Foeniculum vulgare Mill.) and thyme leaves (Thymus vulgaris L.) were obtained by simultaneous distillation-extraction (SDE) and supercritical fluid extraction (SFE) and analyzed by gas chromatography-mass spectrometry (GC-MS). In general, fennel oil extracted by SDE and SFE showed similar compositions, with trans-anethole, estragole, and fenchone as the main components. In contrast, thymol and p-cymene, the most abundant compounds in thyme leaves, showed big differences, with generally higher amounts of monoterpenes obtained by SDE. However, in this case, the differences between the extracts were higher. Key odorants of fennel seeds determined by gas chromatography-olfactometry (GC-O) showed similar patterns when applying SDE and SFE. trans-Anethole (anise, licorice), estragole (anise, licorice, sweet), fenchone (mint, camphor, warm), and 1-octen-3-ol (mushroom) were the most intense odor compounds detected in fennel extracts. Thymol and carvacrol, with oregano, thyme, and spicy notes, were identified as key compounds contributing to the aroma of thyme leaves.

  7. Validated TLC method for simultaneous quantitation of kutkoside and picroside-I from Kutki extract.

    Science.gov (United States)

    Gaikwad, P S; Bhope, S G; Kuber, V V; Patil, M J

    2011-01-01

    The two iridoid glycosides kutkoside and picroside-I are the active hepatoprotective principles of Picrorhiza kurroa Royle ex Benth (Scrophulariaceae), commonly known as Kutki. Quantitation of these phytoconstituents is important for the routine quality control of Kutki extract. To develop and validate a simple, precise and rapid thin-layer chromatography (TLC) method for the simultaneous quantitation of kutkoside and picroside-I in Kutki extract. The analysis was performed on a TLC precoated silica gel 60 F(254) plate with ethyl acetate:methanol:glacial acetic acid:formic acid (25:5:1:1, v/v/v/v) as mobile phase. Densitometric evaluation of kutkoside and picroside-I was carried out at 265  nm and the mobile phase showed good resolution with R(f) values 0.42 ± 0.03 and 0.61 ± 0.03 for kutkoside and picroside-I, respectively. The method was validated in terms of specificity, linearity, accuracy and precision. The content of kutkoside and picroside-I was found to be 2.18 and 1.90%, respectively, and was comparable with those obtained by HPLC. The linearity was found to be in the range of 80-480  ng/spot for both kutkoside and picroside-I. The average recovery values were found to be 96.5 and 96.0% for kutkoside and picroside-I, respectively. The developed method was found to be relatively simple, precise and reproducible for the simultaneous quantitation of kutkoside and picroside-I. The method does not employ any derivatisation procedure and can be used as a quality control tool for the routine analysis of commercial Kutki extracts. Copyright © 2010 John Wiley & Sons, Ltd.

  8. MPLEx: a method for simultaneous pathogen inactivation and extraction of samples for multi-omics profiling

    Energy Technology Data Exchange (ETDEWEB)

    Burnum-Johnson, Kristin E.; Kyle, Jennifer E.; Eisfeld, Amie J.; Casey, Cameron P.; Stratton, Kelly G.; Gonzalez, Juan F.; Habyarimana, Fabien; Negretti, Nicholas M.; Sims, Amy C.; Chauhan, Sadhana; Thackray, Larissa B.; Halfmann, Peter J.; Walters, Kevin B.; Kim, Young-Mo; Zink, Erika M.; Nicora, Carrie D.; Weitz, Karl K.; Webb-Robertson, Bobbie-Jo M.; Nakayasu, Ernesto S.; Ahmer, Brian; Konkel, Michael E.; Motin, Vladimir; Baric, Ralph S.; Diamond, Michael S.; Kawaoka, Yoshihiro; Waters, Katrina M.; Smith, Richard D.; Metz, Thomas O.

    2017-01-01

    The continued emergence and spread of infectious agents is of increasing concern due to increased population growth and the associated increased livestock production to meet food demands, increased urbanization and land-use changes, and greater travel. A systems biology approach to infectious disease research can significantly advance our understanding of host-pathogen relationships and facilitate the development of new therapies and vaccines. Molecular characterization of infectious samples outside of appropriate biosafety containment can only take place subsequent to pathogen inactivation. Herein, we describe a modified Folch extraction using chloroform/methanol that facilitates the molecular characterization of infectious samples by enabling simultaneous pathogen inactivation and extraction of proteins, metabolites, and lipids for subsequent mass spectrometry-based multi-omics measurements. This metabolite, protein and lipid extraction (MPLEx) method resulted in complete inactivation of bacterial and viral pathogens with exposed lipid membranes, including Yersinia pestis, Salmonella Typhimurium, and Campylobacter jejuni in pure culture, and Yersinia pestis, Campylobacter jejuni, West Nile, MERS-CoV, Ebola, and influenza H7N9 viruses in infection studies. Partial inactivation was observed for pathogens without exposed lipid membranes including 99.99% inactivation of community-associated methicillin-resistant Staphylococcus aureus, 99.6% and >99% inactivation of Clostridium difficile spores and vegetative cells, respectively, and 50% inactivation of adenovirus type 5. To demonstrate that MPLEx yields biomaterial of sufficient quality for subsequent multi-omics analyses, we highlight select proteomics, metabolomics and lipidomics data from human epithelial lung cells infected with wild-type and mutant forms of influenza H7N9. We believe that MPLEx will facilitate systems biology studies of infectious samples by enabling simultaneous pathogen inactivation and multi

  9. Effective extraction and assembly methods for simultaneously obtaining plastid and mitochondrial genomes.

    Science.gov (United States)

    Hao, Wanjun; Fan, Shihang; Hua, Wei; Wang, Hanzhong

    2014-01-01

    In conventional approaches to plastid and mitochondrial genome sequencing, the sequencing steps are performed separately; thus, plastid DNA (ptDNA) and mitochondrial DNA (mtDNA) should be prepared independently. However, it is difficult to extract pure ptDNA and mtDNA from plant tissue. Following the development of high-throughput sequencing technology, many researchers have attempted to obtain plastid genomes or mitochondrial genomes using high-throughput sequencing data from total DNA. Unfortunately, the huge datasets generated consume massive computing and storage resources and cost a great deal, and even more importantly, excessive pollution reads affect the accuracy of the assembly. Therefore, it is necessary to develop an effective method that can generate base sequences from plant tissue and that is suitable for all plant species. Here, we describe a highly effective, low-cost method for obtaining plastid and mitochondrial genomes simultaneously. First, we obtained high-quality DNA employing Partial Concentration Extraction. Second, we evaluated the purity of the DNA sample and determined the sequencing dataset size employing Vector Control Quantitative Analysis. Third, paired-end reads were obtained using a high-throughput sequencing platform. Fourth, we obtained scaffolds employing Two-step Assembly. Finally, we filled in gaps using specific methods and obtained complete plastid and mitochondrial genomes. To ensure the accuracy of plastid and mitochondrial genomes, we validated the assembly using PCR and Sanger sequencing. Using this method,we obtained complete plastid and mitochondrial genomes with lengths of 153,533 nt and 223,412 nt separately. A simple method for extracting, evaluating, sequencing and assembling plastid and mitochondrial genomes was developed. This method has many advantages: it is timesaving, inexpensive and reproducible and produces high-quality sequence. Furthermore, this method can produce plastid and mitochondrial genomes

  10. Effective extraction and assembly methods for simultaneously obtaining plastid and mitochondrial genomes.

    Directory of Open Access Journals (Sweden)

    Wanjun Hao

    Full Text Available In conventional approaches to plastid and mitochondrial genome sequencing, the sequencing steps are performed separately; thus, plastid DNA (ptDNA and mitochondrial DNA (mtDNA should be prepared independently. However, it is difficult to extract pure ptDNA and mtDNA from plant tissue. Following the development of high-throughput sequencing technology, many researchers have attempted to obtain plastid genomes or mitochondrial genomes using high-throughput sequencing data from total DNA. Unfortunately, the huge datasets generated consume massive computing and storage resources and cost a great deal, and even more importantly, excessive pollution reads affect the accuracy of the assembly. Therefore, it is necessary to develop an effective method that can generate base sequences from plant tissue and that is suitable for all plant species. Here, we describe a highly effective, low-cost method for obtaining plastid and mitochondrial genomes simultaneously.First, we obtained high-quality DNA employing Partial Concentration Extraction. Second, we evaluated the purity of the DNA sample and determined the sequencing dataset size employing Vector Control Quantitative Analysis. Third, paired-end reads were obtained using a high-throughput sequencing platform. Fourth, we obtained scaffolds employing Two-step Assembly. Finally, we filled in gaps using specific methods and obtained complete plastid and mitochondrial genomes. To ensure the accuracy of plastid and mitochondrial genomes, we validated the assembly using PCR and Sanger sequencing. Using this method,we obtained complete plastid and mitochondrial genomes with lengths of 153,533 nt and 223,412 nt separately.A simple method for extracting, evaluating, sequencing and assembling plastid and mitochondrial genomes was developed. This method has many advantages: it is timesaving, inexpensive and reproducible and produces high-quality sequence. Furthermore, this method can produce plastid and mitochondrial

  11. Simultaneous ultrasound-assisted emulsification-extraction of polar and nonpolar compounds from solid plant samples.

    Science.gov (United States)

    Pérez-Serradilla, J A; Priego-Capote, F; Luque de Castro, M D

    2007-09-01

    A new approach to solid sample preparation for the simultaneous isolation of polar and nonpolar compounds using a microemulsion as leaching medium is proposed. Methanol/water (dispersed-phase)-hexane (continuous-phase) emulsions formed in the presence of ultrasound and a solid sample allow polar and nonpolar compounds to be transferred to the dispersed and continuous phase, respectively. The efficiency of this dual sample preparation approach was assessed in the characterization of natural products of variable hardness including acorns, grape seeds, and alperujo (a residue of olive oil production). The time needed for quantitative extraction of the target fractions (phenol compounds and fatty acids) is 9 min for acorns and alperujo and 20 min for grape seeds; the longer time needed for grape seeds can be attributed to higher matrix hardness. Such good performance can be ascribed to the ultrasound-enhanced formation of methanol/water microdroplets 1-15 microm in size, which act as solid-liquid microextractors spanning a large surface area. The presence of the sample was found to greatly improve emulsion stability, which can be ascribed to the amphiphilic nature of the fatty acids in the samples. Following leaching and separation of the two phases by centrifugation, the polar and nonpolar fractions were analyzed by HPLC-diode array detection and GC/MS, respectively. The proposed approach provides extraction efficiency similar to the Folch method (reference method for fat extraction, 4.5 h) in a shorter time and extraction efficiency equal to or higher than the stirring-based method (reference method for phenol compounds extraction, 24 h).

  12. Development of Transdermal Ondansetron Hydrochloride for the ...

    African Journals Online (AJOL)

    ) transdermal patch for the treatment of chemotherapy-induced nausea and vomiting. Methods: Transdermal patches were prepared by solvent casting method using ethyl cellulose and polyvinyl pyrrolidone as matrix materials, and dibutyl ...

  13. Simultaneous column chromatographic extraction and purification of abscisic acid in peanut plants for direct HPLC analysis.

    Science.gov (United States)

    Zhang, Ya-Wen; Fan, Wei-Wei; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

    2015-10-01

    Abscisic acid (ABA), a universal signaling molecule, plays important roles in regulating plant growth, development and stress responses. The low contents and complex components in plants make it difficult to be accurately analyzed. A novel one-step sample preparation method for ABA in plants was developed. Fresh peanut (Arachis hypogaea) plant materials were fixed by oven-drying, microwave drying, boiling or Carnoy's fixative, and loaded onto a mini-preparing column. After washed the impurities, ABA was eluted with a small amount of solvent. ABA in plant materials was completely extracted and purified in 2mL solution and directly analyzed by HPLC, with a 99.3% recovery rate. Multiple samples can be simultaneously prepared. Analyses using this method indicated that the endogenous ABA in oven-dried peanut leaves increased 20.2-fold from 1.01 to 20.37μgg(-1) dry weight within 12h and then decreased in 30% polyethylene glycol 6000 treated plants, and increased 3.34-fold from 0.85 to 2.84μgg(-1) dry weight in 5 days and then decreased in soil drought treated plants. The method combined the column chromatographic extraction and solid-phase separation technologies in one step and can completely extracted plant endogenous ABA in a purified and highly concentrated form for direct HPLC analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Synthesis of Analcime Crystals and Simultaneous Potassium Extraction from Natrolite Syenite

    Directory of Open Access Journals (Sweden)

    Jian Chen

    2017-01-01

    Full Text Available Analcime single crystals were successfully synthesized from natrolite syenite powder (K2O 10.89% and 92.6% of potassium was extracted simultaneously by means of soda roasting followed by alkali-hydrothermal method. Effects of NaOH concentration, reaction temperature, and holding period on the analcime formation and potassium extraction were investigated systemically. The results indicated that NaOH concentration plays an important role in determining the chemical composition of zeolites and size distribution; by turning the NaOH concentrations, three different pure zeolites (i.e., the phillipsite-Na, the analcime, and the sodalite were prepared. Besides, a higher temperature could accelerate the dissolution of K+ ions and enhance the crystallinity degree of zeolite. The reactions involved in the analcime synthesis can be summarized as follows: sodium aluminum silicate dissolution → precipitation and dissolution of metastable zeolite-P → analcime nucleation → analcime growth. The extraction ratio of K+ is associated with the types of synthesized zeolites, among which analcime is the most effective to promote potassium leaching out from zeolite lattice position. The optimal condition for analcime crystallization and K+ leaching is found to be as follows: 175°C for 4 h in 0.5 mol/L NaOH solution.

  15. Preparation and physicochemical evaluation of transdermal ...

    African Journals Online (AJOL)

    Preparation and physicochemical evaluation of transdermal aerosols containing ketoprofen ... Purpose: To prepare transdermal ketoprofen metered-dose aerosol formulations containing menthol and isopropyl myristate (IPM) as ..... of a transdermal delivery system for aspirin as an antithrombotic drug. Int J Pharm 2006; ...

  16. Simultaneously extracting multiple parameters via fitting one single autocorrelation function curve in diffuse correlation spectroscopy.

    Science.gov (United States)

    Dong, Lixin; He, Lian; Lin, Yu; Shang, Yu; Yu, Guoqiang

    2013-02-01

    Near-infrared diffuse correlation spectroscopy (DCS) has recently been employed for noninvasive acquisition of blood flow information in deep tissues. Based on the established correlation diffusion equation, the light intensity autocorrelation function detected by DCS is determined by a blood flow index αD(B), tissue absorption coefficient μ(a), reduced scattering coefficient μ'(s), and a coherence factor β. This study is designed to investigate the possibility of extracting multiple parameters such as μ(a), μ'(s), β, and αD(B) through fitting one single autocorrelation function curve and evaluate the performance of different fitting methods. For this purpose, computer simulations, tissue-like phantom experiments, and in vivo tissue measurements were utilized. The results suggest that it is impractical to simultaneously fit αD(B) and μ(a) or αD(B) and μ'(s) from one single autocorrelation function curve due to the large crosstalk between these paired parameters. However, simultaneously fitting β and αD(B) is feasible and generates more accurate estimation with smaller standard deviation compared to the conventional two-step fitting method (i.e., first calculating β and then fitting αD(B)). The outcomes from this study provide a crucial guidance for DCS data analysis.

  17. Microwave assisted dehydration of broccoli by-products and simultaneous extraction of bioactive compounds.

    Science.gov (United States)

    Ferreira, Sónia S; Passos, Cláudia P; Cardoso, Susana M; Wessel, Dulcineia F; Coimbra, Manuel A

    2018-04-25

    Broccoli by-products from frozen-food industry account for 45% of the initial broccoli heads. They consist on stalks, inflorescences, and leaves, blanched and non-blanched, sharing the nutritional value and bioactive compounds of commercial broccoli heads. However, their high perishability prevents further valorisation. Therefore, in this study microwave hydrodiffusion and gravity (MHG) technology was used to dehydrate broccoli by-products and simultaneously recover the water-soluble diffused compounds for food ingredients use. The hydrodiffusion allowed to obtain a dried material with 12% moisture in 43 min when 550 g of broccoli by-products were used, preserving polysaccharides and proteins. Diffused water contained up to 317 µg/mL gallic acid equivalents of phenolic compounds, 11 mg/mL free sugars, 9 mg/mL amino acids, and 356 µg/mL glucosinolates, depending on the type of by-product used. These results show the potential of MHG technology for valorisation of broccoli by-products by its simultaneous stabilization by dehydration and extraction of bioactive compounds. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Transdermal opioids for cancer pain.

    Science.gov (United States)

    Cachia, Elaine; Ahmedzai, Sam H

    2011-03-01

    Cancer patients with moderate-to-severe pain require opioids for analgesia. Whereas early guidelines recommend oral morphine as the 'drug of choice', newer synthetic opioids can be given by a reliable and effective nonoral transdermal route. We examine the mode of action of transdermal patches and we review the evidence on two drugs, which are currently available in this formulation - buprenorphine and fentanyl - covering physicochemical characteristics and pharmacokinetics of the patches, clinical efficacy data and adverse effects. Both buprenorphine and fentanyl possess ideal characteristics for transdermal delivery, being small molecules with high lipophilicity. Studies of buprenorphine patches show benefits but there is poor randomized controlled trial evidence comparing them with oral opioids. Fentanyl patches have been used for longer and have a larger body of evidence supporting their use, with data to suggest improved pain relief and reduced opioid side effects compared with sustained release oral morphine. Patients who have used both oral morphine and transdermal fentanyl express a preference for the patch drug. Transdermal buprenorphine and fentanyl are now established for moderate-to-severe cancer pain. There is still a need for further comparative studies with other opioids, especially for buprenorphine.

  19. A single extraction and HPLC procedure for simultaneous analysis of phytosterols, tocopherols and lutein in soybeans.

    Science.gov (United States)

    Slavin, Margaret; Yu, Liangli Lucy

    2012-12-15

    A saponification/extraction procedure and high performance liquid chromatography (HPLC) analysis method were developed and validated for simultaneous analysis of phytosterols, tocopherols and lutein (a carotenoid) in soybeans. Separation was achieved on a phenyl column with a ternary, isocratic solvent system of acetonitrile, methanol and water (48:22.5:29.5, v/v/v). Evaporative light scattering detection (ELSD) was used to quantify β-sitosterol, stigmasterol, campesterol, and α-, δ- and γ-tocopherols, while lutein was quantified with visible light absorption at 450 nm. Peak identification was verified by retention times and spikes with external standards. Standard curves were constructed (R(2)>0.99) to allow for sample quantification. Recovery of the saponification and extraction was demonstrated via analysis of spiked samples. Also, the accuracy of results of four soybeans using the described saponification and HPLC analytical method was validated against existing methods. This method offers a more efficient alternative to individual methods for quantifying lutein, tocopherols and sterols in soybeans. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Simultaneous extraction and derivatization of amino acids and free fatty acids in meat products.

    Science.gov (United States)

    Leggio, Antonella; Belsito, Emilia Lucia; De Marco, Rosaria; Liguori, Angelo; Siciliano, Carlo; Spinella, Mariagiovanna

    2012-06-08

    In meat products the contents of free amino acids and free fatty acids are two important parameters used to establish their quality. These compounds play a very important role in defining the sensorial characteristics and acceptability of meat products. An innovative procedure for the measurement of free amino acid and fatty acid contents in meat and meat derivatives was developed. A single experiment can be performed in order to determine simultaneously the free amino acid and free fatty acid profiles. The analytes of interest are rapidly extracted from the meat matrix and derivatized by using methyl chloroformate. This reagent allows the transformation of the two groups of analytes into the corresponding N-methyloxycarbonyl amino acid methyl esters and fatty acid methyl esters that can easily be extracted and sampled for their further identification and quantitation. The measurement of the obtained amino acid and fatty acid derivatives is performed by GC/MS analysis and their concentrations are calculated by using two appropriate internal standards. The main advantage of the proposed protocol is the determination at the same time of two important classes of analytes that are of great importance in food analysis and characterization. Moreover, minimal sample manipulation and preparation, and reduced total extraction times are required to obtain the response with respect to conventional procedures, in which instead the analysis of both the two classes of compounds must be performed separately. The helpfulness of the protocol was tested in the analysis of a cured meat product that is typical of the South of Italy. The optimized protocol successfully allowed the determination of thirteen free amino acids and six free fatty acids, namely those most abundant in the lipid content of the cured meat product under evaluation. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Transdermal Spray in Hormone Delivery | Algin-Yapar | Tropical ...

    African Journals Online (AJOL)

    This review examines advances in hormone delivery, particularly using transdermal spray. Transdermal gels, emulsions, patches, subcutaneous implants and sprays have been developed for transdermal hormone therapy in recent years. Transdermal sprays, in their general form of metered-dose transdermal spray, ...

  2. Source and Extraction for Simultaneous Four-hall Beam Delivery System at CEBAF

    Energy Technology Data Exchange (ETDEWEB)

    Kazimi, Reza; Wang, Haipeng; Spata, Mike F.; Hansknecht, John C.

    2013-06-01

    A new design for simultaneous delivery of the electron beam to all four 12 GeV CEBAF experimental halls* requires a new 750 MHz RF separator system in the 5th pass extraction region, a 250 MHz repetition rate for its beams, and addition of a fourth laser at the photo-cathode gun. The proposed system works in tandem with the existing 500 MHz RF separators and beam repetition rate on the lower passes. The new 5th pass RF separators will have the same basic design but modified to run at 750 MHz. The change to the beam repetition rate will be at the photo-cathode gun through an innovative upgrade of the seed laser driver system using electro-optic modulators. The new laser system also allows addition of the fourth laser. The new RF separators, the new laser system and other hardware changes required to implement the Four-Hall operation delivery system will be discussed in this paper.

  3. An integrated simultaneous distillation-extraction apparatus for the extraction of essential oils from herb materials and its application in Flos Magnoliae.

    Science.gov (United States)

    Wei, Yuhui; Li, Boxia; Duan, Haogang; Wu, Xin'an; Yao, Xiaojun

    2010-03-01

    A large number of herb materials contain essential oils with extensive bioactivities. In this work, an integrated simultaneous distillation-extraction (ISDE) apparatus was developed. To demonstrate its feasibility, the performance of ISDE was evaluated for the extraction of essential oil from Flos Magnoliae and compared with conventional techniques including steam distillation (SD) and simultaneous distillation-extraction (SDE). According to the product yield, the time consumed and the composition of oil, the essential oils isolated by ISDE were better than that obtained by SD and similar to those obtained by SDE. ISDE was also better than SDE due to its simple operation and lower consumption of energy and organic solvent. 2009 John Wiley & Sons, Ltd.

  4. Simultaneous spectrophotometric determination of synthetic dyes in food samples after cloud point extraction using multiple response optimizations.

    Science.gov (United States)

    Heidarizadi, Elham; Tabaraki, Reza

    2016-01-01

    A sensitive cloud point extraction method for simultaneous determination of trace amounts of sunset yellow (SY), allura red (AR) and brilliant blue (BB) by spectrophotometry was developed. Experimental parameters such as Triton X-100 concentration, KCl concentration and initial pH on extraction efficiency of dyes were optimized using response surface methodology (RSM) with a Doehlert design. Experimental data were evaluated by applying RSM integrating a desirability function approach. The optimum condition for extraction efficiency of SY, AR and BB simultaneously were: Triton X-100 concentration 0.0635 mol L(-1), KCl concentration 0.11 mol L(-1) and pH 4 with maximum overall desirability D of 0.95. Correspondingly, the maximum extraction efficiency of SY, AR and BB were 100%, 92.23% and 95.69%, respectively. At optimal conditions, extraction efficiencies were 99.8%, 92.48% and 95.96% for SY, AR and BB, respectively. These values were only 0.2%, 0.25% and 0.27% different from the predicted values, suggesting that the desirability function approach with RSM was a useful technique for simultaneously dye extraction. Linear calibration curves were obtained in the range of 0.02-4 for SY, 0.025-2.5 for AR and 0.02-4 μg mL(-1) for BB under optimum condition. Detection limit based on three times the standard deviation of the blank (3Sb) was 0.009, 0.01 and 0.007 μg mL(-1) (n=10) for SY, AR and BB, respectively. The method was successfully used for the simultaneous determination of the dyes in different food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. TRANSDERMAL DRUG DELIVERY SYSTEMS: AN OVERVIEW

    OpenAIRE

    Ahmed, Azhar; Karki, Nirmal; Charde, Rita; Charde, Manoj; Gandhare, Bhushan

    2010-01-01

    With the advent of modern era of pharmaceutical dosage forms, transdermal drug delivery system (TDDS) established itself as an integral part of novel drug delivery systems. Transdermal patches are polymeric formulations which when applied to skin deliver the drug at a predetermined rate across dermis to achieve systemic effects. Transdermal dosage forms, though a costly alternative to conventional formulations, are becoming popular because of their unique advantages. Controlled absorption, mo...

  6. Carbon coated magnetic nanoparticles as a novel magnetic solid phase extraction adsorbent for simultaneous extraction of methamphetamine and ephedrine from urine samples.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed

    2017-01-15

    This paper develops a highly selective, specific and efficient method for simultaneous determination of ephedrine and methamphetamine by a new carbon coated magnetic nanoparticles (C/MNPs) as a magnetic solid phase extraction (MSPE) adsorbent in biological urine medium. The characterization of synthesized magnetic nano adsorbent was completely carried out by various characterization techniques like Fourier transform infrared (FT-IR) spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Nine important parameters influencing extraction efficiency including amount of adsorbent, amounts of sample volume, pH, type and amount of extraction organic solvent, time of extraction and desorption, agitation rate and ionic strength of extraction medium, were studied and optimized. Under optimized extraction conditions, a good linearity was observed in the concentration range of 100-2000ng/mL for ephedrine and 100-2500ng/mL for methamphetamine. Analysis of positive urine samples was carried out by proposed method with the recovery of 98.71 and 97.87% for ephedrine and methamphetamine, respectively. The results indicated that carbon coated magnetic nanoparticles could be applied in clinical and forensic laboratories for simultaneous determination of abused drugs in urine media. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Micelle mediated extraction and simultaneous spectrophotometric determination of vanadium(V) and molybdenum(VI) in plant foodstuff samples.

    Science.gov (United States)

    Madrakian, Tayyebeh; Afkhami, Abbas; Siri, Reza; Mohammadnejad, Masoumeh

    2011-07-15

    A micelle-mediated extraction method for preconcentration of trace quantities of V(V) and Mo(VI) as a prior step to their simultaneous spectrophotometric determination has been developed. Bromopyrogallol red, cetyltrimethylammonium bromide (CTAB) (cationic surfactant) and KI were used as chelating, extraction and co-extraction agents, respectively. Mean centering (MC) of ratio spectra has been used for the simultaneous analysis of these metal ions. The optimal reaction and extraction conditions were optimised and the analytical characteristics of the method (e.g., limit of detection, linear range, maximum preconcentration and improvement factor) were obtained. Linearity was obeyed in the range 3.0-50.0ngmL(-1) for V(V) and Mo(VI). The detection limit of the method was 0.5 and 1.0ngmL(-1) for V(V) and Mo(VI), respectively. The method was applied to the simultaneous determination of V(V) and Mo(VI) in several plant foodstuff samples successfully. Copyright © 2011 Elsevier Ltd. All rights reserved.

  8. [Design of transdermal ultrasonophoresis equipment].

    Science.gov (United States)

    Li, Liangcheng; Zhang, Yongshun; Li, Zhonghong

    2009-02-01

    The recent fast development in biotechnology has resulted in a large number of therapeutic biologicals coming in the foreground for clinical application. Transdermal drug delivery (TDD) is designed for patching the drug on the skin, and then the drug molecules permeate through the skin into the subcutaneous capillary vessels. However,very few drugs can be administered transdermally at the therapeutic levels to pass through the barrier of stratum corneum. Several physical and chemical methods are applied to improve the permeability of skin. Research result shows that the low-frequency ultrasonic technique can extraordinarily increase the rate of permeation. As a result, it is becoming one of the potential methods that serve as the substitutes for traditional methods. In this paper is presented a type of equipment based on MSP430. The principle of design, the structure of hardware, and the applied function in this area are described.

  9. Simultaneous extraction, identification and quantification of phenolic compounds in Eclipta prostrata using microwave-assisted extraction combined with HPLC-DAD-ESI-MS/MS.

    Science.gov (United States)

    Fang, Xinsheng; Wang, Jianhua; Hao, Jifu; Li, Xueke; Guo, Ning

    2015-12-01

    A simple and rapid method was developed using microwave-assisted extraction (MAE) combined with HPLC-DAD-ESI-MS/MS for the simultaneous extraction, identification, and quantification of phenolic compounds in Eclipta prostrata, a common herb and vegetable in China. The optimized parameters of MAE were: employing 50% ethanol as solvent, microwave power 400 W, temperature 70 °C, ratio of liquid/solid 30 mL/g and extraction time 2 min. Compared to conventional extraction methods, the optimized MAE can avoid the degradation of the phenolic compounds and simultaneously obtained the highest yields of all components faster with less consumption of solvent and energy. Six phenolic acids, six flavonoid glycosides and one coumarin were firstly identified. The phenolic compounds were quantified by HPLC-DAD with good linearity, precision, and accuracy. The extract obtained by MAE showed significant antioxidant activity. The proposed method provides a valuable and green analytical methodology for the investigation of phenolic components in natural plants. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Chemical Penetration Enhancers for Transdermal Drug Delivery ...

    African Journals Online (AJOL)

    for transdermal administration. The permeation of drug through skin can be enhanced by both chemical penetration enhancement and physical methods. In this review, we have discussed the chemical penetration enhancement technology for transdermal drug delivery as well as the probable mechanisms of action.

  11. [Effects of Frankincense and Myrrh essential oil on transdermal absorption in vitro of Chuanxiong and penetration mechanism of skin blood flow].

    Science.gov (United States)

    Zhu, Xiao-Fang; Luo, Jing; Guan, Yong-Mei; Yu, Ya-Ting; Jin, Chen; Zhu, Wei-Feng; Liu, Hong-Ning

    2017-02-01

    The aim of this paper was to explore the effects of Frankincense and Myrrh essential oil on transdermal absorption in vitro of Chuanxiong, and to investigate the possible penetration mechanism of their essential oil from the perspective of skin blood perfusion changes. Transdermal tests were performed in vitro with excised mice skin by improved Franz diffusion cells. The cumulative penetration amounts of ferulic acid in Chuanxiong were determined by HPLC to investigate the effects of Frankincense and Myrrh essential oil on transdermal permeation properties of Chuanxiong. Simultaneously, the skin blood flows were determined by laser flow doppler. The results showed that the cumulative penetration amount of ferulic acid in Chuanxiong was (8.13±0.76) μg•cm⁻² in 24 h, and was (48.91±4.87), (57.80±2.86), (63.34±4.56), (54.17±4.40), (62.52±7.79) μg•cm⁻² respectively in Azone group, Frankincense essential oil group, Myrrh essential oil, frankincense and myrrh singly extracted essential oil mixture group, and frankincense and myrrh mixed extraction essential oil group. The enhancement ratios of each essential oil groups were 7.68, 8.26, 7.26, 8.28, which were slightly greater than 6.55 in Azone group. In addition, as compared with the conditions before treatment, there were significant differences and obvious increasing trend in blood flow of rats in Frankincense essential oil group, Myrrh essential oil group, frankincense and myrrh singly extracted essential oil mixture group, and frankincense and myrrh mixed extraction essential oil group when were dosed at 10, 20, 30, 10 min respectively, indicating that the skin blood flows were increased under the effects of Frankincense and Myrrh essential oil to a certain extent. Thus, Frankincense and Myrrh essential oil had certain effect on promoting permeability of Chuanxiong both before and after drug combination, and may promote the elimination of drugs from epidermis to dermal capillaries through increase of

  12. Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction.

    Science.gov (United States)

    Li, FuKai; Gong, AiJun; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

    2017-01-01

    The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N', N'-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4-1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.

  13. Simultaneous extraction, optimization, and analysis of flavonoids and polyphenols from peach and pumpkin extracts using a TLC-densitometric method.

    Science.gov (United States)

    Altemimi, Ammar; Watson, Dennis G; Kinsel, Mary; Lightfoot, David A

    2015-01-01

    The use of medicinal plants has been reported throughout human history. In the fight against illnesses, medicinal plants represent the primary health care system for 60 % of the world's population. Flavonoids are polyphenolic compounds with active anti-microbial properties; they are produced in plants as pigments. Quercetin, myricetin, and rutin are among the most well-known and prevalent flavonoids in plants, with an antioxidant activity capable of decreasing the oxidation of low density lipoproteins [LDLs]. To date, this research is the first of its kind to employ a coupled thin-layer chromatography (TLC) and a densitometric quantification method with a Box-Behnken design (BBD) response surface methodology (RSM) for optimization of ultrasonic-assisted extraction and determination of rutin and quercetin from peach and ellagic acid and myricetin from pumpkin fruits. The effect of process variables (extraction temperature (°C), extraction power (%) and extraction time (min)) on ultrasound-assisted extraction (UAE) were examined by using BBD and RSM. TLC followed by Quantity-One™ (BioRad) image analysis as a simple and rapid method was used for identification and quantification of the compounds in complex mixtures. The results were consistent under optimal conditions among the experimental values and their predicted values. A mass spectrometry (MALDI-TOF MS) technique was also used to confirm the identity of the natural products in the TLC spots resolved. The results show that the coupled TLC-densitometric methods & BBD can be a very powerful approach to qualitative and quantitative analysis of; rutin and quercetin from peach extracts; and ellagic acid and myricetin contents from pumpkin extracts.

  14. Microneedles for Transdermal Biosensing: Current Picture and Future Direction.

    Science.gov (United States)

    Ventrelli, Letizia; Marsilio Strambini, Lucanos; Barillaro, Giuseppe

    2015-12-09

    A novel trend is rapidly emerging in the use of microneedles, which are a miniaturized replica of hypodermic needles with length-scales of hundreds of micrometers, aimed at the transdermal biosensing of analytes of clinical interest, e.g., glucose, biomarkers, and others. Transdermal biosensing via microneedles offers remarkable opportunities for moving biosensing technologies and biochips from research laboratories to real-field applications, and envisages easy-to-use point-of-care microdevices with pain-free, minimally invasive, and minimal-training features that are very attractive for both developed and emerging countries. In addition to this, microneedles for transdermal biosensing offer a unique possibility for the development of biochips provided with end-effectors for their interaction with the biological system under investigation. Direct and efficient collection of the biological sample to be analyzed will then become feasible in situ at the same length-scale of the other biochip components by minimally trained personnel and in a minimally invasive fashion. This would eliminate the need for blood extraction using hypodermic needles and reduce, in turn, related problems, such as patient infections, sample contaminations, analysis artifacts, etc. The aim here is to provide a thorough and critical analysis of state-of-the-art developments in this novel research trend, and to bridge the gap between microneedles and biosensors. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Verification of the Simultaneous Local Extraction Method of Base and Thermal Resistance of Bipolar Transistors

    OpenAIRE

    Robert Setekera; Luuk Tiemeijer; Ramses van der Toorn

    2014-01-01

    In this paper an extensive verification of the extraction method (published earlier) that consistently accounts for self-heating and Early effect to accurately extract both base and thermal resistance of bipolar junction transistors is presented. The method verification is demonstrated on advanced RF SiGe HBTs were the extracted results for the thermal resistance are compared with those from another published method that ignores the effect of Early effect on internal base...

  16. Comparison of micro-scale simultaneous distillation-extraction and stir bar sorptive extraction for the determination of volatile organic constituents of grape juice.

    Science.gov (United States)

    Caven-Quantrill, Darren J; Buglass, Alan J

    2006-06-09

    Traditional micro-scale simultaneous distillation-extraction (SDE) and stir bar sorptive extraction (SBSE) were compared for their effectiveness in the extraction of volatile organic compounds in a synthetic grape juice and a real grape juice (Huxelrebe, a variety of half Muscat ancestry) from an English vineyard. The novel immersion-mode SBSE method, using stir bars with PDMS sorbent, was optimised using the synthetic grape juice. Although mean percent relative recoveries and reproducibilities (%CV) of the SBSE method were inferior to SDE (28.4 and 8.5%, respectively, against 86.9 and 6.3%), the former method proved to be significantly more sensitive: 126 aroma compounds in Huxelrebe grape juice were identified using SBSE, against 98 using SDE. This allowed the identification of a number of volatile components that have not been reported previously in the juice or wine from the grapes of Muscat varieties.

  17. Simultaneous preconcentration of a wide variety of organic pollutants in water samples. Comparison of stir bar sorptive extraction and membrane-assisted solvent extraction.

    Science.gov (United States)

    Prieto, A; Telleria, O; Etxebarria, N; Fernández, L A; Usobiaga, A; Zuloaga, O

    2008-12-19

    Stir bar soptive extraction (SBSE) coupled to thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) and membrane-assisted solvent extraction (MASE) coupled to large volume injection-programmed temperature vaporisation-GC-MS (LVI-PTV-GC-MS) were optimised for the simultaneous determination of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), nonylphenols (NPs), polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) in water samples. In the case of SBSE-TD, variables affecting the extraction (extraction time, addition of sodium chloride or methanol and sample volume) and desorption (cryofocusing temperature, desorption time and temperature, vent pressure and desorption flow) were fitted for the simultaneous determination. The extraction solvent nature (n-hexane, cyclohexane, n-heptane, ethyl acetate, toluene, dichloromethane or cyclohexane:ethyl acetate mixtures), as well as the addition of methanol (0-30%) and sodium chloride (0-20%), the extraction temperature (30-60 degrees C), shaking speed (250-750 rpm) and extraction time (5-150 min) were studied for the simultaneous membrane-assisted preconcentration. Finally, PTV-LVI variables such as injection volume (100-600 microL), injection speed (10-40 microL s(-1)), vent pressure (0-12.7 psi), vent time (0.05-0.8 min), vent flow (30-80 mL min(-1)), cryofocusing temperature (20-70 degrees C), split flow (20-100 mL min(-1)) and split time (1-5 min) were optimised. The optimisation was carried out by means of experimental design approaches in most of the cases. Precision (approximately 3-19% for both SBSE-TD and MASE-LVI-PTV), accuracy (approximately 80-120% for both SBSE-TD and MASE-LVI-PTV), limits of detection (LoDs) (0.1-222 ng L(-1) for MASE-LVI-PTV and 0.03-20.4 ng L(-1) for SBSE-TD in dependence of substance) and linearity (from 25 ng L(-1) up to at least 500 ng L(-1) for both procedures) were established for both procedures. Finally

  18. Developing a new micro cloud point extraction method for simultaneous preconcentration and spectrophotometric determination of uranium and vanadium in brine.

    Science.gov (United States)

    Ghasemi, Elham; Kaykhaii, Massoud

    2015-01-01

    A fast, simple, and economical method was developed for simultaneous spectrophotometric determination of uranium(VI) and vanadium(V) in water samples based on micro cloud point extraction (MCPE) at room temperature. This is the first report on the simultaneous extraction and determination of U(VI) and V(V). In this method, Triton X114 was employed as a non-ionic surfactant for the cloud point procedure and 4-(2-pyridylazo) resorcinol (PAR) was used as the chelating agent for both analytes. To reach the cloud point at room temperature, the MCPE procedure was carried out in brine. The factors influencing the extraction efficiency were investigated and optimized. Under the optimized condition, the linear calibration curve was found to be in the concentration range between 100 - 750 and 50 - 600 μg L(-1) for U(VI) and V(V), respectively, with a limit of detection of 17.03 μg L(-1) (U) and 5.51 μg L(-1) (V). Total analysis time including microextraction was less than 5 min.

  19. Transdermal optogenetic peripheral nerve stimulation

    Science.gov (United States)

    Maimon, Benjamin E.; Zorzos, Anthony N.; Bendell, Rhys; Harding, Alexander; Fahmi, Mina; Srinivasan, Shriya; Calvaresi, Peter; Herr, Hugh M.

    2017-06-01

    Objective: A fundamental limitation in both the scientific utility and clinical translation of peripheral nerve optogenetic technologies is the optical inaccessibility of the target nerve due to the significant scattering and absorption of light in biological tissues. To date, illuminating deep nerve targets has required implantable optical sources, including fiber-optic and LED-based systems, both of which have significant drawbacks. Approach: Here we report an alternative approach involving transdermal illumination. Utilizing an intramuscular injection of ultra-high concentration AAV6-hSyn-ChR2-EYFP in rats. Main results: We demonstrate transdermal stimulation of motor nerves at 4.4 mm and 1.9 mm depth with an incident laser power of 160 mW and 10 mW, respectively. Furthermore, we employ this technique to accurately control ankle position by modulating laser power or position on the skin surface. Significance: These results have the potential to enable future scientific optogenetic studies of pathologies implicated in the peripheral nervous system for awake, freely-moving animals, as well as a basis for future clinical studies.

  20. Microneedles for transdermal drug delivery.

    Science.gov (United States)

    Prausnitz, Mark R

    2004-03-27

    The success of transdermal drug delivery has been severely limited by the inability of most drugs to enter the skin at therapeutically useful rates. Recently, the use of micron-scale needles in increasing skin permeability has been proposed and shown to dramatically increase transdermal delivery, especially for macromolecules. Using the tools of the microelectronics industry, microneedles have been fabricated with a range of sizes, shapes and materials. Most drug delivery studies have emphasized solid microneedles, which have been shown to increase skin permeability to a broad range of molecules and nanoparticles in vitro. In vivo studies have demonstrated delivery of oligonucleotides, reduction of blood glucose level by insulin, and induction of immune responses from protein and DNA vaccines. For these studies, needle arrays have been used to pierce holes into skin to increase transport by diffusion or iontophoresis or as drug carriers that release drug into the skin from a microneedle surface coating. Hollow microneedles have also been developed and shown to microinject insulin to diabetic rats. To address practical applications of microneedles, the ratio of microneedle fracture force to skin insertion force (i.e. margin of safety) was found to be optimal for needles with small tip radius and large wall thickness. Microneedles inserted into the skin of human subjects were reported as painless. Together, these results suggest that microneedles represent a promising technology to deliver therapeutic compounds into the skin for a range of possible applications.

  1. Technical note: Characterization of key volatile odorants in rabbit meat using gas chromatography mass spectrometry with simultaneous distillation extraction

    Directory of Open Access Journals (Sweden)

    Y.J. Xie

    2016-12-01

    Full Text Available This study explored the key volatile compounds in both male and female rabbit meat. Simultaneous distillation extraction with dichloromethane was adopted to extract the volatile compounds in Hyla rabbit meat. A total of 35 volatile compounds were identified by gas chromatography–mass spectrometry and quantified with 2, 4, 6-thimethylpyridine as internal standard. Seventeen volatile aldehydes, 4 alcohols, 2 ketones, 2 acids, 1 heterocyclic compound, 2 alkanes and 7 esters were detected. Hexanal, heptanal, octanal, nonanal, (E, E-2, 4-decadienal, 1-octen-3-ol and (Z-2-decenal were the key odorant compounds, with high relative odour activity value. Furthermore, the concentration of volatile compounds in male rabbit meat was higher than that in female rabbit meat.

  2. Simultaneous extraction of oil and antioxidant compounds from oil palm fruit (Elaeis guineensis) by an aqueous enzymatic process.

    Science.gov (United States)

    Teixeira, Camilo B; Macedo, Gabriela A; Macedo, Juliana A; da Silva, Luiza Helena M; da C Rodrigues, Antonio Manoel

    2013-02-01

    Oil palm (Elaeis guineensis) fruit was treated with enzymes to facilitate simultaneous recovery of oil and bioactive compounds. Tannase from Paecilomyces variotii, cellulase and pectinase were evaluated for their influence on oil recovery and antioxidant capacity (DPPH), oxidative stability (Rancimat), fatty acid profile, total phenols, total carotenoids and tocols of the oil. Maximum oil recovery (90-93% total oil) was obtained with central composite design using 4% of enzyme preparation (w/w) as 80 U of tannase, 240 U of cellulase and 178 U of pectinase, pH 4, ratio of solution to pulp of 2:1 and 30 min of incubation at 50 °C. Tannase improved the phenolic compounds extraction by 51% and pectinase plus cellulase improved carotene extraction by 153%. Samples treated with tannase showed a 27% and 53% higher antioxidant capacity for the lipophilic and hydrophilic fractions. Copyright © 2012 Elsevier Ltd. All rights reserved.

  3. Short Communication An efficient method for simultaneous extraction of high-quality RNA and DNA from various plant tissues.

    Science.gov (United States)

    Oliveira, R R; Viana, A J C; Reátegui, A C E; Vincentz, M G A

    2015-12-29

    Determination of gene expression is an important tool to study biological processes and relies on the quality of the extracted RNA. Changes in gene expression profiles may be directly related to mutations in regulatory DNA sequences or alterations in DNA cytosine methylation, which is an epigenetic mark. Correlation of gene expression with DNA sequence or epigenetic mark polymorphism is often desirable; for this, a robust protocol to isolate high-quality RNA and DNA simultaneously from the same sample is required. Although commercial kits and protocols are available, they are mainly optimized for animal tissues and, in general, restricted to RNA or DNA extraction, not both. In the present study, we describe an efficient and accessible method to extract both RNA and DNA simultaneously from the same sample of various plant tissues, using small amounts of starting material. The protocol was efficient in the extraction of high-quality nucleic acids from several Arabidopsis thaliana tissues (e.g., leaf, inflorescence stem, flower, fruit, cotyledon, seedlings, root, and embryo) and from other tissues of non-model plants, such as Avicennia schaueriana (Acanthaceae), Theobroma cacao (Malvaceae), Paspalum notatum (Poaceae), and Sorghum bicolor (Poaceae). The obtained nucleic acids were used as templates for downstream analyses, such as mRNA sequencing, quantitative real time-polymerase chain reaction, bisulfite treatment, and others; the results were comparable to those obtained with commercial kits. We believe that this protocol could be applied to a broad range of plant species, help avoid technical and sampling biases, and facilitate several RNA- and DNA-dependent analyses.

  4. Simultaneous control of apparent extract and volatile compounds concentrations in low-malt beer fermentation.

    Science.gov (United States)

    Kobayashi, Michiko; Nagahisa, Keisuke; Shimizu, Hiroshi; Shioya, Suteaki

    2006-12-01

    Volatile compounds cause undesirable flavor when their concentrations exceed threshold values in beer fermentation. The objective of this study is to develop a system for controlling apparent extract concentration, which indicates the fermentation degree and which should be decreased below a targeted value at a fixed time under a constraint of tolerable amounts of volatile compounds. In beer fermentation, even though the production of volatile compounds is suppressed by maintaining a low fermentation temperature, a low temperature causes a delay in the control of apparent extract concentration. Volatile compound concentration was estimated on-line, and the simulation of apparent extract consumption and volatile compound production was performed. To formulate various beer tastes and conserve energy for attemperation, optimal temperature profiles were determined using a genetic algorithm (GA). The developed feedback control of the brewing temperature profile was successfully applied, and apparent extract and volatile compound concentrations at a fixed time reached their target concentrations. Additionally, the control technique developed in this study enables us to brew a wide variety of beers with different tastes.

  5. Simultaneous extraction of trace organophosphorous pesticides from plasma sample by automated solid phase extraction and determination by gas chromatography coupled with pulsed flame photometric detector.

    Science.gov (United States)

    Wang, Yuanfeng; Du, Ran

    2010-05-20

    The purpose of our work was to develop a simple and efficient analytical method for simultaneous determination of different species of organic phosphorus pesticides from plasma sample by using automated solid phase extraction (SPE) and gas chromatography/pulsed flame photometric detector (GC/PFPD) as a diagnostic tool. Firstly, the developed extraction method was validated using 5 certified reference materials; then, it was applied to plasma sample. Such factors as the category and volume of wash and elution solvent were examined separately. Among these factors, the category of elution solvent is most important. Hexane-acetone (50:50, v/v) seems to be the best choice for it. The eluent was evaporated on a nitrogen stream at room temperature and redissolved by acetone. 1microL of aliquots was chromatographed on GC/PFPD. Response versus the amount of pesticides injected ranging from 0.05 to 2ng showed a good linearity. The detection limits were 0.01ng for dimethoate, 0.03ng for methyl-parathion and malathion, 0.04ng for terbufos and 0.02ng for parathion. Extraction recoveries range from 84.3% to 109.1%.This extraction method for multispecies analysis incorporates many benefits in terms of speed, low solvent use, accuracy of measurement, sensitivity, relative simplicity, as well as the time saving and convenience of multiple species measurement through sample preparation and analysis as an integrated step.

  6. Combination of electromembrane extraction and liquid-phase microextraction in a single step: Simultaneous group separation of acidic and basic drugs

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid

    2015-01-01

    Electromembrane extraction (EME) and liquid-phase microextraction (LPME) were combined in a single step for the first time to realize simultaneous and clear group separation of basic and acidic drugs. Using 2-nitrophenyl octyl ether as the supported liquid membrane (SLM) for EME and dihexyl ether...... as the SLM for LPME, basic and acidic drugs were extracted and separated simultaneously from a low pH sample by EME and LPME, respectively. After 15 min of extraction, basic drugs (citalopram and sertraline) were exhaustively extracted, whereas the recoveries for acidic drugs (ketoprofen and ibuprofen) were...... in the range of 76%-86%. Longer extraction time provided higher recoveries for the acidic drugs, but this somewhat deteriorated the group separation. Matrices effects from the coexisting acidic drugs/basic drugs were tested, and we observed that simultaneous EME/LPME was not affected by coexisting drugs...

  7. Fundamental Chemistry of the Universal Extractant (UNEX) for the Simultaneous Separation of Major Radionuclides (Cesium, Strontium, Actinides, and Lanthanides) from Radioactive Wastes

    Energy Technology Data Exchange (ETDEWEB)

    Herbst, R. Scott; Peterman, Dean R.; Luther, Thomas A.; Garn, Troy G.; Tillotson, Richard D.; Babain, Vasily A.; Smirnov, Igor V.; Stoyanov, Evgenii S.

    2004-03-28

    4 Scientists at the INEEL and KRI collaboratively developed and validated the concept of a Universal Extractant (UNEX) for simultaneously removing the major radionuclides (Cs, Sr, actinides and lanthanides) from acidic radioactive waste in a single solvent extraction process. The UNEX solvent incorporates three active extractants: chlorinated cobalt dicarbollide, polyethylene glycol and a carbamoylmethylphosphine oxide derivative, dissolved in a suitable organic diluent to simultaneously extract target radionuclides. The process chemistry is unique, but complicated, since the extractants operate synergistically to extract the radionuclides. Results indicate that water dissolved in the organic phase dramatically impacts the process chemistry. In order to investigate this phenomenon, we have varied the amount of water dissolved in the organic phase by using several different organic diluents. The results of 137Cs and 89Sr batch distribution studies for the different organic diluents will be presented. These data and data from other spectroscopic techniques will be used to elucidate the details of the extraction mechanism.

  8. A Transdermal Measurement Platform Based on Microfluidics

    Directory of Open Access Journals (Sweden)

    Wen-Ying Huang

    2017-01-01

    Full Text Available The Franz diffusion cell is one of the most widely used devices to evaluate transdermal drug delivery. However, this static and nonflowing system has some limitations, such as a relatively large solution volume and skin area and the development of gas bubbles during sampling. To overcome these disadvantages, this study provides a proof of concept for miniaturizing models of transdermal delivery by using a microfluidic chip combined with a diffusion cell. The proposed diffusion microchip system requires only 80 μL of sample solution and provides flow circulation. Two model compounds, Coomassie Brilliant Blue G-250 and potassium ferricyanide, were successfully tested for transdermal delivery experiments. The diffusion rate is high for a high sample concentration or a large membrane pore size. The developed diffusion microchip system, which is feasible, can be applied for transdermal measurement in the future.

  9. Optimisation and validation of analytical methods for the simultaneous extraction of antioxidants: application to the analysis of tomato sauces.

    Science.gov (United States)

    Motilva, Maria-José; Macià, Alba; Romero, Maria-Paz; Labrador, Agustín; Domínguez, Alba; Peiró, Lluís

    2014-11-15

    In the present study, simultaneous extraction of natural antioxidants (phenols and carotenoids) in complex matrices, such as tomato sauces, is presented. The tomato sauce antioxidant compounds studied were the phenolics hydroxytyrosol, from virgin olive oil, quercetin and its derivatives, from onions, and quercetin-rutinoside as well as the carotenoid, lycopene (cis and trans), from tomatoes. These antioxidant compounds were extracted simultaneously with n-hexane/acetone/ethanol (50/25/25, v/v/v). The phenolics were analysed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS), and lycopene (cis- and trans-forms) was analysed using high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD). After studying the parameters of these methods, they were applied to the analysis of virgin olive oil, fresh onion, tomato concentrate and tomato powder, and commercial five tomato sauces. Subsequently, the results obtained in our laboratory were compared with those from the Gallina Blanca Star Group laboratory. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Myth or Reality?Transdermal Magnesium?

    OpenAIRE

    Gr?ber, Uwe; Werner, Tanja; Vormann, J?rgen; Kisters, Klaus

    2017-01-01

    In the following review, we evaluated the current literature and evidence-based data on transdermal magnesium application and show that the propagation of transdermal magnesium is scientifically unsupported. The importance of magnesium and the positive effects of magnesium supplementation are extensively documented in magnesium deficiency, e.g., cardiovascular disease and diabetes mellitus. The effectiveness of oral magnesium supplementation for the treatment of magnesium deficiency has been ...

  11. Simultaneous Extraction and Depolymerization of Fucoidan from Sargassum muticum in Aqueous Media

    Directory of Open Access Journals (Sweden)

    Elena M. Balboa

    2013-11-01

    Full Text Available The biomass components of the invasive seaweed Sargassum muticum were fractionated to allow their separate valorization. S. muticum (Sm and the solid residue remaining after alginate extraction of this seaweed (AESm were processed with hot, compressed water (hydrothermal processing to assess the effects of temperature on fucoidan solubilization. Fucose-containing oligosaccharides were identified as reaction products. Operating under optimal conditions (170 °C, up to 62 and 85 wt% of the dry mass of Sm and AESm were solubilized, respectively. The reaction media were subjected to precipitation, nanofiltration and freeze-drying. The dried products contained 50% and 85% of the fucoidan present in Sm and AESm, respectively; together with other components such as phenolics and inorganic components. The saccharidic fraction, accounting for up to 35% of the dried extracts, contained fucose as the main sugar, and also galactose, xylose, glucose and mannose. The concentrates were characterized for antioxidant activity using the TEAC assay.

  12. Simultaneous extraction of roads and buildings in remote sensing imagery with convolutional neural networks

    Science.gov (United States)

    Alshehhi, Rasha; Marpu, Prashanth Reddy; Woon, Wei Lee; Mura, Mauro Dalla

    2017-08-01

    Extraction of man-made objects (e.g., roads and buildings) from remotely sensed imagery plays an important role in many urban applications (e.g., urban land use and land cover assessment, updating geographical databases, change detection, etc). This task is normally difficult due to complex data in the form of heterogeneous appearance with large intra-class and lower inter-class variations. In this work, we propose a single patch-based Convolutional Neural Network (CNN) architecture for extraction of roads and buildings from high-resolution remote sensing data. Low-level features of roads and buildings (e.g., asymmetry and compactness) of adjacent regions are integrated with Convolutional Neural Network (CNN) features during the post-processing stage to improve the performance. Experiments are conducted on two challenging datasets of high-resolution images to demonstrate the performance of the proposed network architecture and the results are compared with other patch-based network architectures. The results demonstrate the validity and superior performance of the proposed network architecture for extracting roads and buildings in urban areas.

  13. Automated fast procedure for the simultaneous extraction of hair sample performed with an automated workstation.

    Science.gov (United States)

    Angeli, I; Minoli, M; Ravelli, A; Gigli, F; Lodi, F

    2012-05-10

    Hair testing has a leading role in toxicology practice and even more in those aspects tightly linked to the assessment of psychoactive drug use and abuse in social life. The objective of the present study was to develop and validate an automated SPE sample-preparation step, suited for GC/MS confirmation analysis of basic drugs in hair drug control. The method was studied and optimized for quantitative determination and in a second time it was extended to real hair samples. The purpose of method validation was to ensure good reliability, reproducibility and quickness. Janus Automated Workstation (PerkinElmer) was employed to perform SPE hair extraction, using 96-well plate SPEC MP1 acquired from Varian (Agilent Technologies). After derivatization of dried extracts, screening confirmations were performed using gas chromatography (GC) followed by mass spectrometry (MS). GC/MS data were validated following standard guidelines, but our attention was focused on three headings: samples cross-contamination, "memory effect" and extraction recovery. Validation requests were fully accomplished and we always obtained best results with the automated procedure. For instance, analytes mean recovery was between 70 and 90% and data analysis proved that no contamination between samples occurred. The automated workstation has shown good reliability (cross contamination and "memory effect" were tested and excluded), effectiveness (no false negative was detected), solvent saving (500μL/sample vs traditionally LLE 4mL/sample) and quickness (50min for 96 tests cycle). Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  14. Transdermal patches: history, development and pharmacology.

    Science.gov (United States)

    Pastore, Michael N; Kalia, Yogeshvar N; Horstmann, Michael; Roberts, Michael S

    2015-05-01

    Transdermal patches are now widely used as cosmetic, topical and transdermal delivery systems. These patches represent a key outcome from the growth in skin science, technology and expertise developed through trial and error, clinical observation and evidence-based studies that date back to the first existing human records. This review begins with the earliest topical therapies and traces topical delivery to the present-day transdermal patches, describing along the way the initial trials, devices and drug delivery systems that underpin current transdermal patches and their actives. This is followed by consideration of the evolution in the various patch designs and their limitations as well as requirements for actives to be used for transdermal delivery. The properties of and issues associated with the use of currently marketed products, such as variability, safety and regulatory aspects, are then described. The review concludes by examining future prospects for transdermal patches and drug delivery systems, such as the combination of active delivery systems with patches, minimally invasive microneedle patches and cutaneous solutions, including metered-dose systems. © 2015 The British Pharmacological Society.

  15. Optimization of simultaneous microwave/ultrasonic-assisted extraction of phenolic compounds from walnut flour using response surface methodology.

    Science.gov (United States)

    Luo, Yan; Wu, Wanxing; Chen, Dan; Lin, Yuping; Ma, Yage; Chen, Chaoyin; Zhao, Shenglan

    2017-12-01

    Walnut is a traditional food as well as a traditional medicine recorded in the Chinese Pharmacopoeia; however, the large amounts of walnut flour (WF) generated in walnut oil production have not been well utilized. This study maximized the total polyphenolic yield (TPY) from the walnut flour (WF) by optimizing simultaneous ultrasound/microwave-assisted hydroalcoholic extraction (SUMAE). Response surface methodology was used to optimize the processing parameters for the TPY, including microwave power (20-140 W), ultrasonic power (75-525 W), extraction temperature (25-55 °C), and time (0.5-9.5 min). The polyphenol components were analysed by LC-MS. A second-order polynomial model satisfactorily fit the experimental TPY data (R2 = 0.9932, P < 0.0001 and Radj2    = 0.9868). The optimized quick extraction conditions were microwave power 294.38 W, ultrasonic power 93.5 W, temperature 43.38 °C and time 4.33 min, with a maximum TPY of 34.91 mg GAE/g, which was a rapid extraction. The major phenolic components in the WF extracts were glansreginin A, ellagic acid, and gallic acid with peak areas of 22.15%, 14.99% and 10.96%, respectively, which might be used as functional components for health food, cosmetics and medicines. The results indicated that walnut flour, a waste product from the oil industry, was a rich source of polyphenolic compounds and thus could be used as a high-value functional food ingredient.

  16. Development and validation of a method for the simultaneous determination of 20 organophosphorus pesticide residues in corn by accelerated solvent extraction and gas chromatography with nitrogen phosphorus detection

    OpenAIRE

    Kostik, Vesna; Gjorgjeska, Biljana; Angelovska, Bistra

    2014-01-01

    The method for simultaneous determination of 20 organophosphorus pesticide residues in corn samples has been developed and validated. For the extraction of organophosporus pesticide residues from the samples, the accelerated solvent technique with the mixture of dichloromethane: acetone (1:1, V/V) was used. Clean up was done using liquid – liquid extraction with n – hexane, followed by solid phase extraction on primary secondary amine adsorbent, and elution with the mixture of acetone: toluen...

  17. Ionic-Liquid-Based Acidic Aqueous Biphasic Systems for Simultaneous Leaching and Extraction of Metallic Ions.

    Science.gov (United States)

    Gras, Matthieu; Papaiconomou, Nicolas; Schaeffer, Nicolas; Chainet, Eric; Tedjar, Farouk; Coutinho, Joao A P; Billard, Isabelle

    2017-11-27

    The first instance of an acidic aqueous biphasic system (AcABS) based on tributyltetradecyl phosphonium chloride ([P44414 ][Cl]) and an acid is here reported. This AcABS exhibits pronounced thermomorphic behavior and is shown to be applicable to the extraction of metal ions from concentrated acidic solutions. Metal ions such as cobalt(II), iron(III), platinum(IV) and nickel(II) are found to partition preferentially to one of the phases of the acidic aqueous biphasic system and it is here shown that it successfully allows the difficult separation of CoII from NiII , here studied at 24 and 50 °C. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Simultaneous derivative spectrophotometric determination of cobalt(II) and nickel(II) by dithizone without extraction.

    Science.gov (United States)

    Oztürk, B D; Filik, H; Tütem, E; Apak, R

    2000-10-02

    Dithizone (Dz), a common extractive-photometric ligand for Co(II) and Ni(II), has been dissolved in the water-miscible solvent tetrahydrofurane (THF) so as to constitute a reagent for both metals in aqueous phase without extraction. Complex formation was complete for both metals at pH 12.0 (adjusted by aqueous NH(3)) within 30 min, and the complexes were stable for at least 2 h. First-derivative spectra of the metal dithizonates (singly or as binary mixtures) were preferred to ordinary spectra, because working wavelength determination was more precise and spectral overlap was less. Two wavelengths at which the spectral overlap was minimum were selected as analytical wavelengths, i.e. 620 nm for Co and 740 nm for Ni, and the calibration curves drawn with zero-to-peak values as a function of concentration were linear for these wavelengths. Thus, the total (1)D values at 620 and 740 nm of the mixtures were used to determine Co and Ni concentrations. The relative standard deviation (R.S.D.) for the analysis of Co (3.0 mg l(-1)) individually was 3.5%, and for its admixture with Ni (3.5 mg l(-1)) was 2.5%. The R.S.D. for the analysis of Ni (5.9 mg l(-1)) individually and for its admixture with Co (1.8 mg l(-1)) were 5.5 and 5.8%, respectively. The linear range in (1)D evaluation was between 5.0x10(-6) and 1.0x10(-4) M for Co and 2.0x10(-5)-2.0x10(-4) M for Ni. Interference analysis was performed for individual metal (Co or Ni) determinations. Finally, the method has been applied to a Ni-Cr-based dental alloy (Wiron 99) successfully.

  19. A Microwave-Assisted Simultaneous Distillation and Extraction Method for the Separation of Polysaccharides and Essential Oil from the Leaves of Taxus chinensis Var. mairei

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2016-01-01

    Full Text Available An efficient microwave-assisted simultaneous distillation and extraction (MA-SDE method has been developed for the separation of polysaccharides and essential oil from Taxus chinensis var. mairei. The key operating parameters for MA-SDE were optimized by single factor and central composite design experiments, and the optimal conditions were found to include a particle size of 60–80 mesh, liquid/solid ratio of 22.5 mL/g, extraction time of 17.5 min, microwave power of 547 W, and dichloromethane was used as the extraction solvent of the essential oil. The yields obtained for polysaccharides and essential oil under the optimized conditions were 6.39% ± 0.12% and 0.27% ± 0.03%, respectively. The MA-SDE method was also compared with conventional heat reflux extraction (HRE and hydrodistillation extraction (HDE. The MA-SDE method not only allowed for the simultaneous extraction of polysaccharides and essential oil, but also completed the task with a much shorter extraction time of 17.5 min (HRE and HDE required 3 and 6 h, respectively. Furthermore, the MA-SDE method gave increased extraction yields for polysaccharides (1.14-fold higher than HRE and essential oil (1.23-fold higher than HDE. Based on these results, this MA-SDE method represents a rapid and efficient technique for the simultaneous extraction of polysaccharides and essential oil.

  20. Ultrasound-Assisted Extraction of Arabinogalactan and Dihydroquercetin Simultaneously from Larix gmelinii as a Pretreatment for Pulping and Papermaking

    Science.gov (United States)

    Ma, Chunhui; Yang, Lei; Li, Wei; Yue, Jinquan; Li, Jian; Zu, Yuangang

    2014-01-01

    An ultrasound-assisted extraction (UAE) method using ethanol was applied for extracting arabinogalactan (AG) and dihydroquercetin (DHQ) simultaneously from larch wood, as a pretreatment for pulping and papermaking. The extraction parameters were optimized by a Box-Behnken experimental design with the yields of AG and DHQ as the response values. Under optimum conditions (three extractions, each using 40% ethanol, for 50 min, 200 W ultrasound power and 1∶18 solid-liquid ratio), the yields of AG and DHQ were 183.4 and 36.76 mg/g, respectively. After UAE pretreated, the wood chips were used for Kraft pulping (KP) and high boiling solvent pulping (HBSP). The pulping yield after pretreatment was higher than that of untreated (the pulping yields of untreated HBSP and KP were 42.37% and 39.60%, and the pulping yields of HBSP and KP after UAE-pretreated were 44.23% and 41.50% respectively), as indicated by a lower kappa number (77.91 and 27.30 for untreated HBSP and KP; 77.01 and 26.83 for UAE-pretreated HBSP and KP). Furthermore, the characteristics of paper produced from pretreated wood chips were superior to those from the untreated chips: the basis weight was lower (85.67 and 82.48 g·cm−2 for paper from untreated KP and HBSP; 79.94 and 80.25 g·cm−2 for paper from UAE-pretreated KP and HBSP), and the tensile strengths, tearing strengths, bursting strengths, and folding strengths were higher than these of paper after UAE-pretreated, respectively. PMID:25460911

  1. Ultrasound-assisted extraction of arabinogalactan and dihydroquercetin simultaneously from Larix gmelinii as a pretreatment for pulping and papermaking.

    Science.gov (United States)

    Ma, Chunhui; Yang, Lei; Li, Wei; Yue, Jinquan; Li, Jian; Zu, Yuangang

    2014-01-01

    An ultrasound-assisted extraction (UAE) method using ethanol was applied for extracting arabinogalactan (AG) and dihydroquercetin (DHQ) simultaneously from larch wood, as a pretreatment for pulping and papermaking. The extraction parameters were optimized by a Box-Behnken experimental design with the yields of AG and DHQ as the response values. Under optimum conditions (three extractions, each using 40% ethanol, for 50 min, 200 W ultrasound power and 1∶18 solid-liquid ratio), the yields of AG and DHQ were 183.4 and 36.76 mg/g, respectively. After UAE pretreated, the wood chips were used for Kraft pulping (KP) and high boiling solvent pulping (HBSP). The pulping yield after pretreatment was higher than that of untreated (the pulping yields of untreated HBSP and KP were 42.37% and 39.60%, and the pulping yields of HBSP and KP after UAE-pretreated were 44.23% and 41.50% respectively), as indicated by a lower kappa number (77.91 and 27.30 for untreated HBSP and KP; 77.01 and 26.83 for UAE-pretreated HBSP and KP). Furthermore, the characteristics of paper produced from pretreated wood chips were superior to those from the untreated chips: the basis weight was lower (85.67 and 82.48 g·cm(-2) for paper from untreated KP and HBSP; 79.94 and 80.25 g·cm(-2) for paper from UAE-pretreated KP and HBSP), and the tensile strengths, tearing strengths, bursting strengths, and folding strengths were higher than these of paper after UAE-pretreated, respectively.

  2. Ultrasound-assisted extraction of arabinogalactan and dihydroquercetin simultaneously from Larix gmelinii as a pretreatment for pulping and papermaking.

    Directory of Open Access Journals (Sweden)

    Chunhui Ma

    Full Text Available An ultrasound-assisted extraction (UAE method using ethanol was applied for extracting arabinogalactan (AG and dihydroquercetin (DHQ simultaneously from larch wood, as a pretreatment for pulping and papermaking. The extraction parameters were optimized by a Box-Behnken experimental design with the yields of AG and DHQ as the response values. Under optimum conditions (three extractions, each using 40% ethanol, for 50 min, 200 W ultrasound power and 1∶18 solid-liquid ratio, the yields of AG and DHQ were 183.4 and 36.76 mg/g, respectively. After UAE pretreated, the wood chips were used for Kraft pulping (KP and high boiling solvent pulping (HBSP. The pulping yield after pretreatment was higher than that of untreated (the pulping yields of untreated HBSP and KP were 42.37% and 39.60%, and the pulping yields of HBSP and KP after UAE-pretreated were 44.23% and 41.50% respectively, as indicated by a lower kappa number (77.91 and 27.30 for untreated HBSP and KP; 77.01 and 26.83 for UAE-pretreated HBSP and KP. Furthermore, the characteristics of paper produced from pretreated wood chips were superior to those from the untreated chips: the basis weight was lower (85.67 and 82.48 g·cm(-2 for paper from untreated KP and HBSP; 79.94 and 80.25 g·cm(-2 for paper from UAE-pretreated KP and HBSP, and the tensile strengths, tearing strengths, bursting strengths, and folding strengths were higher than these of paper after UAE-pretreated, respectively.

  3. Simultaneous Distillation Extraction of Some Volatile Flavor Components from Pu-erh Tea Samples—Comparison with Steam Distillation-Liquid/Liquid Extraction and Soxhlet Extraction

    Science.gov (United States)

    Gu, Xungang; Zhang, Zhengzhu; Wan, Xiaochun; Ning, Jingming; Yao, Chengcheng; Shao, Wanfang

    2009-01-01

    A simutaneous distillation extraction (SDE) combined GC method was constructed for determination of volatile flavor components in Pu-erh tea samples. Dichloromethane and ethyl decylate was employed as organic phase in SDE and internal standard in determination, respectively. Weakly polar DB-5 column was used to separate the volatile flavor components in GC, 10 of the components were quantitatively analyzed, and further confirmed by GC-MS. The recovery covered from 66.4%–109%, and repeatability expressed as RSD was in range of 1.44%–12.6%. SDE was most suitable for the extraction of the anlytes by comparing with steam distillation-liquid/liquid extraction and Soxhlet extraction. Commercially available Pu-erh tea samples, including Pu-erh raw tea and ripe tea, were analyzed by the constructed method. the high-volatile components, such as benzyl alcohol, linalool oxide, and linalool, were greatly rich in Pu-erh raw teas, while the contents of 1,2,3-Trimethoxylbenzene and 1,2,4-Trimethoxylbenzene were much high in Pu-erh ripe teas. PMID:20169174

  4. Antibacterial and antioxidant activities and chemical compositions of volatile oils extracted from Schisandra chinensis Baill. seeds using simultaneous distillation extraction method, and comparison with Soxhlet and microwave-assisted extraction.

    Science.gov (United States)

    Teng, Hui; Lee, Won Y

    2014-01-01

    The volatile oils were isolated from dried Schisandra chinensis Baill. seeds by Soxhlet extraction (SE), microwave-assisted extraction (MAE), and simultaneous distillation extraction (SDE), and fractions were identified by gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography (HPLC). The essential oils were assessed for their antioxidant and antibacterial activities. GC-MS results also revealed that the major ingredients in the oil extracted by SDE were terpenoids compounds such as ylangene (15.01%), α-phellandrene (8.23%), β-himachalene (6.95%), and cuparene (6.74), and the oil extracts of MAE and SE mainly contained aromatics such as schizandrins, wuweizisu C, and gomisin A. HPLC analysis results confirmed that more schizandrin was obtained through extraction by MAE (996.64 μg/g) and SE (722.13 μg/g). SDE oil extract showed more significant antioxidant activity than MAE or SE oil. Only volatile oil from SDE showed good antibacterial activity against all tested strains.

  5. Hyaluronan-Based Nanohydrogels as Effective Carriers for Transdermal Delivery of Lipophilic Agents: Towards Transdermal Drug Administration in Neurological Disorders

    Directory of Open Access Journals (Sweden)

    Seong Uk Son

    2017-12-01

    Full Text Available We suggest a convenient nanoemulsion fabrication method to create hyaluronan (HA-based nanohydrogels for effective transdermal delivery. First, hyaluronan-conjugated dodecylamine (HA–Do HA-based polymers to load the lipophilic agents were synthesized with hyaluronan (HA and dodecylamine (Do by varying the substitution ratio of Do to HA. The synthetic yield of HA–Do was more than 80% (HA–Do (A: 82.7 ± 4.7%, HA–Do (B: 87.1 ± 3.9% and HA–Do (C: 81.4 ± 4.5%. Subsequently, nanohydrogels were fabricated using the nanoemulsion method. Indocyanine green (ICG simultaneously self-assembled with HA–Do, and the size depended on the substitution ratio of Do in HA–Do (nanohydrogel (A: 118.0 ± 2.2 nm, nanohydrogel (B: 121.9 ± 11.4 nm, and nanohydrogel (C: 142.2 ± 3.8 nm. The nanohydrogels were delivered into cells, and had excellent biocompatibility. Especially, nanohydrogel (A could deliver and permeate ICG into the deep skin layer, the dermis. This suggests that nanohydrogels can be potent transdermal delivery systems.

  6. Transdermal Photopolymerization for Minimally Invasive Implantation

    Science.gov (United States)

    Elisseeff, J.; Anseth, K.; Sims, D.; McIntosh, W.; Randolph, M.; Langer, R.

    1999-03-01

    Photopolymerizations are widely used in medicine to create polymer networks for use in applications such as bone restorations and coatings for artificial implants. These photopolymerizations occur by directly exposing materials to light in "open" environments such as the oral cavity or during invasive procedures such as surgery. We hypothesized that light, which penetrates tissue including skin, could cause a photopolymerization indirectly. Liquid materials then could be injected s.c. and solidified by exposing the exterior surface of the skin to light. To test this hypothesis, the penetration of UVA and visible light through skin was studied. Modeling predicted the feasibility of transdermal polymerization with only 2 min of light exposure required to photopolymerize an implant underneath human skin. To establish the validity of these modeling studies, transdermal photopolymerization first was applied to tissue engineering by using "injectable" cartilage as a model system. Polymer/chondrocyte constructs were injected s.c. and transdermally photopolymerized. Implants harvested at 2, 4, and 7 weeks demonstrated collagen and proteoglycan production and histology with tissue structure comparable to native neocartilage. To further examine this phenomenon and test the applicability of transdermal photopolymerization for drug release devices, albumin, a model protein, was released for 1 week from photopolymerized hydrogels. With further study, transdermal photpolymerization potentially could be used to create a variety of new, minimally invasive surgical procedures in applications ranging from plastic and orthopedic surgery to tissue engineering and drug delivery.

  7. Microemulsion liquid chromatographic method for simultaneous separation and determination of six flavonoids of Apocynum venetum leaf extract.

    Science.gov (United States)

    Song, Rui juan; Zhou, Jun

    2015-07-15

    A simple, cost-effective, and efficient method was developed for the rapid simultaneous separation and determination of six flavonoids (rutin, hyperoside, quercetin-3-O-sophoroside, isoquercitrin, astragalin and quercetin) of Apocynum venetum leaf extract by reversed phase high performance liquid chromatography using a microemulsion system mixture as the mobile phase. Separations were performed on the Zorbax Extend-C18 column with UV detection at 360nm. The flow rate was 0.8mLmin(-1). The optimized microemulsion mobile phase consisted of 2.5% (v/v) n-butanol, 1.2% (v/v) of Genapol X-080, 0.5% (v/v) ethyl acetate and 95.8% (w/v) of aqueous 20mM phosphoric acid, pH adjusted to 6.0 with 0.3% triethylamine. Under the optimized conditions, the calibration curve for six flavonoids was linear in the range of 5-1000μgmL(-1) with the correlation coefficients greater than 0.9994. The intra-day and inter-day precision (RSD) were below 8.11% and the limits of detection (LOD) for the six flavonoids were 1.7-6.0μgmL(-1) (S/N=3). The microemulsion liquid chromatography (MELC) method was successfully applied to separate and determine the six flavonoids of A. venetum leaf extract. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. [Simultaneous determination of madecassoside, asiaticoside and their aglycones in Centella asiatica (L.) urban extracts by RP-HPLC].

    Science.gov (United States)

    Shen, Qian; Yu, Lu-shan; Zhou, Hui; Zeng, Su

    2014-03-01

    To establish a HPLC method for simultaneous determination of four major constituents (madecassoside, asiaticoside, madecassic acid and asiatic acid) in Centella asiatica (L.) urban extracts. The analysis was performed on an Agilent 1100 HPLC system with a ZORBAX Eclipse XDB-C8 column (4.6 mm×150 mm, 5μm). The four major constituents were separated with gradient mobile phase that consists of 1mmol/L potassium dihydrogen phosphate and acetonitrile at the detection wavelength of 205 nm. The four major constituents all had good linear response in the determination ranges (R(2)≥0.9998). The average recoveries (n=9) were 97.4%, 93.7%, 97.5% and 99.8% with RSDs of 3.4%, 1.4%, 4.7% and 4.4%, respectively. The developed method is sensitive and has good reproducibility, which can be used as a reference for quality control of Centella asiatica (L.) urban extracts.

  9. [Simultaneous determination of four mercapturic acids in human urine using solid phase extraction and liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Hou, Hongwei; Xiong, Wei; Gao, Na; Song, Dongkui; Tang, Gangling; Hu, Qingyuan

    2011-01-01

    A method was developed for the simultaneous extraction and determination of four mercapturic acids (MAs), N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine (DHBMA), N-acetyl-S-(3-hydroxypropyl)-L-cysteine (3-HPMA), N-acetyl-S-(2-carboxyethyl)-L-cysteine ( CEMA) and S-phenylmercapturic acid (SPMA), in human urine using solid phase extraction and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Frozen urine samples were thawed at room temperature, and centrifuged to remove any settled precipitate. The supernatant was then purified and concentrated by a C18 solid phase extraction column, and analyzed by HPLC-MS/MS in the multiple reaction monitoring (MRM) mode for the quantitative analysis. The ranges of recovery for DHBMA, 3-HPMA, CEMA and SPMA spiked in human urine matrix at three concentration levels were 105.6%-124.4%, 102.7%-106.5%, 103.2%-103.9% and 101.7%-104.3%, respectively, with the relative standard deviations of 2.6%-7.7%. The limits of detection (LOD, S/N > or = 3) were 0. 062, 0. 031, 0. 020 and 0. 003 microg/L for DHBMA, 3-HPMA, CEMA and SPMA, respectively. The method was successfully used to detect 4 MAs in 37 human urine samples from smokers and non-smokers. It was found that the contents of 3-HPMA, CEMA and SPMA in the urines from cigarette smokers were about three to six-fold more than those in the urines from the non-smokers.

  10. Combination of Electromembrane Extraction and Liquid-Phase Microextraction in a Single Step: Simultaneous Group Separation of Acidic and Basic Drugs.

    Science.gov (United States)

    Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid; Shen, Xiantao; Pedersen-Bjergaard, Stig

    2015-07-07

    Electromembrane extraction (EME) and liquid-phase microextraction (LPME) were combined in a single step for the first time to realize simultaneous and clear group separation of basic and acidic drugs. Using 2-nitrophenyl octyl ether as the supported liquid membrane (SLM) for EME and dihexyl ether as the SLM for LPME, basic and acidic drugs were extracted and separated simultaneously from a low pH sample by EME and LPME, respectively. After 15 min of extraction, basic drugs (citalopram and sertraline) were exhaustively extracted, whereas the recoveries for acidic drugs (ketoprofen and ibuprofen) were in the range of 76%-86%. Longer extraction time provided higher recoveries for the acidic drugs, but this somewhat deteriorated the group separation. Matrices effects from the coexisting acidic drugs/basic drugs were tested, and we observed that simultaneous EME/LPME was not affected by coexisting drugs at high concentration. This approach was further investigated from human plasma. Extraction recoveries were strongly dependent on dilution of plasma with buffer and on extraction time. Finally, this simultaneous EME/LPME approach was evaluated in combination with liquid chromatography (LC)-MS. The linearity ranges for the basic and acidic drugs were 10-600 ng/mL and 1-60 μg/mL, respectively, with R(2) > 0.997 for all analytes. The repeatability at three different levels for all analytes was less than 15%. The limits of quantification (LOQ, S/N = 10) were found to be 4.0-6.3 ng/mL and 0.6-0.9 μg/mL for basic and acidic drugs, respectively. Simultaneous EME/LPME enabled efficient group separation of basic and acidic analytes under optimum experimental conditions for both EME and LPME.

  11. Cosmetic devices based on active transdermal technologies.

    Science.gov (United States)

    Scott, Jessica A; Banga, Ajay K

    2015-01-01

    Active transdermal technology, commonly associated with drug delivery, has been used in recent years by the cosmetic industry for the aesthetic restoration of skin and delivery of cosmetic agents. In this article, we provide an overview of the skin's structure, various skin types, skin's self-repair mechanisms that are stimulated from the usage of cosmetic devices and discuss cosmetic applications. Summaries of the most common active transdermal technologies such as microneedles, iontophoresis, sonophoresis, lasers and microdermabrasion will be provided, in relation to the marketed cosmetic devices available that incorporate these technologies. Lastly, we cover combinations of active technologies that allow for more enhanced cosmetic results, and the current limitations of cosmetic devices.

  12. Simultaneous quantification of lycopene, β-carotene, retinol and α -tocopherol in plasma after a simple extraction procedure: stability study and application to human volunteers

    OpenAIRE

    Charão, Mariele F.; Moro, Angela M.; Brucker, Natália; Bulcão, Rachel P.; Baierle, Marília; Freitas, Fernando; Durgante, Juliano; Nascimento, Sabrina; Bubols, Guilherme B.; Saldiva, Paulo H.; Bohrer, Denise; Garcia, Solange C.

    2012-01-01

    A method for the simultaneous quantification of lycopene, β-carotene, retinol and α-tocopherol by high-performance liquid chromatography (HPLC) with Vis/fluorescence detection with isocratic elution was optimized and validated. The method consists of a rapid and simple liquid-liquid extraction procedure and a posterior quantification of extracted supernatants by HPLC. Aliquots of plasma were stored at -20°C for three months for stability study. The methodology was applied to samples from pain...

  13. In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

    Science.gov (United States)

    Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

    2015-12-18

    A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Simultaneous quantification of triterpenoic acids by high performance liquid chromatography method in the extracts of gum resin of Boswellia serrata obtained by different extraction techniques.

    Science.gov (United States)

    Sharma, Neha; Bhardwaj, Vikram; Singh, Samar; Ali, Sheikh Abid; Gupta, D K; Paul, Satya; Satti, Naresh K; Chandra, Suresh; Verma, Mahendra K

    2016-01-01

    Boswellia serrata, also known as Indian frankincense is a commercially important medicinal plant which has been used for hundreds of years as an Ayurvedic medicine for the attempted treatment of arthritis. It contains naturally occurring triterpenoic acids, called as boswellic acids (BA's). A highly reproducible High performance liquid chromatography-ultraviolet diode array detection (HPLC-UV-DAD) method was developed for the simultaneous determination and quantitative analysis of eight major triterpenoic acids in Boswellia serrata gum resin obtained by different extraction techniques. All the calibration curves exhibited good linear regression (R(2) > 0.997) within the test ranges. The established method showed good precision and overall recoveries of the boswellic acids. The eight triterpenoic acids coded as BS-1 (11-keto-beta-boswellic acid), BS-2 (3-O-acetyl-11-keto-beta-boswellic acid), BS-3 (3-keto tirucallic acid), BS-4 (3-O-acetyl-alpha-tirucallic acid), BS-5 (3-O-acetyl-beta-tirucallic acid), BS-6 (alpha-boswellic acid), BS-7 (beta-boswellic acid) and BS-8 (3-O-acetyl-beta-boswellic acid) were isolated from the processed gum resin of Boswellia serrata by column chromatography. The proposed HPLC method is simple, reliable and has been very useful for the qualitative as well as quantitative analysis of boswellic acids in the gum resin of Boswellia serrata. The proposed method allows to quantify boswellic acids in appreciable amounts by HPLC-UV (DAD) method in the extracts and the available marketed formulations.Graphical abstractIsolation & separation of eight Triterpenoic acids from Boswellia serrata.

  15. Simultaneous Determination of Arsenic and Selenium Species in Sediment Extracts Utilizing Coupled Techniques with Mass Spectrometric Detection

    Science.gov (United States)

    Yoon, H.; Yoon, C.

    2009-12-01

    Arsenic has been recognized as one of the major problems of toxicity in several parts of the world. It is well known that the toxicity of arsenic depends on its chemical form. Selenium is one of the minor but plays an important biological role in human health. The multiple roles of selenium, deficiency and toxicity, depend on its chemical form and concentration. The multielement detection capability of ICP-MS makes it an ideal detector for multielement chromatographic separation. Most of multielement separation analyses by LC-ICP-MS are applied to standard or to water samples. Only very few reports deal with solid matrices. A procedure for the simultaneous determination of arsenic and selenium species in phosphoric acid extracts of sediment samples by liquid chromatography coupled to ICP-MS has been developing. Arsenic species, arsenite [As(III)], arsenate [As(V)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and selenium species, selenite [Se(IV)], selenate [Se(VI)] were separated on anion exchange column by a mobile phase of ammonium dihydrogen phosphate. The total analysis took less than 10 min with gradient elution at flow rate of 1.0 mL/min. The sonication extraction was used with dry sediment and phosphoric acid. Reaction gases such as methane and oxygen was used to remove spectral interferences on arsenic and selenium measurement. The estimated detection limits in the sediment ranged between 1 and 25 ng/g for the arsenic and selenium species. The repeatability was less than 15% (RSD) for 1 µg/L arsenic species and 5 µg/L selenium species. Accuracy of the method was assessed through the recovery of the spiked sediment. Recoveries ranged between 82 and 115 % for all the species.

  16. Simultaneous determination of pesticide residues and antioxidants in blended oil using a liquid-liquid extraction combined with dispersive solid phase extraction method.

    Science.gov (United States)

    Fang, Yong; Tian, Wen; Pei, Fei; Li, Peng; Shao, XiaoLong; Fan, Yan; Hu, Qiuhui

    2017-08-15

    This article developed a method to detect two antioxidants (butylated hydroxyl anisole (BHA), butylated hydroxyl toluene (BHT)) and twelve pesticides (dichlorvos, pirimicarb, prothiofos, fenitrothion, ethoprophos, malathion, beta-Cypermethrin, profenofos, diazinon, propoxur, procymidon, captan) in blended oil samples after their extraction simultaneously. The establishment of the method was based on two-step process of screening and optimization experiment design. With a Plackett-Burman (PB) design, significant parameters were found by screening experiment and single factor experiment accompanied by a central composite design (CCD) experiment were used to make important parameters optimal. The coefficients of determination (r(2)) was between 0.9931 and 0.9996 while the limits of quantification (LOQs) and limits of detection (LODs) were found in scope of 0.002-0.04mg·kg(-1) and 0.0006-0.0012mg·kg(-1). Recovery values of analytes were above 74%, at the same time the relative standard deviations (RSDs) under 10% at the concentrations ranging from 0.05mg·kg(-1) to 0.20mg·kg(-1). To sum up, this method with shorter time and fewer consumption of reagents could be employed in various occasions to detect antioxidants and pesticides. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Navigating sticky areas in transdermal product development.

    Science.gov (United States)

    Strasinger, Caroline; Raney, Sam G; Tran, Doanh C; Ghosh, Priyanka; Newman, Bryan; Bashaw, Edward D; Ghosh, Tapash; Shukla, Chinmay G

    2016-07-10

    The benefits of transdermal delivery over the oral route to combat such issues of low bioavailability and limited controlled release opportunities are well known and have been previously discussed by many in the field (Prausnitz et al. (2004) [1]; Hadgraft and Lane (2006) [2]). However, significant challenges faced by developers as a product moves from the purely theoretical to commercial production have hampered full capitalization of the dosage forms vast benefits. While different technical aspects of transdermal system development have been discussed at various industry meetings and scientific workshops, uncertainties have persisted regarding the pharmaceutical industry's conventionally accepted approach for the development and manufacturing of transdermal systems. This review provides an overview of the challenges frequently faced and the industry's best practices for assuring the quality and performance of transdermal delivery systems and topical patches (collectively, TDS). The topics discussed are broadly divided into the evaluation of product quality and the evaluation of product performance; with the overall goal of the discussion to improve, advance and accelerate commercial development in the area of this complex controlled release dosage form. Published by Elsevier B.V.

  18. Enhanced Controlled Transdermal Delivery of Torasemide Using ...

    African Journals Online (AJOL)

    Purpose: To develop an ethylene-vinyl acetate (EVA) matrix system containing a permeation enhancer for enhanced transdermal delivery of torasemide. Methods: The solubility of torasemide was studied at various volume fraction of polyethylene glycol (PEG) 400. The effect of drug concentration was tested at 1.0, 2.0 and ...

  19. Development and Evaluation of Ibuprofen Transdermal Gel ...

    African Journals Online (AJOL)

    Erah

    1Dubai Pharmacy College, Dubai, UAE, 2Helwan University, Helwan, Egypt. Abstract. Purpose: To develop an ibuprofen transdermal gel with a capability for both topical and systemic drug delivery. Methods: Ibuprofen gel formulations, incorporating various permeation enhancers, were prepared using chitosan as a gelling ...

  20. Development and Evaluation of Ketoprofen Acrylic Transdermal ...

    African Journals Online (AJOL)

    Results: DSC thermograms demonstrate that the drug was dispersed molecularly in the polymer in all the formulations. Increase in PSA content increased the W/A ratio and adhesiveness of KTPs. Ketoprofen release from the transdermal patches followed the Higuchi diffusion model. Ketoprofen flux increased with increase ...

  1. Preparation and physicochemical evaluation of transdermal ...

    African Journals Online (AJOL)

    induced pain, as well as vascular headache and dysmenorrhea. It is usually administered through the oral or ... migraine, postoperative sore throat, and muscle soreness [15,16]. In recent years, transdermal metered-dose .... revealed a considerable increase in the flux of the drug through the rat skin. The increased drug.

  2. Development and Evaluation of Ketoprofen Acrylic Transdermal ...

    African Journals Online (AJOL)

    Purpose: To fabricate ketoprofen transdermal patches (KTPs) using an acrylic pressure-sensitive adhesive (PSA) polymer. Methods: KTPs were prepared using solvent casting method. The influence of the amount of PSA, drug content, and terpenes as penetration enhancers on the characteristics of the patch, namely, ...

  3. Feasibility of retroreflective transdermal optical wireless communication.

    Science.gov (United States)

    Gil, Yotam; Rotter, Nadav; Arnon, Shlomi

    2012-06-20

    There is an increasing demand for transdermal high-data-rate communication for use with in-body devices, such as pacemakers, smart prostheses, neural signals processors at the brain interface, and cameras acting as artificial eyes as well as for collecting signals generated within the human body. Prominent requirements of these communication systems include (1) wireless modality, (2) noise immunity and (3) ultra-low-power consumption for the in-body device. Today, the common wireless methods for transdermal communication are based on communication at radio frequencies, electrical induction, or acoustic waves. In this paper, we will explore another alternative to these methods--optical wireless communication (OWC)--for which modulated light carries the information. The main advantages of OWC in transdermal communication, by comparison to the other methods, are the high data rates and immunity to external interference availed, which combine to make it a promising technology for next-generation systems. In this paper, we present a mathematical model and experimental results of measurements from direct link and retroreflection link configurations with Gallus gallus domesticus derma as the transdermal channel. The main conclusion from this work is that an OWC link is an attractive communication solution in medical applications. For a modulating retroreflective link to become a competitive solution in comparison with a direct link, low-energy-consumption modulating retroreflectors should be developed.

  4. Molecularly imprinted polymers with synthetic dummy template for simultaneously selective removal and enrichment of ginkgolic acids from Ginkgo biloba L. leaves extracts.

    Science.gov (United States)

    Ji, Wenhua; Ma, Xiuli; Xie, Hongkai; Chen, Lingxiao; Wang, Xiao; Zhao, Hengqiang; Huang, Luqi

    2014-11-14

    Dummy molecularly imprinted polymers (DMIPs) for simultaneously selective removal and enrichment of ginkgolic acids (GAs) during the processing of Ginkgo biloba leaves have been prepared. Two dummy template molecule with similar structural skeleton to GAs, 6-methoxysalicylic acid (MOSA, DT-1) and 6-hexadecyloxysalicylic acid (HOSA, DT-2), have been designed and synthesized. The performance of the DMIPs and NIPs were evaluated including selective recognition capacity, adsorption isotherm, and adsorption kinetics. The selective recognition capacity of the three GAs with four analogues on the sorbents illustrated that the DMIPs sorbents have high specificity for GAs. An efficient method based on DMIP-HOSA coupled with solid-phase extraction (SPE) was developed for simultaneously selective removal and enrichment of ginkgolic acids (GAs) during the processing of Ginkgo biloba leaves. The method showed excellent recoveries (82.5-88.7%) and precision (RSD 0.5-2.6%, n=5) for licorice extracts, Gastrodia elata extracts and pepper extracts spiked at three concentration levels each (50, 100, 200 μg mL(-1)). The results indicated that GAs and standardized Ginkgo biloba leaves extracts could be obtained simultaneously through the DMIP-SPE. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Simultaneous determination of 106 pesticides in nuts by LC-MS/MS using freeze-out combined with dispersive solid-phase extraction purification.

    Science.gov (United States)

    Wang, Jingjing; Gong, Zhiguo; Zhang, Tingting; Feng, Shun; Wang, Jide; Zhang, Yi

    2017-06-01

    As a result of the low water content and high fat matrices in nuts, it is very difficult to simultaneously determine multi-pesticides in trace levels. Here, a sample pretreatment method was developed in which, microwave-assisted solvent extraction was firstly used to extract pesticides, and then a two-step cleanup method was conducted combining freeze-out with dispersive solid-phase extraction to remove the lipidic matrix. By this way, 106 pesticides were simultaneously determined in the complicated nut sample by using an ultra-high pressure liquid chromatography coupled with a tandem mass spectrometer. Average recoveries were 75.3-119.3% with relative standard deviations pesticides in 180 commercial nut samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Simultaneous extraction and analysis by high performance liquid chromatography coupled to diode array and mass spectrometric detectors of bixin and phenolic compounds from annatto seeds.

    Science.gov (United States)

    Chisté, Renan Campos; Yamashita, Fábio; Gozzo, Fábio Cesar; Mercadante, Adriana Zerlotti

    2011-01-07

    This study was designed to identify and quantify the carotenoids and phenolic compounds from annatto seeds using high performance liquid chromatography coupled to diode array and mass spectrometer detectors (HPLC-DAD-MS/MS). Furthermore, using response surface methodology, an optimized procedure for simultaneous extraction of these compounds was established. In addition to bixin, known to be the main carotenoid in annatto seeds, hypolaetin and a caffeoyl acid derivative were identified as the main phenolic compounds. The optimized procedure involved 15 extractions using acetone:methanol:water (50:40:10, v/v/v) as solvent, a solid-liquid ratio of 1:9 (m/v) and an extraction time of 5 min. Validation data indicated that the HPLC method proposed provided good linearity, sensitivity, procedure accuracy, system precision and suggested its suitability for the simultaneous analysis of phenolic compounds and carotenoids in annatto seeds. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Recent advances in peptides for enhancing transdermal macromolecular drug delivery.

    Science.gov (United States)

    Ruan, Renquan; Chen, Ming; Zou, Lili; Wei, Pengfei; Liu, Juanjuan; Ding, Weiping; Wen, Longping

    2016-01-01

    Transdermal delivery of drugs, a compelling route of systemic drug delivery, provides painless, reliable, targeted, efficient and cost effective therapeutic regimen for patients. However, its use is limited by skin barrier especially the stratum corneum barrier. Moreover, transdermal delivery of macromolecules remains a challenge. Naturally, varieties of physical methods, chemical enhancers and drug carriers have been used to counteract this limitation. Recently, transdermal peptides discovered as safer, more efficient and more specific enhancers could promote the delivery of macromolecules across the skin. Herein, the underlying transdermal peptides are included. Subsequently, we have discussed typical applications and the possible mechanism of two groups of biologically inspired transdermal peptide enhancers, namely cell penetration peptides and transdermal enhanced peptides.

  8. [Simultaneous determination of twelve sweeteners and nine preservatives in foods by solid-phase extraction and LC-MS/MS].

    Science.gov (United States)

    Tsuruda, Sayuri; Sakamoto, Tomonori; Akaki, Kouichi

    2013-01-01

    A rapid and simple method for the simultaneous determination of twelve sweeteners and nine preservatives in various foods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The sweeteners and preservatives were extracted from solid samples with 80% and 50% methanol and from liquid samples with 80% methanol, followed by Oasis WAX cartridge cleanup. The LC separation was performed on a XSelect CSH Phenyl-Hexyl column (5 μm, 2.1 mm ×150 mm) with a mobile phase of 10 mmol/L acetate buffer (pH 4.0)-acetonitrile and MS detection with negative ion electrospray ionization. The quantification limits of acesulfame K (AK), alitame (AL), aspartame (ASP), cyclamic acid (CYC), neotame (NEO), saccharin Na (SAC), p-hydroxybenzoic acid methyl (PHBA-Me), p-hydroxybenzoic acid ethyl (PHBA-Et), p-hydroxybenzoic acid isopropyl (PHBA-iPr), p-hydroxybenzoic acid propyl (PHBA-Pr), p-hydroxybenzoic acid isobutyl (PHBA-iBu) and p-hydroxybenzoic acid butyl (PHBA-Bu) were 0.001 g/kg, those of dulcin (DU), glycyrrhizic acid (GLY), neohesperidin dihydrochalcone (NHDC), rebaudioside A (REB), stevioside (STV), sucralose (SUC) and benzoic acid (BA) were 0.005 g/kg, and those of sorbic acid (SOA) and dehydroacetic acid (DHA) were 0.02 g/kg. The mean recoveries from ten kinds of foods fortified at the levels of 0.02 and 0.2 g/kg were 70.9-119.0%, and their relative standard deviations were 0.1-11.7%.

  9. Synthesis and transdermal properties of acetylsalicylic acid and selected esters

    OpenAIRE

    Gerber, Minja; Breytenbach, Jaco C.; Hadgraft, Jonathan; du Plessis, Jeanetta

    2006-01-01

    The primary aim of this study was to determine the transdermal penetration of acetylsalicylic acid and some of its derivatives, to establish a correlation, if any, with selected physicochemical properties and to determine if transdermal application of acetylsalicylic acid and its derivatives will give therapeutic drug concentrations with respect to transdermal flux. Ten derivatives of acetylsalicylic acid were prepared by esterification of acetylsalicyloyl chloride with ten different alcohols...

  10. Transdermal Delivery of Drugs with Microneedles—Potential and Challenges

    OpenAIRE

    Kevin Ita

    2015-01-01

    Transdermal drug delivery offers a number of advantages including improved patient compliance, sustained release, avoidance of gastric irritation, as well as elimination of pre-systemic first-pass effect. However, only few medications can be delivered through the transdermal route in therapeutic amounts. Microneedles can be used to enhance transdermal drug delivery. In this review, different types of microneedles are described and their methods of fabrication highlighted. Microneedles can be ...

  11. Simultaneous extraction of Cr(III) and Cr(VI) with a dithiocarbamate reagent followed by HPLC separation for chromium speciation.

    Science.gov (United States)

    Wang, Joanna Shaofen; Chiu, KongHwa

    2004-05-01

    A simultaneous extraction of Cr3+ and Cr6+ species in aqueous solution was developed. The extraction behaviors of ammonium pyrrolidinedithiocarbamate (APDC) for both Cr6+ and Cr3+ are carefully discussed in this report. X-ray diffraction and spectroscopic studies indicate that Cr6+ reacts with the ammonium pyrrolidinedithiocarbamate ligand to form two products, Cr(PDC)2(OPDC) and Cr(PDC)3, where OPDC represents an oxygen insertion between Cr and S atoms. A high concentration of APDC in the phthalate buffer under an elevated temperature (50 degrees C) was applied in solvent extraction (SE) to increase the extraction efficiency of Cr3+, so that both Cr3+ and Cr6+ could be extracted by APDC simultaneously. The complex involving the oxygen insertion bonding Cr-O-S is separable from the normal Cr(PDC)3 complex chromatographically, thus allowing the quantification of Cr6+. The major product of Cr6+ has a structure of Cr(PDC)2(OPDC) and the minor product is Cr(PDC)3 with a ratio of Cr(PDC)2(OPDC)/Cr(PDC)3 being 8.5. The extraction conditions for Cr6+ and Cr3+ as well as the chromatographic separation of the complexes using high-performance liquid chromatography (HPLC) are reported. Potential applications for the chemical speciation of chromium by SE/HPLC in environmental aqueous solutions are also discussed.

  12. Recent advances in the design of polymeric microneedles for transdermal drug delivery and biosensing.

    Science.gov (United States)

    Wang, Min; Hu, Lianzhe; Xu, Chenjie

    2017-04-11

    Microneedles are an efficient and minimally invasive approach to transdermal drug delivery and extraction of skin interstitial fluid. Compared to solid microneedles made of silicon, metals and ceramics, polymeric microneedles have attracted extensive attention due to their excellent biocompatibility, biodegradability and nontoxicity. They are easy to fabricate in large scale and can load drugs in high amounts. More importantly, polymers with different degradation profiles, swelling properties, and responses to biological/physical stimuli can be employed to fabricate polymeric microneedles with different mechanical properties and performance. This review provides a guideline for the selection of polymers and the corresponding fabrication methods for polymeric microneedles while summarizing their recent application in drug delivery and fluid extraction. It should be noted that although polymeric microneedles can achieve efficient transdermal delivery of drugs, their wide applications were limited by their unsatisfactory transdermal therapeutic efficiency. Delivery of nanomedicines that incorporate drugs into functional nanoparticles/capsules can address this problem and thus may be an interesting direction in the future.

  13. Simultaneous application of chemical oxidation and extraction processes is effective at remediating soil Co-contaminated with petroleum and heavy metals.

    Science.gov (United States)

    Yoo, Jong-Chan; Lee, Chadol; Lee, Jeung-Sun; Baek, Kitae

    2017-01-15

    Chemical extraction and oxidation processes to clean up heavy metals and hydrocarbon from soil have a higher remediation efficiency and take less time than other remediation processes. In batch extraction/oxidation process, 3% hydrogen peroxide (H2O2) and 0.1 M ethylenediaminetetraacetic acid (EDTA) could remove approximately 70% of the petroleum and 60% of the Cu and Pb in the soil, respectively. In particular, petroleum was effectively oxidized by H2O2 without addition of any catalysts through dissolution of Fe oxides in natural soils. Furthermore, heavy metals bound to Fe-Mn oxyhydroxides could be extracted by metal-EDTA as well as Fe-EDTA complexation due to the high affinity of EDTA for metals. However, the strong binding of Fe-EDTA inhibited the oxidation of petroleum in the extraction-oxidation sequential process because Fe was removed during the extraction process with EDTA. The oxidation-extraction sequential process did not significantly enhance the extraction of heavy metals from soil, because a small portion of heavy metals remained bound to organic matter. Overall, simultaneous application of oxidation and extraction processes resulted in highly efficient removal of both contaminants; this approach can be used to remove co-contaminants from soil in a short amount of time at a reasonable cost. Copyright © 2016 Elsevier Ltd. All rights reserved.

  14. Optimization of Ionic Liquid Based Simultaneous Ultrasonic- and Microwave-Assisted Extraction of Rutin and Quercetin from Leaves of Velvetleaf (Abutilon theophrasti by Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2014-01-01

    Full Text Available An ionic liquids based simultaneous ultrasonic and microwave assisted extraction (ILs-UMAE method has been proposed for the extraction of rutin (RU, quercetin (QU, from velvetleaf leaves. The influential parameters of the ILs-UMAE were optimized by the single factor and the central composite design (CCD experiments. A 2.00 M 1-butyl-3-methylimidazolium bromide ([C4mim]Br was used as the experimental ionic liquid, extraction temperature 60°C, extraction time 12 min, liquid-solid ratio 32 mL/g, microwave power of 534 W, and a fixed ultrasonic power of 50 W. Compared to conventional heating reflux extraction (HRE, the RU and QU extraction yields obtained by ILs-UMAE were, respectively, 5.49 mg/g and 0.27 mg/g, which increased, respectively, 2.01-fold and 2.34-fold with the recoveries that were in the range of 97.62–102.36% for RU and 97.33–102.21% for QU with RSDs lower than 3.2% under the optimized UMAE conditions. In addition, the shorter extraction time was used in ILs-UMAE, compared with HRE. Therefore, ILs-UMAE was a rapid and an efficient method for the extraction of RU and QU from the leaves of velvetleaf.

  15. Optimization of ionic liquid based simultaneous ultrasonic- and microwave-assisted extraction of rutin and quercetin from leaves of velvetleaf (Abutilon theophrasti) by response surface methodology.

    Science.gov (United States)

    Zhao, Chunjian; Lu, Zhicheng; Li, Chunying; He, Xin; Li, Zhao; Shi, Kunming; Yang, Lei; Fu, Yujie; Zu, Yuangang

    2014-01-01

    An ionic liquids based simultaneous ultrasonic and microwave assisted extraction (ILs-UMAE) method has been proposed for the extraction of rutin (RU), quercetin (QU), from velvetleaf leaves. The influential parameters of the ILs-UMAE were optimized by the single factor and the central composite design (CCD) experiments. A 2.00 M 1-butyl-3-methylimidazolium bromide ([C4mim]Br) was used as the experimental ionic liquid, extraction temperature 60°C, extraction time 12 min, liquid-solid ratio 32 mL/g, microwave power of 534 W, and a fixed ultrasonic power of 50 W. Compared to conventional heating reflux extraction (HRE), the RU and QU extraction yields obtained by ILs-UMAE were, respectively, 5.49 mg/g and 0.27 mg/g, which increased, respectively, 2.01-fold and 2.34-fold with the recoveries that were in the range of 97.62-102.36% for RU and 97.33-102.21% for QU with RSDs lower than 3.2% under the optimized UMAE conditions. In addition, the shorter extraction time was used in ILs-UMAE, compared with HRE. Therefore, ILs-UMAE was a rapid and an efficient method for the extraction of RU and QU from the leaves of velvetleaf.

  16. Coupled Hydro-Mechanical Simulations of CO2 Storage Supported by Pressure Management Demonstrate Synergy Benefits from Simultaneous Formation Fluid Extraction

    Directory of Open Access Journals (Sweden)

    Kempka Thomas

    2015-04-01

    Full Text Available We assessed the synergetic benefits of simultaneous formation fluid extraction during CO2 injection for reservoir pressure management by coupled hydro-mechanical simulations at the prospective Vedsted storage site located in northern Denmark. Effectiveness of reservoir pressure management was investigated by simulation of CO2 storage without any fluid extraction as well as with 66% and 100% equivalent volume formation fluid extraction from four wells positioned for geothermal heat recovery. Simulation results demonstrate that a total pressure reduction of up to about 1.1 MPa can be achieved at the injection well. Furthermore, the areal pressure perturbation in the storage reservoir can be significantly decreased compared to the simulation scenario without any formation fluid extraction. Following a stress regime analysis, two stress regimes were considered in the coupled hydro-mechanical simulations indicating that the maximum ground surface uplift is about 0.24 m in the absence of any reservoir pressure management. However, a ground uplift mitigation of up to 37.3% (from 0.24 m to 0.15 m can be achieved at the injection well by 100% equivalent volume formation fluid extraction. Well-based adaptation of fluid extraction rates can support achieving zero displacements at the proposed formation fluid extraction wells located close to urban infrastructure. Since shear and tensile failure do not occur under both stress regimes for all investigated scenarios, it is concluded that a safe operation of CO2 injection with simultaneous formation fluid extraction for geothermal heat recovery can be implemented at the Vedsted site.

  17. Transdermal microneedles for drug delivery applications

    Energy Technology Data Exchange (ETDEWEB)

    Teo, Ai Ling [Defence Medical and Environmental Research Institute, DSO National Laboratories (Kent Ridge), 27 Medical Drive, 12-00, Singapore 117510 (Singapore); Shearwood, Christopher [School of Mechanical and Aerospace Engineering, 50 Nanyang Avenue, Singapore 639798 (Singapore); Ng, Kian Chye [Defence Medical and Environmental Research Institute, DSO National Laboratories (Kent Ridge), 27 Medical Drive, 12-00, Singapore 117510 (Singapore); Lu Jia [Defence Medical and Environmental Research Institute, DSO National Laboratories (Kent Ridge), 27 Medical Drive, 12-00, Singapore 117510 (Singapore); Moochhala, Shabbir [Defence Medical and Environmental Research Institute, DSO National Laboratories (Kent Ridge), 27 Medical Drive, 12-00, Singapore 117510 (Singapore)]. E-mail: mshabbir@dso.org.sg

    2006-07-25

    Transdermal drug delivery (TDD) has many advantages, the main one being the ability to maintain the prolonged release of drugs to attain optimal blood concentrations. Unfortunately, nature has provided a very effective protective barrier, the stratum corneum (sc), which limits TDD to certain types of drugs with specific properties. In order to enhance TDD, the idea of using microneedles to painlessly penetrate the sc barrier has previously been proposed. In this paper, we will review the different microneedles that are currently being developed as well as our own efforts in this area. Based on our experiences, we will offer our view on the key parameters for effective transdermal microneedle design as well as future directions in this area.

  18. Pressurized liquid extraction and GC-MS analysis for simultaneous determination of seven components in Cinnamomum cassia and the effect of sample preparation.

    Science.gov (United States)

    Lv, Guang-Ping; Huang, Wei-Hua; Yang, Feng-Qing; Li, Jing; Li, Shao-Ping

    2010-08-01

    A pressurized liquid extraction and GC-MS method was developed for simultaneous quantitative determination of the seven components, including cinnamaldehyde, copaene, cinnamic acid, coumarin, 2-methoxycinnamaldehyde, 2-methoxycinnamic acid and safrole in Cinnamomum cassia. The results showed that methanol and ethanol was not available for extraction of cinnamaldehyde and 2-methoxycinnamaldehyde due to aldol reaction. The developed method was validated to be sensitive, accurate and simple, and was successfully employed for the analysis of 15 samples of C. cassia. The contents of the investigated components were significantly variant and cinnamaldehyde is the most abundant compound, but safrole was not detected in all samples.

  19. Proniosomes for Penetration Enhancement in Transdermal System

    OpenAIRE

    Samita Singla; S. L. HariKumar; Geeta Aggarwal

    2012-01-01

    Over the last few years an inclusive research has been done over provesicular approach for transdermal drug delivery. Skin has a very tough diffusion barrier inhibiting penetration of drug moiety which is rate limiting barrier for penetration of drugs. There are several approaches that deal with penetration enhancement across the skin. Vesicular and provesicular systems are promising amongst them. Vesicular systems including (niosomes, ethosomes, transfersomes and liposomes) are promising sys...

  20. Membrane Assisted Simultaneous Extraction and Derivatization with Triphenylphosphine of Elemental Sulfur in Arabian Crude Samples by Gas Chromatography/Mass Spectrometry

    OpenAIRE

    Al-Zahrani, Ibrahim; Aneel Mohammed, Munzir H.; Basheer, Chanbasha; Siddiqui, Mohammad Nahid; Al-Arfaj, Abdulrahman

    2015-01-01

    Determination of trace level elemental sulfur from crude oil samples is a tedious task. Recently, several gas chromatographic methods were reported in which selective triphenylphosphine derivatization of sulfur was used to form triphenylphosphine sulfide. Direct quantitation of elemental sulfur from crude oil requires an efficient sample preparation method. This paper describes how simultaneous extraction derivatization of elemental sulfur was performed for the first time using porous hollow ...

  1. Statistical design-principal component analysis optimization of a multiple response procedure using cloud point extraction and simultaneous determination of metals by ICP OES

    OpenAIRE

    Bezerra, Marcos de Almeida; Bruns, Roy Edward; Ferreira, Sergio Luis Costa

    2006-01-01

    RESTRITO A procedure has been developed for the simultaneous determination of traces amounts of Cd, Cr, Cu, Mn, Ni and Pb from saline oil-refinery effluents and digested vegetable samples using inductively coupled plasma optical emission spectrometry (ICP OES). The procedure is based on cloud point extraction (CPE) of these metals as 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) complexes into a micellar phase of octylphenoxypolyethoxyethanol (Triton X-114). Optimization of the ...

  2. Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction

    National Research Council Canada - National Science Library

    FuKai Li; AiJun Gong; LiNa Qiu; WeiWei Zhang; JingRui Li; Yu Liu; YuNing Liu; HuiTing Yuan

    2017-01-01

    .... In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES...

  3. Simultaneous chemical fingerprint and quantitative analysis of Rhizoma Smilacis Glabrae by accelerated solvent extraction and high-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Dai, Weiquan; Zhao, Weiquan; Gao, Fangyuan; Shen, Jingjing; Lv, Diya; Qi, Yunpeng; Fan, Guorong

    2015-05-01

    Rhizoma Smilacis Glabrae (RSG) is a well-known herbal medicine with the homology of medicine and food. In this study, simultaneous chemical fingerprint and quantitative analysis of the bioactive flavonoid components of RSG were developed using accelerated solvent extraction and high-performance liquid chromatography coupled with ion trap tandem mass spectrometry. The operational parameters of accelerated solvent extraction including extraction solvent, extraction temperature, static extraction time, solid-to-liquid ratio, and extraction cycles were optimized. Hierarchical cluster analysis, similarity analysis, and principal component analysis were performed to evaluate the similarity and variation of the samples collected from several provinces in China. Subsequently, high-performance liquid chromatography fingerprints were established for the discrimination of 16 batches of RSG samples, and the major six flavonoids, namely, toxifolin, neoastilbin, astilbin, neoisoastilbin, isoastilbin, and engeletin were then quantitatively determined. The calibration curves for all the six analytes showed good linearity (r(2) > 0.999), and the limits of detection and quantification were less than 0.10 and 0.27 μg·mL(-1) , respectively. Therefore, the proposed extraction and determination methods were proved to be robust and reliable for the quality control of RSG. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Penetration Enhancement Effect of Turpentine Oil on Transdermal ...

    African Journals Online (AJOL)

    Purpose: To prepare transdermal films of ketorolac tromethamine (KT) and study the effect of turpentine oil as a penetration enhancer for the drug. Methods: Transdermal films of KT were prepared with Carbopol-934 and ethyl cellulose, with turpentine oil as the penetration enhancer, using solvent evaporation method.

  5. Some Recent Advances in Transdermal Drug Delivery Systems ...

    African Journals Online (AJOL)

    Transdermal delivery systems are forms of drug delivery involving the dermis, as distinct from topical, oral or other forms of parenteral dosage forms. Over the years transdermal drug delivery systems have progressed in terms of usage and innovations making it gain increasing popularity. The route has a lot of advantages ...

  6. TRANSFEROSOMES: A NOVEL APPROACH FOR TRANSDERMAL DRUG DELIVERY

    OpenAIRE

    Kumar Ravi; Manvir Singh; Rajni bala; Nimrata seth; Rana, A. C.

    2012-01-01

    Transdermal drug delivery system appears to be most promising delivery system due to their merits over conventional delivery systems. Recently, various strategies have been used to augment the transdermal delivery of bioactives. Mainly, they include iontophoresis, electrophoresis, sonophoresis, chemical permeation enhancers, microneedles, and vesicular system (liposomes, niosomes, elastic liposomes such as ethosomes and transfersomes). Among these strategies transferosomes appear promising. T...

  7. Current advances in the fabrication of microneedles for transdermal delivery

    NARCIS (Netherlands)

    Indermun, Sunaina; Lüttge, Regina; Choonara, Yahya E.; Kumar, Pradeep; du Toit, Lisa C.; Modi, Girish; Pillay, Viness

    2014-01-01

    The transdermal route is an excellent site for drug delivery due to the avoidance of gastric degradation and hepatic metabolism, in addition to easy accessibility. Although offering numerous attractive advantages, many available transdermal systems are not able to deliver drugs and other compounds

  8. Evaluation of Extraction Protocols for Simultaneous Polar and Non-Polar Yeast Metabolite Analysis Using Multivariate Projection Methods

    OpenAIRE

    Nicolas P. Tambellini; Weljie, Aalim M.; Turner, Raymond J.; Vanina Zaremberg

    2013-01-01

    Metabolomic and lipidomic approaches aim to measure metabolites or lipids in the cell. Metabolite extraction is a key step in obtaining useful and reliable data for successful metabolite studies. Significant efforts have been made to identify the optimal extraction protocol for various platforms and biological systems, for both polar and non-polar metabolites. Here we report an approach utilizing chemoinformatics for systematic comparison of protocols to extract both from a single sample of t...

  9. A systematic review of medication administration errors with transdermal patches.

    Science.gov (United States)

    Lampert, Anette; Seiberth, Jasmin; Haefeli, Walter E; Seidling, Hanna M

    2014-08-01

    Transdermal patches provide an attractive route of drug delivery with considerable advantages over other routes of administration, for example maintenance of constant plasma drug levels and convenient usage. However, medication administration errors abound with this dosage form and frequently result in harm or treatment failure. A systematic literature search was conducted according to the Preferred Reporting Items for Systematic Reviews and Meta-Analyses guidelines using appropriate keywords to identify articles reporting faulty transdermal patch administration. Common pitfalls and errors that were identified through the systematic literature search were discussed alongside individual steps of the transdermal patch administration process. The systematic investigation of published errors illustrated that every step in the transdermal patch administration process is prone to errors. Thereby, the lack of knowledge and awareness of the importance of a correct administration practice were a major source of risk. Based on the identified errors and causes of errors prevention strategies were developed as a first step in avoiding transdermal patch administration errors.

  10. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-01

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  11. Simultaneous determination of multi-class veterinary drugs in chicken processed foods and muscle using solid-supported liquid extraction clean-up.

    Science.gov (United States)

    Yoshikawa, Souichi; Nagano, Chieko; Kanda, Maki; Hayashi, Hiroshi; Matsushima, Yoko; Nakajima, Takayuki; Tsuruoka, Yumi; Nagata, Marie; Koike, Hiroshi; Sekimura, Kotaro; Hashimoto, Tsuneo; Takano, Ichiro; Shindo, Tetsuya

    2017-07-01

    We developed a simultaneous determination method for 37 veterinary drugs in two chicken processed foods (deep-fried chicken and non-fried chicken cutlet) and muscle via liquid chromatography-mass spectrometry. The veterinary drugs belong to 7 different classes, including 4 antifolics, 4 benzimidazoles, 5 macrolides, 7 polyethers, 2 quinolones, 7 sulfonamides, and 8 other classes. The samples were extracted with ethyl acetate followed by acetonitrile with salt and buffers extraction. The two-step extraction enabled analyte extraction from highly lipid samples. The clean-up procedure, a solid-supported liquid extraction clean-up using a diatomaceous earth mini-cartridge, eliminated lipid co-extraction. The prepared sample matrix did not have an effect on the 36 analytes. The method was validated in accordance with the requirements of Japanese validation guidelines. Almost all targeted veterinary drugs successfully satisfied the guideline criteria in the three types of food matrices. The method exhibited recoveries of 70-105%, and the precision of repeatability and within-laboratory reproducibility ranged from 1 to 11% and 1 to 15%, respectively. The limits of quantification were estimated to range from 0.2 to 1.0μg/kg. Applying this method to samples commercially available in Tokyo, residues were detected in 3 out of 26 deep-fried chickens, 5 out of 20 non-fried chicken cutlets, and 17 out of 39 chicken muscles. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Microwave-assisted extraction for the simultaneous determination of Novolac glycidyl ethers, bisphenol A diglycidyl ether, and its derivatives in canned food using HPLC with fluorescence detection.

    Science.gov (United States)

    Zhang, Hong; Xue, Ming; Lu, Yanbin; Dai, Zhiyuan; Wang, Honghai

    2010-02-01

    A microwave-assisted extraction (MAE) protocol and an efficient HPLC analysis method were first developed for the fast extraction and simultaneous determination of bisphenol F diglycidyl ether (Novolac glycidyl ether 2-Ring), Novolac glycidyl ether 3-Ring, Novolac glycidyl ether 4-Ring, Novolac glycidyl ether 5-Ring, Novolac glycidyl ether 6-Ring, bisphenol A diglycidyl ether, bisphenol A (2,3-dihydroxypropyl) glycidyl ether, bisphenol A (3-chloro-2-hydroxypropyl) glycidyl ether, bisphenol A bis(3-chloro-2-hydroxypropyl) ether, bisphenol A (3-chloro-2-hydroxypropyl) (2,3-dihydroxypropyl) ether in canned fish and meat. After being optimized in terms of solvents, microwave power and irradiation time, MAE was selected to carry out the extraction of ten target compounds. Analytes were purified by poly(styrene-co-divinylbenzene) SPE columns and determined by HPLC-fluorescence detection. LOD varied from 0.79 to 3.77 ng/g for different target compounds based on S/N=3; LOQ were from 2.75 to 10.92 ng/g; the RSD for repeatability were <8.64%. The analytical recoveries ranged from 70.46 to 103.44%. This proposed method was successfully applied to 16 canned fish and meat, and the results acquired were in good accordance with the studies reported. Compared with the conventional liquid-liquid extraction and ultrasonic extraction, the optimized MAE approach gained the higher extraction efficiency (20-50% improved).

  13. Optimization of an analytical methodology for the simultaneous determination of different classes of ultraviolet filters in cosmetics by pressurized liquid extraction-gas chromatography tandem mass spectrometry.

    Science.gov (United States)

    Vila, Marlene; Lamas, J Pablo; Garcia-Jares, Carmen; Dagnac, Thierry; Llompart, Maria

    2015-07-31

    A methodology based on pressurized liquid extraction (PLE) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for the simultaneous analysis of different classes of UV filters including methoxycinnamates, benzophenones, salicylates, p-aminobenzoic acid derivatives, and others in cosmetic products. The extractions were carried out in 1mL extraction cells and the amount of sample extracted was only 100mg. The experimental conditions, including the acetylation of the PLE extracts to improve GC performance, were optimized by means of experimental design tools. The two main factors affecting the PLE procedure such as solvent type and extraction temperature were assessed. The use of a matrix matched approach consisting of the addition of 10μL of diluted commercial cosmetic oil avoided matrix effects. Good linearity (R(2)>0.9970), quantitative recoveries (>80% for most of compounds, excluding three banned benzophenones) and satisfactory precision (RSDcosmetic formulations including sunscreens, hair products, nail polish, and lipsticks, amongst others. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Simultaneous extraction of acetylsalicylic acid and salicylic acid from human plasma and simultaneous estimation by liquid chromatography and atmospheric pressure chemical ionization/tandem mass spectrometry detection. Application to a pharmacokinetic study.

    Science.gov (United States)

    Nirogi, Ramakrishna; Kandikere, Vishwottam; Mudigonda, Koteshwara; Ajjala, Devender; Suraneni, Ramakrishna; Thoddi, Parthasarathi

    2011-01-01

    A simple analytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in atmospheric chemical ionization mode (APCI) for the simultaneous estimation of acetylsalicylic acid (ASA, CAS 50-78-2) and its active metabolite salicylic acid (SA, CAS 69-72-7) in human plasma has been developed and validated. ASA and SA were analyzed simultaneously despite differences in plasma concentration ranges of ASA and SA after oral administration of ASA. In spite of having different chemical, ionization and chromatographic properties, ASA and SA were extracted simultaneously from the plasma sample using acetonitrile protein precipitation followed by liquid-liquid extraction. The analytes were separated on a reversed phase column with rapid gradient program using mobile phase consisting of ammonium acetate buffer and methanol. The structural analogue diclofenac was used as an internal standard. The multiple reaction monitoring (MRM) transitions m/z 179 --> 137 for ASA, m/z 137 --> 65 for SA and m/z 294 --> 250 for IS were used. The assay exhibited a linear dynamic range of 0.02-10 microg/mL for ASA and 0.1-50 microg/mL for SA. The between-batch precision (%CV) ranged from 2.1 to 7.9% for ASA and from 0.2 to 5.2% for SA. The between-batch accuracy ranged from 95.4 to 96.7% for ASA and from 94.6 to 111.3% for SA. The validated method was successfully applied for the evaluation of pharmacokinetics of ASA after single oral administration of 650 mg test formulation versus two 325 mg reference formulations of ASA in human subjects.

  15. [Study on preparation of testosterone undecanoate ethosomes and its in vitro transdermal penetration].

    Science.gov (United States)

    Meng, Shu; Yang, Li-Qun; Ma, Li-Ying; Guo, Jing; Li, Miao; Yang, Dan

    2013-05-01

    Ethosomes, as a new vector for transdermal drug delivery, could obviously improve the transdermal penetration of drugs. In this study, we prepared testosterone undecanoate ethosomes, with TU ethosomes as the basic remedy, to determine its appearance, particle size, entrapment efficiency (EE) and membrane fluidity. Meanwhile, a transdermal test was conducted in mice, in order to determine the permeability characteristics of ethosomes as a vector for transdermal drug delivery, and compare transdermal behaviors of TU ethosomes, liposomes and their ethanol solutions.

  16. Simultaneous extraction and determination of HBCD isomers and TBBPA by ASE and LC-MSMS in fish

    NARCIS (Netherlands)

    Dam, ten G.; Pardo, O.; Traag, W.A.; Lee, van der M.K.; Peters, R.J.B.

    2012-01-01

    Since the EFSA enquired a call for data for TBBPA and HBCD in 2009, the analytical determination of these compounds in food became of regulatory interest. Therefore, a method for the simultaneous determination of TBBPA and the three major HBCD stereoisomers was developed. Conventional techniques

  17. Effects of cinnamene enhancers on transdermal delivery of ligustrazine hydrochloride.

    Science.gov (United States)

    Zhang, Chun-feng; Yang, Zhong-lin; Luo, Jia-bo; Zhu, Quan-hong; Zhao, Hui-nan

    2007-09-01

    Cinnamene compounds, cinnamic acid, cinnamaldehyde and cinnamic alcohol, were employed as enhancers. The effects and mechanisms of penetration promoters on the in vitro percutaneous absorption of ligustrazine hydrochloride across hairless porcine dorsal skin were investigated. Transdermal fluxes of ligustrazine hydrochloride through porcine skin were determined in vitro by Franz-type diffusion cells. The results indicated that the penetration flux of ligustrazine hydrochloride by cinnamic acid was the greatest. Significant statistical differences (Pextract the stratum corneum lipids to different extent. Morphological changes of the skin treated with enhancers were monitored by a scanning electron microscope. It was demonstrated that the extraction of the stratum corneum lipids by the enhancers led to the disruption of stratum corneum and the desquamation of stratum corneum flake. Apparent density was newly proposed to estimate the desquamated extent of stratum corneum flake. Correlation analysis revealed that there was a linear relationship between apparent density and decrease in peak area. The results showed that the permeation enhancement mechanisms of cinnamene were pleiotropic ones, including disordering the lipids, extracting the lipids and competitive hydrogen bonding between cinnamene enhancers and amides of ceramide head groups in stratum corneum.

  18. Simultaneous determination of quercetin, rutin and kaempferol in the leaf extracts of Moringa oleifera Lam. and Raphinus sativus Linn. by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Devaraj, Venkatapura C; Krishna, Burdipad G; Viswanatha, Gollapalle L

    2011-09-01

    To develop a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze quercetin (QU), rutin (RU) and kaempferol (KA) simultaneously in the leaf extracts of Moringa oleifera Lam. and Raphinus sativus Linn. Samples were prepared by extracting the leaves of the M. oleifera and R. sativus by cold-maceration technique using 90% ethanol. Chromatographic separation was operated with a mixture of 0.2% formic acid in water and acetonitrile at a flow rate of 0.4 mL/min on a Phenomenex Gemini C18 column with a total run time of 5.01 min. The MS/MS ion transitions monitored were 303.03 to 153.1 for QU, 611.1 to 303.1 for RU, 287.1 to 153.2 for KA and 180.1 to 110.1 for internal standard. The lower limit of quantitation achieved for QU, RU and KA was 5 ng/mL and the linearity was observed from 5 to 2 000 ng/mL. The correlation coefficients of linear regression analysis were 0.994 6, 0.995 1 and 0.996 9 for QU, RU and KA, respectively. The results indicate that the LC-MS/MS method is fast and sensitive and may provide excellent specificity for simultaneous determination of QU, RU and KA in leaf extracts of M.oleifera and R.sativus.

  19. Simultaneous extraction of polycyclic aromatic hydrocarbons through the complete dissolution of solid biological samples in sodium hydroxide/urea/thiourea aqueous solution.

    Science.gov (United States)

    Mohammad, Sedigheh Ale; Ghanemi, Kamal; Larki, Arash

    2016-12-09

    In order to precisely and simultaneously extract polycyclic aromatic hydrocarbons (PAHs) for measurement using a high performance liquid chromatography-fluorescence detector (HPLC-FL), a novel sample preparation method was developed. This method is based on the complete and fast dissolution of biological samples in a new non-alcoholic alkaline medium. A solution composed of NaOH/urea/thiourea at an optimized ratio was used for complete dissolution of approximately 0.25g dried fish samples within 20min. The proposed method was conducted at 10°C and under atmospheric pressure to obtain a stable and highly homogeneous solution, without the need for microwaves or any other apparatus. This process operates at considerably lower temperature than conventional methods and provides an opportunity to simultaneously extract the target analytes from their matrices by adding the extracting solvent in the initial steps of the dissolution; this process greatly reduced the time of analysis and the loss of analytes via vaporization. Several key parameters were identified and their effects on precision and extraction recoveries were investigated. Linearity over a calibration range of 1.0-100 and 2.5-100ngg(-1) was achieved, with high coefficients of determination (r(2)) ranging between 0.9987 and 0.9998. Based on relative standard deviations (n=5), the intra-day and inter-day precisions of the spiked PAHs were found to be better than 3.1% and 3.2%, respectively, at a concentration level of 25ngg(-1). The recoveries of PAH from spiked marine fish tissues and shrimp samples were in the range of 90.6%-100.4%. The spiked samples were also treated with the alcoholic alkaline and Soxhlet extraction methods in order to provide a comparison. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Conductive polymer nanotube patch for fast and controlled in vivo transdermal drug delivery

    Science.gov (United States)

    Nguyen, Thao M.

    Transdermal drug delivery has created new applications for existing therapies and offered an alternative to the traditional oral route where drugs can prematurely metabolize in the liver causing adverse side effects. Opening the transdermal delivery route to large hydrophilic drugs is one of the greatest challenges due to the hydrophobicity of the skin. However, the ability to deliver hydrophilic drugs using a transdermal patch would provide a solution to problems of other delivery methods for hydrophilic drugs. The switching of conductive polymers (CP) between redox states cause simultaneous changes in the polymer charge, conductivity, and volume—properties that can all be exploited in the biomedical field of controlled drug delivery. Using the template synthesis method, poly(3,4-ethylenedioxythiophene (PEDOT) nanotubes were synthesized electrochemically and a transdermal drug delivery patch was successfully designed and developed. In vitro and in vivo uptake and release of hydrophilic drugs were investigated. The relationship between the strength of the applied potential and rate of drug release were also investigated. Results revealed that the strength of the applied potential is proportional to the rate of drug release; therefore one can control the rate of drug release by controlling the applied potential. The in vitro studies focused on the kinetics of the drug delivery system. It was determined that the drug released mainly followed zero-order kinetics. In addition, it was determined that applying a releasing potential to the transdermal drug delivery system lead to a higher release rate constant (up to 7 times greater) over an extended period of time (˜24h). In addition, over 24 hours, an average of 80% more model drug molecules were released with an applied potential than without. The in vivo study showed that the drug delivery system was capable of delivering model hydrophilic drugs molecules through the dermis layer of the skin within 30 minutes

  1. Influence of monoolein on progesterone transdermal delivery

    Directory of Open Access Journals (Sweden)

    Wanessa de Souza Cardoso Quintão

    2015-12-01

    Full Text Available abstract This work aimed to investigate in vitro the influence of monoolein (MO on progesterone (PG transdermal delivery and skin retention. Information about the role of MO as an absorption enhancer for lipophilic molecules can help on innovative product development capable of delivering the hormone through the skin in a consistent manner, improving transdermal therapy of hormonal replacement. MO was dispersed in propylene glycol under heat at concentrations of 0% (control, 5% w/w, 10% w/w and 20% w/w. Then, 0.6% of PG (w/w was added to each formulation. Permeation profile of the hormone was determined in vitro for 48 h using porcine skin in Franz diffusion cells. PG permeation doubled when 5% (w/w of MO was present in formulation in comparison to both the control and higher MO concentrations (10% and 20% w/w. An equal trend was observed for PG retention in stratum corneum (SC and reminiscent skin (E+D. PG release rates from the MO formulations, investigated using cellulose membranes, revealed that concentrations of MO higher than 5% (w/w hindered PG release, which indeed negatively reflected on the hormone permeation through the skin. In conclusion, this work demonstrated the feasibility of MO addition (at 5% w/w in formulations as a simple method to increase transdermal PG delivery for therapies of hormonal replacement. In contrast, higher MO concentrations (from 10% to 20% w/w can control active release, and this approach could be extrapolated to other lipophilic, low-molecular-weight molecules.

  2. Evaluation of extraction protocols for simultaneous polar and non-polar yeast metabolite analysis using multivariate projection methods.

    Science.gov (United States)

    Tambellini, Nicolas P; Zaremberg, Vanina; Turner, Raymond J; Weljie, Aalim M

    2013-07-23

    Metabolomic and lipidomic approaches aim to measure metabolites or lipids in the cell. Metabolite extraction is a key step in obtaining useful and reliable data for successful metabolite studies. Significant efforts have been made to identify the optimal extraction protocol for various platforms and biological systems, for both polar and non-polar metabolites. Here we report an approach utilizing chemoinformatics for systematic comparison of protocols to extract both from a single sample of the model yeast organism Saccharomyces cerevisiae. Three chloroform/methanol/water partitioning based extraction protocols found in literature were evaluated for their effectiveness at reproducibly extracting both polar and non-polar metabolites. Fatty acid methyl esters and methoxyamine/trimethylsilyl derivatized aqueous compounds were analyzed by gas chromatography mass spectrometry to evaluate non-polar or polar metabolite analysis. The comparative breadth and amount of recovered metabolites was evaluated using multivariate projection methods. This approach identified an optimal protocol consisting of 64 identified polar metabolites from 105 ion hits and 12 fatty acids recovered, and will potentially attenuate the error and variation associated with combining metabolite profiles from different samples for untargeted analysis with both polar and non-polar analytes. It also confirmed the value of using multivariate projection methods to compare established extraction protocols.

  3. Evaluation of Extraction Protocols for Simultaneous Polar and Non-Polar Yeast Metabolite Analysis Using Multivariate Projection Methods

    Directory of Open Access Journals (Sweden)

    Nicolas P. Tambellini

    2013-07-01

    Full Text Available Metabolomic and lipidomic approaches aim to measure metabolites or lipids in the cell. Metabolite extraction is a key step in obtaining useful and reliable data for successful metabolite studies. Significant efforts have been made to identify the optimal extraction protocol for various platforms and biological systems, for both polar and non-polar metabolites. Here we report an approach utilizing chemoinformatics for systematic comparison of protocols to extract both from a single sample of the model yeast organism Saccharomyces cerevisiae. Three chloroform/methanol/water partitioning based extraction protocols found in literature were evaluated for their effectiveness at reproducibly extracting both polar and non-polar metabolites. Fatty acid methyl esters and methoxyamine/trimethylsilyl derivatized aqueous compounds were analyzed by gas chromatography mass spectrometry to evaluate non-polar or polar metabolite analysis. The comparative breadth and amount of recovered metabolites was evaluated using multivariate projection methods. This approach identified an optimal protocol consisting of 64 identified polar metabolites from 105 ion hits and 12 fatty acids recovered, and will potentially attenuate the error and variation associated with combining metabolite profiles from different samples for untargeted analysis with both polar and non-polar analytes. It also confirmed the value of using multivariate projection methods to compare established extraction protocols.

  4. Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

    Science.gov (United States)

    Sheikhian, Leila; Bina, Sedigheh

    2016-01-15

    In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Combined ion-pair extraction and gas chromatography-mass spectrometry for the simultaneous determination of diamines, polyamines and aromatic amines in Port wine and grape juice.

    Science.gov (United States)

    Fernandes, J O; Ferreira, M A

    2000-07-21

    An accurate and very sensitive method which allows for the simultaneous determination of the diamines (1,3-diaminopropane, putrescine and cadaverine), of the polyamines (spermidine and spermine), and of the aromatic amines (beta-phenylethylamine and tyramine) found in Port wines and corresponding grape juices is presented. Sample clean-up consisted of the extraction of the amines with the ion-pairing reagent bis-2-ethylhexylphosphate dissolved in chloroform followed by a back-extraction with 0.1 M HCl. The hydrochloric extract obtained was dried and the amines were further derivatized with heptafluorobutyric anhydride and analyzed by GC-MS in the selected ion-monitoring mode, with a total run time of 18 min. Under the adopted conditions, the extraction of all the studied compounds was almost complete and the obtained extracts were free of potential interferents present in the samples, namely sugars, and most of the amino acids and polyphenols. Via the use of a set of five selected internal standards (amphetamine, [2H8]putrescine, 1,7-diaminoheptane, norspermidine and norspermine), the data obtained from the linearity, repeatability and recovery experiments were very good for all the compounds assayed. The corresponding limits of detection were invariably below 10 microg l(-1). The method was successfully applied to measure the content of biogenic amines in twelve young and five aged Port wine samples, eleven grape juice samples as well as in ten Portuguese red and white table wines. Results are presented and briefly discussed.

  6. Development of an ionic liquid-based microwave-assisted method for simultaneous extraction and distillation for determination of proanthocyanidins and essential oil in Cortex cinnamomi.

    Science.gov (United States)

    Liu, Ye; Yang, Lei; Zu, Yuangang; Zhao, Chunjian; Zhang, Lin; Zhang, Ying; Zhang, Zhonghua; Wang, Wenjie

    2012-12-15

    Cortex cinnamomi is associated with many health benefits and is used in the food and pharmaceutical industries. In this study, an efficient ionic liquid-based microwave-assisted simultaneous extraction and distillation (ILMSED) technique was used to extract cassia oil and proanthocyanidins from Cortex cinnamomi; these were quantified by gas chromatography/mass spectrometry (GC-MS) and the vanillin-HCl colorimetric method, respectively. 0.5M 1-butyl-3-methylimidazolium bromide ionic liquid was selected as solvent. The optimum parameters of dealing with 20.0 g sample were 230 W microwave irradiation power, 15 min microwave extraction time and 10 liquid-solid ratio. The yields of essential oil and proanthocyanidins were 1.24 ± 0.04% and 4.58 ± 0.21% under the optimum conditions. The composition of the essential oil was analysed by GC-MS. Using the ILMSED method, the energy consumption was reduced and the extraction yields were improved. The proposed method was validated using stability, repeatability, and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the extraction of both the essential oil and proanthocyanidins from Cortex cinnamomi. Copyright © 2012 Elsevier Ltd. All rights reserved.

  7. An anaphylactic reaction to transdermal delivered fentanyl.

    Science.gov (United States)

    Dewachter, P; Lefebvre, D; Kalaboka, S; Bloch-Morot, E

    2009-09-01

    Immediate allergic hypersensitivity reactions with fentanyl are rarely reported. We diagnosed a presumably IgE-mediated allergic hypersensitivity reaction comprising generalized erythema and bronchospasm 4 h after the first-time application of transdermal fentanyl. Prick test remained negative with fentanyl whereas an intradermal test (IDT) with fentanyl was positive (dilution 10(-2)). Cross-reactivity was found with sufentanil but not with remifentanil. The diagnosis was supported by the clinical history and a positive IDT with fentanyl. This case report confirms the need for a systematic allergological investigation in case of immediate hypersensitivity reactions for all drugs and all modes of administration.

  8. Development of cup shaped microneedle array for transdermal drug delivery.

    Science.gov (United States)

    Vinayakumar, Kadayar B; Hegde, Gopal M; Ramachandra, Subbaraya G; Nayak, Mangalore M; Dinesh, Narasimhian S; Rajanna, Konandur

    2015-06-08

    Microneedle technology is one of the attractive methods in transdermal drug delivery. However, the clinical applications of this method are limited owing to: complexity in the preparation of multiple coating solutions, drug leakage while inserting the microneedles into the skin and the outer walls of the solid microneedle can hold limited quantity of drug. Here, the authors present the fabrication of an array of rectangular cup shaped silicon microneedles, which provide for reduced drug leakage resulting in improvement of efficiency of drug delivery and possibility of introducing multiple drugs. The fabricated solid microneedles with rectangular cup shaped tip have a total height of 200 μm. These cup shaped tips have dimensions: 60 × 60 μm (length × breadth) with a depth of 60 μm. The cups are filled with drug using a novel in-house built drop coating system. Successful drug dissolution was observed when the coated microneedle was used on mice. Also, using the above method, it is possible to fill the cups selectively with different drugs, which enables simultaneous multiple drug delivery.

  9. Biodiesel production by simultaneous extraction and conversion of total lipids from microalgae, cyanobacteria, and wild mixed-cultures.

    Science.gov (United States)

    Wahlen, Bradley D; Willis, Robert M; Seefeldt, Lance C

    2011-02-01

    Microalgae have been identified as a potential biodiesel feedstock due to their high lipid productivity and potential for cultivation on marginal land. One of the challenges in utilizing microalgae to make biodiesel is the complexities of extracting the lipids using organic solvents followed by transesterification of the extracts to biodiesel. In the present work, reaction conditions were optimized that allow a single step extraction and conversion to biodiesel in high yield from microalgae. From the optimized conditions, it is demonstrated that quantitative conversion of triglycerides from several different microalgae and cyanobacteria could be achieved, including from mixed microbial biomass collected from a municipal wastewater lagoon. Evidence is presented that for some samples, significantly more biodiesel can be produced than would be expected from available triglycerides, indicating conversion of fatty acids contained in other molecules (e.g., phospholipids) using this approach. The effectiveness of the approach on wet algae is also reported. Copyright © 2010 Elsevier Ltd. All rights reserved.

  10. Simultaneous determination of 16 polycyclic aromatic hydrocarbons in reclaimed water using solid-phase extraction followed by ultra-performance convergence chromatography with photodiode array detection.

    Science.gov (United States)

    Zhang, Yun; Xiao, Zhiyong; Lv, Surong; Du, Zhenxia; Liu, Xiaoxia

    2016-03-01

    A new fast and effective analysis method has been developed to simultaneously determine 16 polycyclic aromatic hydrocarbons in reclaimed water samples by ultra-performance convergence chromatography with photodiode array detection and solid-phase extraction. The parameters of ultra-performance convergence chromatography on the separation behaviors and the crucial condition of solid-phase extraction were investigated systematically. Under optimal conditions, the 16 polycyclic aromatic hydrocarbons could be separated within 4 min. The limits of detection and quantification were in the range of 0.4-4 and 1-10 μg/L in water, respectively. This approach has been applied to a real industrial wastewater treatment plant successfully. The results showed that polycyclic aromatic hydrocarbons were dramatically decreased after chemical treatment procedure, and the oxidation procedure was effective to remove trace polycyclic aromatic hydrocarbons. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Wine yeast molecular typing using a simplified method for simultaneously extracting mtDNA, nuclear DNA and virus dsRNA.

    Science.gov (United States)

    Maqueda, Matilde; Zamora, Emiliano; Rodríguez-Cousiño, Nieves; Ramírez, Manuel

    2010-04-01

    Quick and accurate methods are required for the identification of industrial, environmental, and clinical yeast strains. We propose a rapid method for the simultaneous extraction of yeast mtDNA, nuclear DNA, and virus dsRNA. It is simpler, cheaper, and faster than the previously reported methods. It allows one to choose among a broad range of molecular analysis approaches for yeast typing, avoiding the need to use of several different methods for the separate extraction of each nucleic acid type. The application of this method followed by the combined analysis of mtDNA and dsRNA (ScV-M and W) is a highly attractive option for fast and efficient wine yeast typing.

  12. Simultaneous molecular formula determinations of natural compounds in a plant extract using 15 T Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Park, Kyu Hwan; Kim, Min Sun; Baek, Sun Jong; Bae, Ik Hyun; Seo, Sang-Wan; Kim, Jongjin; Shin, Yong Kook; Lee, Yong-Moon; Kim, Hyun Sik

    2013-01-01

    Plant extracts are a reservoir of pharmacologically active substances; however, conventional analytical methods can analyze only a small portion of an extract. Here, we report a high-throughput analytical method capable of determining most phytochemicals in a plant extract and of providing their molecular formulae from a single experiment using ultra-high-resolution electrospray ionization mass spectrometry (UHR ESI MS). UHR mass profiling was used to analyze natural compounds in a 70% ethanol ginseng extract, which was directly infused into a 15 T Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometer for less than 10 min without a separation process. The UHR FT-ICR MS yielded a mass accuracy of 0.5 ppm and a mass resolving power (m/Δm) of 1,000,000-270,000 for the range m/z 290-1,100. The mass resolution was sufficient to resolve the isotopic fine structure (IFS) of many compounds in the extract. After noise removal from 1,552 peaks, 405 compounds were detected. The molecular formulae of 123 compounds, including 33 ginsenosides, were determined using the observed IFS, exact monoisotopic mass, and exact mass difference. Liquid chromatography (LC)/FT-ICR MS of the extract was performed to compare the high-throughput performance of UHR ESI FT-ICR MS. The LC/FT-ICR MS detected only 129 compounds, including 19 ginsenosides. The result showed that UHR ESI FT-ICR MS identified three times more compounds than LC/FT-ICR MS and in a relatively shorter time. The molecular formula determination by UHR FT-ICR MS was validated by LC and tandem MS analyses of three known ginsenosides. UHR mass profiling of a plant extract by 15 T FT-ICR MS showed that multiple compounds were simultaneously detected and their molecular formulae were decisively determined by a single experiment with ultra-high mass resolution and mass accuracy. Simultaneous molecular determination of multiple natural products by UHR ESI FT-ICR MS would be a powerful method to profile a wide

  13. Device-assisted transdermal drug delivery.

    Science.gov (United States)

    Lee, Hyunjae; Song, Changyeong; Baik, Seungmin; Kim, Dokyoon; Hyeon, Taeghwan; Kim, Dae-Hyeong

    2017-09-01

    Transdermal drug delivery is a prospective drug delivery strategy to complement the limitations of conventional drug delivery systems including oral and injectable methods. This delivery route allows both convenient and painless drug delivery and a sustained release profile with reduced side effects. However, physiological barriers in the skin undermine the delivery efficiency of conventional patches, limiting drug candidates to small-molecules and lipophilic drugs. Recently, transdermal drug delivery technology has advanced from unsophisticated methods simply relying on natural diffusion to drug releasing systems that dynamically respond to external stimuli. Furthermore, physical barriers in the skin have been overcome using microneedles, and controlled delivery by wearable biosensors has been enabled ultimately. In this review, we classify the evolution of advanced drug delivery strategies based on generations and provide a comprehensive overview. Finally, the recent progress in advanced diagnosis and therapy through customized drug delivery systems based on real-time analysis of physiological cues is highlighted. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Fluorescent Penetration Enhancers for Transdermal Applications

    Science.gov (United States)

    Seto, Jennifer E.; Polat, Baris E.; VanVeller, Brett; Lopez, Renata F.V.; Langer, Robert; Blankschtein, Daniel

    2011-01-01

    Chemical penetration enhancers are often used to enhance transdermal drug delivery. However, the fundamental mechanisms that govern the interactions between penetration enhancers and skin are not fully understood. Therefore, the goal of this work was to identify naturally fluorescent penetration enhancers (FPEs) in order to utilize well-established fluorescence techniques to directly study the behavior of FPEs within skin. In this study, 12 fluorescent molecules with amphiphilic characteristics were evaluated as skin penetration enhancers. Eight of the molecules exhibited significant activity as skin penetration enhancers, determined using skin current enhancement ratios. In addition, to illustrate the novel, direct, and non-invasive visualization of the behavior of FPEs within skin, three case studies involving the use of two-photon fluorescence microscopy (TPM) are presented, including visualizing glycerol-mitigated and ultrasound-enhanced FPE skin penetration. Previous TPM studies have indirectly visualized the effect of penetration enhancers on skin by using a fluorescent dye to probe the transdermal pathways of the enhancer. These effects can now be directly visualized and investigated using FPEs. Finally, future studies are proposed for generating FPE design principles. The combination of FPEs with fluorescence techniques represents a useful novel approach for obtaining physical insights on the behavior of penetration enhancers within skin. PMID:22062691

  15. Microneedles: an emerging transdermal drug delivery system.

    Science.gov (United States)

    Bariya, Shital H; Gohel, Mukesh C; Mehta, Tejal A; Sharma, Om Prakash

    2012-01-01

    One of the thrust areas in drug delivery research is transdermal drug delivery systems (TDDS) due to their characteristic advantages over oral and parenteral drug delivery systems. Researchers have focused their attention on the use of microneedles to overcome the barrier of the stratum corneum. Microneedles deliver the drug into the epidermis without disruption of nerve endings. Recent advances in the development of microneedles are discussed in this review for the benefit of young scientists and to promote research in the area. Microneedles are fabricated using a microelectromechanical system employing silicon, metals, polymers or polysaccharides. Solid coated microneedles can be used to pierce the superficial skin layer followed by delivery of the drug. Advances in microneedle research led to development of dissolvable/degradable and hollow microneedles to deliver drugs at a higher dose and to engineer drug release. Iontophoresis, sonophoresis and electrophoresis can be used to modify drug delivery when used in concern with hollow microneedles. Microneedles can be used to deliver macromolecules such as insulin, growth hormones, immunobiologicals, proteins and peptides. Microneedles containing 'cosmeceuticals' are currently available to treat acne, pigmentation, scars and wrinkles, as well as for skin tone improvement. Literature survey and patents filled revealed that microneedle-based drug delivery system can be explored as a potential tool for the delivery of a variety of macromolecules that are not effectively delivered by conventional transdermal techniques. © 2011 The Authors. JPP © 2011 Royal Pharmaceutical Society.

  16. Optimized methodology for the simultaneous extraction of glucosinolates, phenolic compounds and antioxidant activity from maca (Lepidium meyenii)

    NARCIS (Netherlands)

    Campos, D.; Chirinos, R.; Barreto, O.; Noratto, G.; Pedreschi Plasencia, R.P.

    2013-01-01

    Maca is a highly appreciated Andean crop with multiple attributed health claims due to its assortment of bioactive compounds. The extraction parameters of glucosinolates (GLs), total phenolic compounds (TPC) and antioxidant capacity (AC) of maca (Lepidium meyenii) hypocotyls were optimized using

  17. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    Science.gov (United States)

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-03

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  18. Development of a new sorptive extraction method based on simultaneous direct and headspace sampling modes for the screening of polycyclic aromatic hydrocarbons in water samples.

    Science.gov (United States)

    Triñanes, Sara; Pena, Ma Teresa; Casais, Ma Carmen; Mejuto, Ma Carmen

    2015-01-01

    A new straightforward and inexpensive sample screening method for both EPA and EU priority polycyclic aromatic hydrocarbons (PAHs) in water has been developed. The method is based on combined direct immersion and headspace (DIHS) sorptive extraction, using low-cost disposable material, coupled to ultraperformance liquid chromatography with fluorescence and UV detection (UPLC-FD-UV). Extraction parameters, such as the sampling mode, extraction time and ionic strength were investigated in detail and optimized. Under optimized conditions, water samples (16 mL) were concentrated in silicone disks by headspace (HS) and direct immersion (DI) modes simultaneously, at room temperature for 9h for the majority of the 24 studied compounds. Ultrasound-assisted desorption of extracted analytes in acetonitrile was carried out also at room temperature. The optimized chromatographic method provided a good linearity (R≥0.9991) and a broad linear range for all studied PAHs. The proposed analytical procedure exhibited a good precision level with relative standard deviations below 15% for all analytes. Quantification limits between 0.7 and 2.3 µg L(-1) and 0.16 and 3.90 ng L(-1) were obtained for compounds analyzed by UV (acenaphtylene, cyclopenta[c,d]pyrene and benzo[j]fluoranthene) and fluorescence, respectively. Finally, the proposed method was applied to the determination of PAHs in different real tap, river and wastewater samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

    Science.gov (United States)

    Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

    2016-09-01

    The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

  20. Ultrasonic nebulization extraction assisted dispersive liquid-liquid microextraction followed by gas chromatography for the simultaneous determination of six parabens in cosmetic products.

    Science.gov (United States)

    Wei, Hongmin; Yang, Jinjuan; Zhang, Hanqi; Shi, Yuhua

    2014-09-01

    A simple, rapid, and efficient method of ultrasonic nebulization extraction assisted dispersive liquid-liquid microextraction was developed for the simultaneous determination of six parabens in cosmetic products. The analysis was carried out by gas chromatography. Water was used as the dispersive solvent instead of traditional organic disperser. The experimental factors affecting the extraction yield, such as the extraction solvent and volume, extraction time, dispersive solvent and volume, ionic strength, and centrifuging condition were studied and optimized in detail. The limit of detections for the target analytes were in the range of 2.0-9.5 μg/g. Good linear ranges were obtained with the coefficients ranging from 0.9934 to 0.9969. The proposed method was successfully applied to the analysis of six parabens in 16 cosmetic products. The recoveries of the target analytes in real samples ranged from 81.9 to 108.7%, and the relative standard deviations were <5.3%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Selective and simultaneous determination of trace bisphenol A and tebuconazole in vegetable and juice samples by membrane-based molecularly imprinted solid-phase extraction and HPLC.

    Science.gov (United States)

    Wu, Ya-Ting; Zhang, Yan-Hong; Zhang, Meng; Liu, Fei; Wan, Ying-Chun; Huang, Zheng; Ye, Lei; Zhou, Qi; Shi, Yun; Lu, Bin

    2014-12-01

    Nanofibrous molecularly imprinted membranes (nano-MIMs) with multi-analyte selectivity were prepared by encapsulating two types of molecularly imprinted polymer nanoparticles (MIP-NPs) into electrospun polyvinyl alcohol nanofibers. The obtained nano-MIMs maintained high molecular selectivity offered by each of the MIP-NPs. Nano-MIM embedding BPA-imprinted nanoparticles and TBZ-imprinted nanoparticles together showed the highest binding selectivity for acid bisphenol A (BPA) and basic tebuconazole (TBZ). This nano-MIM was used as affinity material of membrane-based molecularly imprinted solid-phase extraction (m-MISPE) to extract trace BPA and TBZ in vegetables and juices simultaneously. The recoveries of BPA and TBZ from different samples were higher than 70.33% with RSDs lower than 9.57%. m-MISPE gave better HPLC separation efficiencies and higher recoveries than conventional SPE based on C18/SCX. Multi-analyte selective m-MISPE combined with HPLC realized selective and simultaneous determination of several trace analytes with opposite charges/polarities in different food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  3. Carbon nanotube-based benzyl polymethacrylate composite monolith as a solid phase extraction adsorbent and a stationary phase material for simultaneous extraction and analysis of polycyclic aromatic hydrocarbon in water.

    Science.gov (United States)

    Al-Rifai, Asma'a; Aqel, Ahmad; Wahibi, Lamya Al; ALOthman, Zeid A; Badjah-Hadj-Ahmed, Ahmed-Yacine

    2018-02-02

    A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m-1 for chrysene at flow rate of 0.5 μL min-1. The method showed a wide linear range (1-500 μg L-1 with R2 more than 0.9938), acceptable extraction repeatability (RSDs extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L-1). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges. Copyright © 2018. Published by Elsevier B.V.

  4. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods.

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-05

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40μg mL-1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08μg mL-1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Topical and transdermal drug delivery: principles and practice

    National Research Council Canada - National Science Library

    Benson, Heather A. E; Watkinson, Adam C

    2012-01-01

    .... Providing an overview of the current science in drug and cosmetic application to and through the skin, Topical and Transdermal Drug Delivery includes treatment of skin conditions, skin permeation...

  6. Diclofenac transdermal patch versus the sustained release tablet: A ...

    African Journals Online (AJOL)

    Conclusion: Transdermal films of diclofenac, formulated with permeation enhancers, may have greater therapeutic advantages over conventional oral tablets in terms of prolonged release and improvement of patient compliance in rheumatoid arthritis. Keywords: Analgesic activity, Diclofenac, Permeation enhancer, ...

  7. 3D printing applications for transdermal drug delivery.

    Science.gov (United States)

    Economidou, Sophia N; Lamprou, Dimitrios A; Douroumis, Dennis

    2018-01-20

    The role of two and three-dimensional printing as a fabrication technology for sophisticated transdermal drug delivery systems is explored in literature. 3D printing encompasses a family of distinct technologies that employ a virtual model to produce a physical object through numerically controlled apparatuses. The applicability of several printing technologies has been researched for the direct or indirect printing of microneedle arrays or for the modification of their surface through drug-containing coatings. The findings of the respective studies are presented. The range of printable materials that are currently used or potentially can be employed for 3D printing of transdermal drug delivery (TDD) systems is also reviewed. Moreover, the expected impact and challenges of the adoption of 3D printing as a manufacturing technique for transdermal drug delivery systems, are assessed. Finally, this paper outlines the current regulatory framework associated with 3D printed transdermal drug delivery systems. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Modified Transdermal Technologies: Breaking the Barriers of Drug ...

    African Journals Online (AJOL)

    In-depth analysis, formulation approaches, applications, advantages and disadvantages of these newer technologies are discussed. Keywords: Transdermal drug delivery, microneedles, macroflux, iontophoresis, ultrasound, powderject, skin abrasion. > Tropical Journal of Pharmaceutical Research Vol. 6 (1) 2007: pp. 633- ...

  9. Using pollen grains as novel hydrophilic solid-phase extraction sorbents for the simultaneous determination of 16 plant growth regulators.

    Science.gov (United States)

    Lu, Qian; Wu, Jian-Hong; Yu, Qiong-Wei; Feng, Yu-Qi

    2014-11-07

    In this article, pollen grains were for the first time used as a hydrophilic solid-phase extraction (HILIC-SPE) sorbent for the determination of 16 plant growth regulators (PGRs) in fruits and vegetables. Fourier transform infrared spectroscopy (FT-IR), scanning electronic microscopy (SEM) and nitrogen sorption porosimetry (NSP) were used to investigate the chemical structure and the surface properties of the pollen grains. Pollen grains exhibited an excellent adsorption capacity for some polar compounds due to their particular functional groups. Several parameters influencing extraction performance were investigated. A green and simple HILIC-SPE-method using pollen grain cartridge for purification of fruit and vegetable extractions, followed by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UHPLC-MS/MS) was established. Good linear relationships were obtained for 16 PGRs with correlation coefficients (R) above 0.9980. The limits of detection (LODs) of 16 PGRs in cucumber were in the range of 0.01-1.10 μg · kg(-1). Reproducibility of the method was evaluated by intra-day and inter-day precisions with relative standard deviations (RSDs), which were less than 14.4%. We successfully applied this methodology to analyze 16 PGRs in 8 different kinds of fruits and vegetables. The recoveries from samples spiked with 16 PGRs were from 80.5% to 119.2%, with relative standard deviations less than 15.0%. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Noninvasive measurement of transdermal drug delivery by impedance spectroscopy

    OpenAIRE

    Arpaia, Pasquale; Cesaro, Umberto; Moccaldi, Nicola

    2017-01-01

    The effectiveness in transdermal delivery of skin permeation strategies (e.g., chemical enhancers, vesicular carrier systems, sonophoresis, iontophoresis, and electroporation) is poorly investigated outside of laboratory. In therapeutic application, the lack of recognized techniques for measuring the actually-released drug affects the scientific concept itself of dosage for topically- and transdermally-delivered drugs. Here we prove the suitability of impedance measurement for assessing the a...

  11. Hybrid electrospun chitosan-phospholipids nanofibers for transdermal drug delivery

    DEFF Research Database (Denmark)

    Mendes, Ana Carina Loureiro; Gorzelanny, Christian; Halter, Natalia

    2016-01-01

    Chitosan (Ch) polysaccharide was mixed with phospholipids (P) to generate electrospun hybrid nanofibers intended to be used as platforms for transdermal drug delivery. Ch/P nanofibers exibithed average diameters ranging from 248 +/- 94 nm to 600 +/- 201 nm, depending on the amount of phospholipid...... culture plate (control). The release of curcumin, diclofenac and vitamin B12, as model drugs, from Ch/P hybrid nanofibers was investigated, demonstrating their potential utilization as a transdermal drug delivery system....

  12. Simultaneous determination of UV-filters and estrogens in aquatic invertebrates by modified quick, easy, cheap, effective, rugged, and safe extraction and liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    He, Ke; Timm, Anne; Blaney, Lee

    2017-08-04

    Ultraviolet-filters (UV-filters) and estrogens have attracted increased attention as contaminants of emerging concern (CECs) due to their widespread occurrence in the environment. Most of these CECs are hydrophobic and have the potential to accumulate in aquatic organisms. To date, co-analysis of UV-filters and estrogens has not been reported due, in part, to the complex environmental matrices. Here, a multi-residue method has been developed for simultaneous determination of five UV-filters and three estrogens in tissue from aquatic and marine organisms. The procedure involved a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction with a novel reverse-solid-phase extraction (reverse-SPE) cleanup in place of dispersive-SPE, followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis. The tissue mass, acetonitrile content, and salt conditions for QuEChERS extraction, along with the reverse-SPE cartridge material and elution conditions, were thoroughly investigated and optimized. Five UV-filters (i.e., 3-(4-methylbenzylidene) camphor, benzophenone-3, ethylhexylmethoxycinnamate, homosalate, and octocrylene) and three estrogens (i.e., estrone, 17β-estradiol, and 17α-ethinylestradiol) were simultaneously analyzed by taking advantage of wrong-way-round ionization in LC-MS/MS. The optimized analytical protocol exhibited good recoveries (>80%) for target compounds and enabled their detection at concentrations as low as 0.2ng/g in 50mg tissue samples. The method was applied to determine concentrations of target analytes in four invertebrates (i.e., Orconectes virilis, Procambarus clarkii, Crassostrea virginica, and Ischadium recurvum). All eight target analytes were detected at least once in the tissue samples, with the highest concentration being 399ng/g of homosalate in O. virilis. These results highlight the ubiquitous bioaccumulation of CECs in aquatic and marine invertebrates. Copyright © 2017 Elsevier B.V. All rights

  13. Drug crystallization - implications for topical and transdermal delivery.

    Science.gov (United States)

    Hadgraft, Jonathan; Lane, Majella E

    2016-06-01

    Crystallization of actives in skin following topical application was suggested by studies in the 1950s and 1960s but is poorly understood. In contrast, the problem of crystallization of actives on skin and in transdermal formulations has been known for many years. With respect to crystallization in skin, this review describes early reports of a skin 'reservoir' and possible reasons underlying its genesis. Techniques to study crystallization on and in skin and in transdermal patches are outlined. The role of the vehicle in skin delivery is emphasised. Studies which have investigated permeation from crystalline particles are described. Approaches to limit crystallization of actives are discussed. Using supersaturation and antinuclean polymers, control of crystal size is possible; controlled release from crystals is also employed in transdermal patches. Drug crystallization has significant implications for topical and transdermal delivery. Approaches have been developed to counteract the issue for transdermal patches but crystallization in and on the skin for other formulations remains unresolved. Greater knowledge of residence time of excipients and their interaction with skin at the molecular level is critical in order to address the problem. This will lay the foundations for better design of topical/transdermal formulations.

  14. Simultaneous Extraction and Identification of Phenolic Compounds in Anoectochilus roxburghii Using Microwave-Assisted Extraction Combined with UPLC-Q-TOF-MS/MS and Their Antioxidant Activities.

    Science.gov (United States)

    Xu, Mengjie; Shao, Qingsong; Ye, Shenyi; Li, Shuailing; Wu, Mei; Ding, Mozhi; Li, Yanjing

    2017-01-01

    This study used MAE and RSM to extract phenolic compounds from Anoectochilus roxburghii, and the optimum conditions defined by the model to give an optimum yield of 1.31%. The antioxidant activity in vitro showed when the concentration of phenolic compounds was reached 1 mg mL-1, the clearance rates were 82.58% for DPPH and 97.62% for ABTS+. In vivo antioxidant experiments used D-galactose to build oxidative damage in healthy Kunming mice. The result showed that the extractions of A. roxburghii can improve the antioxidant ability and the medium and low dose groups had better ability to scavenge free radicals. The UPLC-Q-TOF-MS/MS was developed to identify 21 kinds of phenolic compounds by molecular mass, ms/ms fragmentation, as well as retention time. The result showed that the phenolic compounds of A. roxburghii had significant potential as a natural antioxidant to promote health and to reduce the risk of disease.

  15. Optimization of simultaneous flavanol, phenolic acid, and anthocyanin extraction from grapes using an experimental design: application to the characterization of champagne grape varieties.

    Science.gov (United States)

    Mané, C; Souquet, J M; Ollé, D; Verriés, C; Véran, F; Mazerolles, G; Cheynier, V; Fulcrand, H

    2007-09-05

    Optimization of polyphenol extraction from grape skin, seed, and pulp was performed on Vitis vinifera L. cv. Pinot Noir, by response surface methodology using a Doehlert design. An acidified mixture of acetone/water/methanol was the best solvent for simultaneous extraction of major polyphenol groups from all berry parts, while optimum extraction times and solid-to-liquid ratios varied according to the part. The determined composition from the model agreed with independent experimental results. Analysis of the three Champagne grape varieties showed that proanthocyanidins were the major phenolic compounds in each part (60-93%). The total berry proanthocyanidin content was highest in Pinot Meunier (11 g kg(-1)) and lowest in Chardonnay (5 g kg(-1)), but Pinot Meunier pulp contained lower amounts of proanthocyanidins and phenolic acids (210 and 127 mg kg(-1) berry, respectively) than that of the other two varieties. The berry anthocyanin content was equivalent in both Pinot Noir and Pinot Meunier (632 and 602 mg kg(-1), respectively).

  16. Membrane Assisted Simultaneous Extraction and Derivatization with Triphenylphosphine of Elemental Sulfur in Arabian Crude Samples by Gas Chromatography/Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ibrahim Al-Zahrani

    2015-01-01

    Full Text Available Determination of trace level elemental sulfur from crude oil samples is a tedious task. Recently, several gas chromatographic methods were reported in which selective triphenylphosphine derivatization of sulfur was used to form triphenylphosphine sulfide. Direct quantitation of elemental sulfur from crude oil requires an efficient sample preparation method. This paper describes how simultaneous extraction derivatization of elemental sulfur was performed for the first time using porous hollow fiber membrane. A thick (0.25 um pore size; 1550 μm wall thickness; and 5500 μm inner diameter hollow fiber membrane filled with triphenylphosphine (dissolved N-methylpyrrolidone is used as a solvent bar. The solvent bar is tumbled freely in the crude oil sample; the elemental sulfur was extracted and derivatized. Finally, the derivatized sulfur was analyzed by gas chromatography/mass spectrometry. Various experimental conditions of solvent bar microextraction (SBME were optimized to achieve higher extraction. The linear range was established between 1 and 50 μg/mL, while a squared regression coefficient was found to be 0.9959 μg/mL. Relative standard deviation (RSD was below 10%. Relative recoveries were calculated for SBME in crude oil samples and were in the range between 98.2% and 101.2%.

  17. A Rapid and Optimized LC-MS/MS Method for the Simultaneous Extraction and Determination of Sofosbuvir and Ledipasvir in Human Plasma.

    Science.gov (United States)

    Elkady, Ehab F; Aboelwafa, Ahmed A

    2016-09-01

    A new validated bioanalytical method based on LC tandem MS has been developed for the simultaneous extraction and determination of sofosbuvir and ledipasvir in human plasma using antiviral daclatasvir as an internal standard (IS). Liquid-liquid extraction of samples was used for the purification and preconcentration of the analytes from a human plasma matrix. Good and consistent recoveries were obtained, with average extraction recoveries of 91.61 and 88.93% for sofosbuvir and ledipasvir, respectively. The chromatographic separation of the three analytes was achieved within only 2.8 min by an isocratic mobile phase consisting of 10 mM ammonium acetate, which was then adjusted to pH 4.0 by acetic acid-acetonitrile-0.1% methanolic formic acid (12 + 25 + 63, v/v/v) flowing through a C18 Zorbax eclipse plus column (5 μm, 100 × 4.6 mm; Agilent). Multiple reaction monitoring transitions were measured in positive ion mode for sofosbuvir, ledipasvir, and daclatasvir (IS). A detailed validation of the method was performed and the standard curves were found to be linear in the range of 0.5 to 2500 and 5 to 2100 ng/mL for sofosbuvir and ledipasvir, respectively, applying weighted (1/X(2)) linear regression. The developed method was applied to the analysis of the two drugs after a single oral administration of Harvoni 400/90 mg film-coated tablets containing 400 mg sofosbuvir and 90 mg ledipasvir to four healthy volunteers.

  18. Simultaneous quantification of sulforaphene and sulforaphane by reverse phase HPLC and their content in Raphanus sativus L. var. caudatus Alef extracts.

    Science.gov (United States)

    Sangthong, Sarita; Weerapreeyakul, Natthida

    2016-06-15

    A simple, rapid and precise HPLC assay was developed for the well-known anti-cancer isothiocyanates-sulforaphene (SE) and sulforaphane (SF). The analytical system comprised RP-C18 column with isocratic 5% THF-95% water. High resolution was obtained (and eluted) of two distinct HPLC peaks of similar structures SE and SF analytes (at 23.01±0.02 and 25.65±0.03 min, respectively). The respective LOD vs. LOQ for SE and SF was 0.34 and 0.36 μg/ml vs. 1.02 and 1.08 μg/ml. This assay had the best linearity and accuracy. The recoveries were in the range of 96.83-101.17%. SF and SE were quantified in the pod of Raphanus sativus L. var. caudatus Alef extracts (2253.05±246.18 and 111.94±16.49 μg/g in the crude extract, respectively), while only SE was detected in the stem (1105.14±243.10 μg/g crude extract), as SF was lower than the detection limit. The validated method thus minimized and expedited simultaneous SE and SF analysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Simultaneous Determination of Crypto-Chlorogenic Acid, Isoquercetin, and Astragalin Contents in Moringa oleifera Leaf Extracts by TLC-Densitometric Method

    Directory of Open Access Journals (Sweden)

    Boonyadist Vongsak

    2013-01-01

    Full Text Available Moringa oleifera Lamarck (Moringaceae is used as a multipurpose medicinal plant for the treatment of various diseases. Isoquercetin, astragalin, and crypto-chlorogenic acid have been previously found to be major active components in the leaves of this plant. In this study, a thin-layer-chromatography (TLC-densitometric method was developed and validated for simultaneous quantification of these major components in the 70% ethanolic extracts of M. oleifera leaves collected from 12 locations. The average amounts of crypto-chlorogenic acid, isoquercetin, and astragalin were found to be 0.0473, 0.0427, and 0.0534% dry weight, respectively. The method was validated for linearity, precision, accuracy, limit of detection, limit of quantitation, and robustness. The linearity was obtained in the range of 100–500 ng/spot with a correlation coefficient (r over 0.9961. Intraday and interday precisions demonstrated relative standard deviations of less than 5%. The accuracy of the method was confirmed by determining the recovery. The average recoveries of each component from the extracts were in the range of 98.28 to 99.65%. Additionally, the leaves from Chiang Mai province contained the highest amounts of all active components. The proposed TLC-densitometric method was simple, accurate, precise, and cost-effective for routine quality controlling of M. oleifera leaf extracts.

  20. Simultaneous accelerated solvent extraction and hydrolysis of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid glucuronide in meconium samples for gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Mantovani, Cinthia de Carvalho; Silva, Jefferson Pereira E; Forster, Guilherme; Almeida, Rafael Menck de; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

    2018-02-01

    Cannabis misuse during pregnancy is associated with severe impacts on the mother and baby health, such as newborn low birth weight, growth restriction, pre-term birth, neurobehavioral and developmental deficits. In most of the cases, drug abuse is omitted or denied by the mothers. Thus, toxicological analyzes using maternal-fetal matrices takes place as a suitable tool to assess drug use. Herein, meconium was the chosen matrix to evaluate cannabis exposure through identification and quantification of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic (THCCOOH). Accelerated solvent extraction (ASE) was applied for sample preparation technique to simultaneously extract and hydrolyze conjugated THCCOOH from meconium, followed by a solid-phase extraction (SPE) procedure. The method was developed and validated for gas chromatography-mass spectrometry (GC-MS), reaching hydrolysis efficiency of 98%. Limits of detection (LOD) and quantification (LOQ) were, respectively, 5 and 10 ng/g. The range of linearity was LOQ to 500 ng/g. Inter and intra-batch coefficients of variation were <8.4% for all concentration levels. Accuracy was in 101.7-108.9% range. Recovery was on average 60.3%. Carryover effect was not observed. The procedure was applied in six meconium samples from babies whose mothers were drug users and showed satisfactory performance to confirm fetal cannabis exposure. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Simultaneous Determination of Tetracyclines Residues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method.

    Science.gov (United States)

    Mesgari Abbasi, Mehran; Babaei, Hossein; Ansarin, Masoud; Nourdadgar, Ashraf-O-Sadat; Nemati, Mahboob

    2011-01-01

    Tetracyclines (TCs) are widely used in animal husbandry and their residues in milk may resultin harmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs) residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC) method using Fluorescence detector. The mean of total TCs residues in all samples (114 samples) was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and 24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g). This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  2. Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

    Directory of Open Access Journals (Sweden)

    Mehra Mesgari Abbasi

    2011-06-01

    Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  3. Polymer microneedles for transdermal drug delivery.

    Science.gov (United States)

    Lee, Jeong Woo; Han, Mee-Ree; Park, Jung-Hwan

    2012-11-20

    A microneedle system has been developed to deliver chemical and biological agents through the stratum corneum, which is the main barrier to drug delivery. Recently, microneedles have been fabricated from various kinds of polymers, including biocompatible polymer, biodegradable polymer, and water-soluble polymer. Polymer microneedles offer the benefits of ease of fabrication, cost-effectiveness, and mass production, as well as controlled drug release using the water solubility and degradation properties of polymer. In this review, the key features of polymer microneedles are discussed, including fabrication, materials, mechanical properties, drug delivery properties, and applications. Polymer microneedles provide a promising method for transdermal drug delivery by utilizing various physical and chemical properties of polymer.

  4. Enhanced transdermal delivery of ketobemidone with prodrugs

    DEFF Research Database (Denmark)

    Hansen, L.B.; Fullerton, A.; Christrup, Lona Louring

    1992-01-01

    ability to permeate the skin from either polar or apolar vehicles the ester prodrugs very readily penetrated through the skin from solutions in isopropyl myristate and, in particular, from ethanol and ethanol-water solutions. Thus, steady-state fluxes in the range of 40-140 μg ketobemidone base/cm per h...... the feasibility of achieving transdermal delivery of ketobemidone based on the ready enzymatic conversion and the favourable skin penetration properties of the ester prodrugs which in turn are attributed to their high solubilities in both polar and apolar solvents....... were observed for the ketobemidone esters from 20% w/v solutions in ethanol and ethanol-water (3:1 and 1:1 v/v) vehicles. The esters were rapidly hydrolyzed to the parent drug in the presence of skin enzymes and only from ketobemidone was detected in the receptor phase. The study demonstrates...

  5. Microneedle Coating Techniques for Transdermal Drug Delivery

    Directory of Open Access Journals (Sweden)

    Rita Haj-Ahmad

    2015-11-01

    Full Text Available Drug administration via the transdermal route is an evolving field that provides an alternative to oral and parenteral routes of therapy. Several microneedle (MN based approaches have been developed. Among these, coated MNs (typically where drug is deposited on MN tips are a minimally invasive method to deliver drugs and vaccines through the skin. In this review, we describe several processes to coat MNs. These include dip coating, gas jet drying, spray coating, electrohydrodynamic atomisation (EHDA based processes and piezoelectric inkjet printing. Examples of process mechanisms, conditions and tested formulations are provided. As these processes are independent techniques, modifications to facilitate MN coatings are elucidated. In summary, the outcomes and potential value for each technique provides opportunities to overcome formulation or dosage form limitations. While there are significant developments in solid degradable MNs, coated MNs (through the various techniques described have potential to be utilized in personalized drug delivery via controlled deposition onto MN templates.

  6. Transdermal fluid loss in severely burned patients

    Directory of Open Access Journals (Sweden)

    Lange, Thomas

    2010-01-01

    Full Text Available Introduction: The skin protects against fluid and electrolyte loss. Burn injury does affect skin integrity and protection against fluid loss is lost. Thus, a systemic dehydration can be provoked by underestimation of fluid loss through burn wounds. Purpose: We wanted to quantify transdermal fluid loss in burn wounds. Method: Retrospective study. 40 patients admitted to a specialized burn unit were analyzed and separated in two groups without (Group A or with (Group B hypernatremia. Means of daily infusion-diuresis-ratio (IDR and the relationship to totally burned surface area (TBSA were analyzed. Results: In Group A 25 patients with a mean age of 47±18 years, a mean TBSA of 23±11%, and a mean abbreviated burned severity index (ABSI score of 6.9±2.1 were summarized. In Group B 15 patients with a mean age of 47±22 years, a mean TBSA of 30±13%, and a mean ABSI score of 8.1±1.7 were included. Statistical analysis of the period from day 3 to day 6 showed a significant higher daily IDR-amount in Group A (Group A vs. Group B: 786±1029 ml vs. –181±1021 ml; p<0.001 and for daily IDR-TBSA-ratio (Group A vs. Group B: 40±41 ml/% vs. –4±36 ml/%; p<0.001. Conclusions: There is a systemic relevant transdermal fluid loss in burn wounds after severe burn injury. Serum sodium concentration can be used to calculate need of fluid resuscitation for fluid maintenance. There is a need of an established fluid removal strategy to avoid water and electrolyte imbalances.

  7. Testosterone ethosomes for enhanced transdermal delivery.

    Science.gov (United States)

    Ainbinder, Denize; Touitou, Elka

    2005-01-01

    Physiological decrease in testosterone levels in men with age causes various changes with clinical significance. Recent testosterone replacement therapy is based mainly on transdermal nonpatch delivery systems. These products have the drawback of application on extremely large areas to achieve required hormone blood levels. The objective of the present study was to design and test a testosterone nonpatch formulation using ethosomes for enhanced transdermal absorption. The ethosomal formulation was characterized by transmission electron microscopy and dynamic light scattering for structure and size distribution and by ultracentrifugation for entrapment capacity. To evaluate the feasibility of this delivery system to enhance testosterone permeation through the skin, first the systemic absorption in rats was compared with a currently used gel (AndroGel). Further, theoretical estimation of testosterone blood concentration following ethosomal application in men was made. For this purpose, in vitro permeation experiments through human skin were performed to establish testosterone skin permeation values. In the design of these experiments, testosterone solubility in various solutions was measured and the effect of the receiver medium on the skin barrier function was assessed by confocal laser scanning microscopy. Theoretical estimation shows that testosterone human plasma concentration value in the upper part of the physiological range could be achieved by application of the ethosomal formulation on an area of 40 cm(2). This area is about 10 times smaller than required with current nonpatch formulations. Our work shows that the ethosomal formulation could enhance testosterone systemic absorption and also be used for designing new products that could solve the weaknesses of the current testosterone replacement therapies.

  8. Rapidly separating microneedles for transdermal drug delivery.

    Science.gov (United States)

    Zhu, Dan Dan; Wang, Qi Lei; Liu, Xu Bo; Guo, Xin Dong

    2016-09-01

    The applications of polymer microneedles (MNs) into human skin emerged as an alternative of the conventional hypodermic needles. However, dissolving MNs require many minutes to be dissolved in the skin and typically have difficulty being fully inserted into the skin, which may lead to the low drug delivery efficiency. To address these issues, we introduce rapidly separating MNs that can rapidly deliver drugs into the skin in a minimally invasive way. For the rapidly separating MNs, drug loaded dissolving MNs are mounted on the top of solid MNs, which are made of biodegradable polylactic acid which eliminate the biohazardous waste. These MNs have sufficient mechanical strength to be inserted into the skin with the drug loaded tips fully embedded for subsequent dissolution. Compared with the traditional MNs, rapidly separating MNs achieve over 90% of drug delivery efficiency in 30s while the traditional MNs needs 2min to achieve the same efficiency. With the in vivo test in mice, the micro-holes caused by rapidly separating MNs can heal in 1h, indicating that the rapidly separating MNs are safe for future applications. These results indicate that the design of rapidly separating dissolvable MNs can offer a quick, high efficient, convenient, safe and potentially self-administered method of drug delivery. Polymer microneedles offer an attractive, painless and minimally invasive approach for transdermal drug delivery. However, dissolving microneedles require many minutes to be dissolved in the skin and typically have difficulty being fully inserted into the skin due to the skin deformation, which may lead to the low drug delivery efficiency. In this work we proposed rapidly separating microneedles which can deliver over 90% of drug into the skin in 30s. The in vitro and in vivo results indicate that the new design of these microneedles can offer a quick, high efficient, convenient and safe method for transdermal drug delivery. Copyright © 2016 Acta Materialia Inc

  9. Preparation of a novel sorptive stir bar based on vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma.

    Science.gov (United States)

    Torabizadeh, Mahsa; Talebpour, Zahra; Adib, Nuoshin; Aboul-Enein, Hassan Y

    2016-04-01

    A new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The polymerization step was performed using different contents of monomer, cross-linker and porogenic solvent, and the best formulation was selected. The quality of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate stir bars was satisfactory, demonstrating good repeatability within batch (relative standard deviation diazepam and nordazepam in human plasma samples. To optimize the extraction step, a three-level, four-factor, three-block Box-Behnken design was applied. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for diazepam (36-1200 ng/mL) and nordazepam (25-1200 ng/mL), with correlation coefficients of 0.9986 and 0.9968 and detection limits of 12 and 10 ng/mL, respectively. The intra- and interday recovery ranged from 93 to 106%, and the relative standard deviations were less than 6%. Finally, the proposed method was successfully applied to the analysis of diazepam and nordazepam at their therapeutic levels in human plasma. The novelty of this study is the improved polarity of the stir bar coating and its application for the simultaneous extraction of diazepam and its active metabolite, nordazepam in human plasma sample. The method was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of diazepam and nordazepam in biological fluids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. A COMPREHENSIVE REVIEW ON MICRONEEDLES - AN ARCHETYPE SWING IN TRANSDERMAL DRUG DELIVERY

    OpenAIRE

    G. Ravi*, N. Vishal Gupta, M. P. Gowrav

    2017-01-01

    Transdermal drug delivery is the non-invasive delivery of medications through the skin surface into the systemic circulation. The advantage of transdermal drug delivery system is that it is painless technique of administration of drugs. The advantage of transdermal drug delivery system is that it is painless technique of administration of drugs. Transdermal drug delivery system can improve the therapeutic efficacy and safety of the drugs because drug delivered through the skin at a predetermi...

  11. Determination of tin, vanadium, iron, and molybdenum in various matrices by atomic absorption spectrometry using a simultaneous liquid-liquid extraction procedure.

    Science.gov (United States)

    Sánchez-Viñas, M; Bagur, G M; Gázquez, D; Camino, M; Romero, R

    1999-01-01

    An atomic-absorption spectrometric method is described for the determination of tin, vanadium, iron, and molybdenum in two certified reference materials, food samples, and petroleum crude. After treatment with acids, these elements are separated from matrix elements by simultaneous solvent extraction of 5,5'-methylenedisalicylohydroxamic acid complexes from HCl/NaClO4 solution into an isobutyl methyl ketone/tributyl phosphate solution. The detection limits range from 0.018 to 0.19 microg/mL (n = 3), and the relative standard deviations do not exceed 2.0% at levels of 0.5, 0.6, 2.0, and 7.0 microg/mL of Fe, Mo, V, and Sn, respectively. The method is selective and suffers only from interference by Zr(IV), Ti(IV), Th(IV), W(VI), PO4(3-), and F-.

  12. Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2010-01-01

    procedures were investigated and compared for the adjustment of oxidation states of plutonium and neptunium to Pu(IV) and Np(IV), respectively. A two-step protocol using sulfite and concentrated nitric acid as redox reagents was proven to be the most effective method. The analytical results for both...... plutonium and neptunium in three reference materials were in agreement with the recommended or literature values at the 0.05 significance level. The developed method is suitable for the analysis of up to 10 g of soil and 20 g of seaweed samples. The extraction chromatographic separation within the SI system...... for a single sample takes less than 1.5 h. As compared to batchwise procedures, the developed method significantly improves the analysis efficiency, reduces the labor intensity and expedites the simultaneous determination of plutonium and neptunium as demanded in emergency actions....

  13. A solid phase extraction procedure for the simultaneous determination of total inorganic arsenic and trace metals in seawater: Sample preparation for total-reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Staniszewski, B. [Department of Analytical Chemistry, Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan (Poland)], E-mail: bstanisz@amu.edu.pl; Freimann, P. [Bundesamt fuer Seeschifffahrt und Hydrographie, Wuestland 2, 22589 Hamburg (Germany)], E-mail: peter.freimann@bsh.de

    2008-11-15

    In this paper we present a procedure allowing total-reflection X-ray fluorescence spectrometry (TXRF) determinations of arsenic in water samples, especially in seawater samples. The procedure consists of an arsenate reduction step (performed by using a L-cysteine solution) followed by a complexation of As{sup +3} with sodium dibenzyldithiocarbamate and solid phase extraction. The new procedure is a modification of a method developed by Prange and allows a simultaneous determination of As together with V, Fe, Ni, Cu, Zn, Pb, and U in seawater by TXRF. The procedure was tested using the Certified Reference Material CASS-4 and was later applied to regular seawater samples collected from the North Sea. The detection limit for arsenic is 10 ng L{sup -1}.

  14. A solid phase extraction procedure for the simultaneous determination of total inorganic arsenic and trace metals in seawater: Sample preparation for total-reflection X-ray fluorescence

    Science.gov (United States)

    Staniszewski, B.; Freimann, P.

    2008-11-01

    In this paper we present a procedure allowing total-reflection X-ray fluorescence spectrometry (TXRF) determinations of arsenic in water samples, especially in seawater samples. The procedure consists of an arsenate reduction step (performed by using a L-cysteine solution) followed by a complexation of As +3 with sodium dibenzyldithiocarbamate and solid phase extraction. The new procedure is a modification of a method developed by Prange and allows a simultaneous determination of As together with V, Fe, Ni, Cu, Zn, Pb, and U in seawater by TXRF. The procedure was tested using the Certified Reference Material CASS-4 and was later applied to regular seawater samples collected from the North Sea. The detection limit for arsenic is 10 ng L - 1 .

  15. Simultaneous determination of antimony and boron in beverage and dairy products by flame atomic absorption spectrometry after separation and pre-concentration by cloud-point extraction.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2016-01-01

    A new cloud-point extraction (CPE) method was developed for the pre-concentration and simultaneous determination of Sb(III) and B(III) by flame atomic absorption spectrometry (FAAS). The method was based on complexation of Sb(III) and B(III) with azomethine-H in the presence of cetylpyridinium chloride (CPC) as a signal-enhancing agent, and then extraction into the micellar phase of Triton X-114. Under optimised conditions, linear calibration was obtained for Sb(III) and B(III) in the concentration ranges of 0.5-180 and 2.5-600 μg l(-1) with LODs of 0.15 and 0.75 μg l(-1), respectively. Relative standard deviations (RSDs) (25 and 100 μg l(-1) of Sb(III) and B(III), n = 6) were in a range of 2.1-3.8% and 1.9-2.3%, respectively. Recoveries of spiked samples of Sb(III) and B(III) were in the range of 98-103% and 99-102%, respectively. Measured values for Sb and B in three standard reference materials were within the 95% confidence limit of the certified values. Also, the method was used for the speciation of inorganic antimony. Sb(III), Sb(V) and total Sb were measured in the presence of excess boron before and after pre-reduction with an acidic mixture of KI-ascorbic acid. The method was successfully applied to the simultaneous determination of total Sb and B in selected beverage and dairy products.

  16. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  17. A rapid and sensitive method for the simultaneous analysis of aliphatic and polar molecules containing free carboxyl groups in plant extracts by LC-MS/MS

    Directory of Open Access Journals (Sweden)

    Bonaventure Gustavo

    2009-11-01

    Full Text Available Abstract Background Aliphatic molecules containing free carboxyl groups are important intermediates in many metabolic and signalling reactions, however, they accumulate to low levels in tissues and are not efficiently ionized by electrospray ionization (ESI compared to more polar substances. Quantification of aliphatic molecules becomes therefore difficult when small amounts of tissue are available for analysis. Traditional methods for analysis of these molecules require purification or enrichment steps, which are onerous when multiple samples need to be analyzed. In contrast to aliphatic molecules, more polar substances containing free carboxyl groups such as some phytohormones are efficiently ionized by ESI and suitable for analysis by LC-MS/MS. Thus, the development of a method with which aliphatic and polar molecules -which their unmodified forms differ dramatically in their efficiencies of ionization by ESI- can be simultaneously detected with similar sensitivities would substantially simplify the analysis of complex biological matrices. Results A simple, rapid, specific and sensitive method for the simultaneous detection and quantification of free aliphatic molecules (e.g., free fatty acids (FFA and small polar molecules (e.g., jasmonic acid (JA, salicylic acid (SA containing free carboxyl groups by direct derivatization of leaf extracts with Picolinyl reagent followed by LC-MS/MS analysis is presented. The presence of the N atom in the esterified pyridine moiety allowed the efficient ionization of 25 compounds tested irrespective of their chemical structure. The method was validated by comparing the results obtained after analysis of Nicotiana attenuata leaf material with previously described analytical methods. Conclusion The method presented was used to detect 16 compounds in leaf extracts of N. attenuata plants. Importantly, the method can be adapted based on the specific analytes of interest with the only consideration that the

  18. A rapid and sensitive method for the simultaneous analysis of aliphatic and polar molecules containing free carboxyl groups in plant extracts by LC-MS/MS.

    Science.gov (United States)

    Kallenbach, Mario; Baldwin, Ian T; Bonaventure, Gustavo

    2009-11-25

    Aliphatic molecules containing free carboxyl groups are important intermediates in many metabolic and signalling reactions, however, they accumulate to low levels in tissues and are not efficiently ionized by electrospray ionization (ESI) compared to more polar substances. Quantification of aliphatic molecules becomes therefore difficult when small amounts of tissue are available for analysis. Traditional methods for analysis of these molecules require purification or enrichment steps, which are onerous when multiple samples need to be analyzed. In contrast to aliphatic molecules, more polar substances containing free carboxyl groups such as some phytohormones are efficiently ionized by ESI and suitable for analysis by LC-MS/MS. Thus, the development of a method with which aliphatic and polar molecules -which their unmodified forms differ dramatically in their efficiencies of ionization by ESI- can be simultaneously detected with similar sensitivities would substantially simplify the analysis of complex biological matrices. A simple, rapid, specific and sensitive method for the simultaneous detection and quantification of free aliphatic molecules (e.g., free fatty acids (FFA)) and small polar molecules (e.g., jasmonic acid (JA), salicylic acid (SA)) containing free carboxyl groups by direct derivatization of leaf extracts with Picolinyl reagent followed by LC-MS/MS analysis is presented. The presence of the N atom in the esterified pyridine moiety allowed the efficient ionization of 25 compounds tested irrespective of their chemical structure. The method was validated by comparing the results obtained after analysis of Nicotiana attenuata leaf material with previously described analytical methods. The method presented was used to detect 16 compounds in leaf extracts of N. attenuata plants. Importantly, the method can be adapted based on the specific analytes of interest with the only consideration that the molecules must contain at least one free carboxyl group.

  19. A novel molecularly imprinted polymer for simultaneous extraction and determination of sudan dyes by on-line solid phase extraction and high performance liquid chromatography.

    Science.gov (United States)

    Zhao, Chuande; Zhao, Ting; Liu, Xiaoyan; Zhang, Haixia

    2010-11-05

    A novel molecularly imprinted polymer was synthesized with attapulgite employed as matrix, which is simple and time-saving. In this method, sudan I was chosen as template molecule, 2-vinylpyridine as functional monomer and ethylene glycol dimethacrylate as cross-linking agent, respectively. The imprinted polymer was characterized by the infrared spectroscopy and transmission electron microscopy. Then the selectivity experiments were performed on sudan dyes and the recognition coefficients for sudan I, sudan II, sudan III and sudan IV were 2.9, 1.9, 1.9 and 2.3, respectively. As the packing material of solid-phase extraction, the imprinted polymer has been applied to on-line concentration of the four sudan dyes in samples from Yellow River water, tomato sauce and sausage. The corresponding analytical methods to determine these sudan dyes have been developed. The limits of detection for these sudan dyes were in the range of 0.01-0.05 ng mL(-1) for Yellow River water, 1.0-3.0 ng g(-1) for tomato sauce and 0.8-3.0 ng g(-1) for sausage. Crown Copyright © 2010. Published by Elsevier B.V. All rights reserved.

  20. On-line solid phase extraction CZE for the simultaneous determination of lanthanum and gadolinium at picogram per liter levels.

    Science.gov (United States)

    Vizioli, Nora; Gil, Raúl; Martínez, Luis Dante; Silva, María Fernanda

    2009-08-01

    A non-specific on-line method is presented for the extraction and preconcentration of two rare earth elements using a microcartridge containing C(18)-derivatized silica particles prior to their analysis by CZE. The microcartridge, named analyte concentrator, was coupled on-line to the inlet of the separation capillary (fused-silica (FS) capillary, 75 microm id x12 cm from the inlet to the microcartidge and 37 cm from the microcartridge to the detector). The reversed-phase sorbent quantitatively retained gadolinium (Gd) and lanthanum (La) as 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complexes in the presence of non-ionic micelles of polyethylene glycol tert-octylphenyl ether, enabling sample clean-up and concentration enhancement with minimum sample handling. The rare earth elements chelates were released from the sorbent with methanol and then analyzed by CZE with diode array detection. A background electrolyte of 20 mM sodium tetraborate containing 8% ACN, pH 9.0, was found to be optimal for the separation of metal chelates. The concentration limits of detection were lowered to picogram per liter levels (20 pg/L for La and 80 pg/L for Gd). A 1000-fold improvement in concentration sensitivity for La- and Gd-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complexes with respect to CZE without preconcentration was reached.

  1. A universal route for the simultaneous extraction and functionalization of cellulose nanocrystals from industrial and agricultural celluloses

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Guo-Yin; Yu, Hou-Yong, E-mail: phdyu@zstu.edu.cn; Zhang, Cai-Hong [Zhejiang Sci-Tech University, The Key Laboratory of Advanced Textile Materials and Manufacturing Technology of Ministry of Education, College of Materials and Textiles (China); Zhou, Ying; Yao, Ju-Ming, E-mail: yaoj@zstu.edu.cn [Zhejiang Sci-Tech University, National Engineering Lab for Textile Fiber Materials & Processing Technology (China)

    2016-02-15

    A simple route was designed to extract the cellulose nanocrystals (CNCs) with formate groups from industrial and agricultural celluloses like microcrystalline cellulose (MCC), viscose fiber, ginger fiber, and bamboo fiber. The effect of reaction time on the microstructure and properties of the CNCs was investigated in detail, while microstructure and properties of different CNCs were compared. The rod-like CNCs (MCC) with hundreds of nanometers in length and about 10 nm in width, nanofibrillated CNCs (ginger fiber bamboo fiber) with average width of 30 nm and the length of 1 μm, and spherical CNCs (viscose fiber) with the width of 56 nm were obtained by one-step HCOOH/HCl hydrolysis. The CNCs with improved thermal stability showed the maximum degradation temperature (T{sub max}) of 368.9–388.2 °C due to the introduction of formate groups (reducibility) and the increased crystallinity. Such CNCs may be used as an effective template for the synthesis of nanohybrids or reinforcing material for high-performance nanocomposites.

  2. A Preliminary Study of a Transdermal Radiofrequency Device for Body Slimming.

    Science.gov (United States)

    Key, Douglas J

    2015-11-01

    The use and potential of radiofrequency energy for tissue contracture and body contouring has been established in the literature. Maximum reduction of laxity can be achieved by simultaneously tightening surface tissue and reducing unwanted fat below by the transdermal application of heat to reach and maintain tissue temperature targets within a well-defined range, inducing collagen remodeling in skin as well as apoptosis of fat cells and creating an overall slimming effect. A novel device utilizes transcutaneous monopolar RF for body slimming in this manner, employing a thermistor feedback control mechanism to safely manage energy delivery and tissue temperature. Subjects (n=14) presenting with abdominal laxity were treated up to four times using the transcutaneous monopolar RF device at one or two zones in the abdominal region (at operator's discretion). Non-expert blinded graders rated correction on an arbitrary scale (0=no laxity, 4=maximum laxity) after choosing the order of the before-and-after photo sets. A patient satisfaction survey was also administered. The two graders correctly ordered 10 of 14 photo sets in agreement. Average rated improvement was 0.75 and 0.80 for graders 1 and 2, respectively. Patient survey results revealed average perceived tightening of 2.14 points on a 0 to 4 scale (0=lowest tightening result, 4=highest tightening), and 8 of 14 subjects would recommend treatment to others. Transdermal monopolar RF is a safe and effective modality for non-invasive body slimming.

  3. [Simultaneous determination of 23 ester compounds in cigarette water-borne adhesives by liquid-liquid extraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Gong, Shuguo; Kong, Bo; Tuo, Suxing; Dai, Yunhui; Wu, Mingjian; Tan, Liquan; Liu, Wei

    2013-10-01

    A method of gas chromatography-mass spectrometry (GC-MS) with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds including acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 microm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column (60 m x 0.25 mm x 0.25 microm), and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4-50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8%-109.1%, and the relative standard deviations (RSDs, n = 5) were less than 4%. The limits of detection (LODs) and limits of quantification (LOQs were in the ranges of 0.02-0.76 mg/kg and 0.04-2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.

  4. Dual cloud point extraction coupled with hydrodynamic-electrokinetic two-step injection followed by micellar electrokinetic chromatography for simultaneous determination of trace phenolic estrogens in water samples.

    Science.gov (United States)

    Wen, Yingying; Li, Jinhua; Liu, Junshen; Lu, Wenhui; Ma, Jiping; Chen, Lingxin

    2013-07-01

    A dual cloud point extraction (dCPE) off-line enrichment procedure coupled with a hydrodynamic-electrokinetic two-step injection online enrichment technique was successfully developed for simultaneous preconcentration of trace phenolic estrogens (hexestrol, dienestrol, and diethylstilbestrol) in water samples followed by micellar electrokinetic chromatography (MEKC) analysis. Several parameters affecting the extraction and online injection conditions were optimized. Under optimal dCPE-two-step injection-MEKC conditions, detection limits of 7.9-8.9 ng/mL and good linearity in the range from 0.05 to 5 μg/mL with correlation coefficients R(2) ≥ 0.9990 were achieved. Satisfactory recoveries ranging from 83 to 108% were obtained with lake and tap water spiked at 0.1 and 0.5 μg/mL, respectively, with relative standard deviations (n = 6) of 1.3-3.1%. This method was demonstrated to be convenient, rapid, cost-effective, and environmentally benign, and could be used as an alternative to existing methods for analyzing trace residues of phenolic estrogens in water samples.

  5. Simultaneous determination of anthracyclines and taxanes in human serum using online sample extraction coupled to high performance liquid chromatography with UV detection.

    Science.gov (United States)

    Bermingham, Shane; O'Connor, Robert; Regan, Fiona; McMahon, Gillian P

    2010-06-01

    An online SPE-LC method that can determine both anthracyclines and taxanes simultaneously in human serum samples is reported. The entire method of extraction, separation and UV detection was achieved online by column switching between an SPE column (Biotrap 500 (20 x 4 mm)) and an analytical column (Zorbax XDB C18, 150 x 4.6 mm, 5 microm) with a 23 min total cycle time. The method is linear (r(2)>0.998) over the range of 0.5-25 microg/mL. The analytes of interest are retained on the SPE column with good recovery (84-117%), while proteins and other serum components elute to waste. This online clean-up is much faster (150 s) and less manual than traditional off-line extraction methods. Using 0.1 mL spiked serum samples, the LOQ was 0.5 microg/mL. Intra- and inter-day precision were acceptable (serum samples from patients undergoing chemotherapy with these agents.

  6. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    Science.gov (United States)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

  7. Simultaneous speciation of inorganic selenium and antimony in water samples by electrothermal vaporization inductively coupled plasma mass spectrometry following selective cloud point extraction.

    Science.gov (United States)

    Li, Yingjie; Hu, Bin; He, Man; Xiang, Guoqiang

    2008-02-01

    A new method was developed for the simultaneous speciation of inorganic selenium and antimony in water by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) following selective cloud point extraction (CPE). The method is based on the fact that Se(IV) and Sb(III) could form complexes with diethyldithiocarbamate (DDTC) at pH 6.00, and the complexes were quantitatively extracted into the non-ionic surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114), whereas the Se(VI) and Sb(V) remained as free species in aqueous solutions. Sb(III) and Se(IV) in concentrate were determined by ETV-ICP-MS after proper disposal. The total Se and total Sb were determined by the same protocol after Se(VI) and Sb(V) were reduced by l-cysteine, and Se(VI) and Sb(V) concentrations were obtained by respectively subtracting Se(IV) and Sb(III) from the total Se and the total Sb. Under the optimized conditions, the limits of detection (LODs) were 0.05 microg L(-1) for Se(IV) and 0.03 microg L(-1) for Sb(III), the relative standard deviations (RSDs) were 3.5% for Se(IV) and 4.2% for Sb(III) (C=1.00 microg L(-1), n=5). The proposed method was applied to the speciation of inorganic selenium and antimony in different water samples with satisfactory results.

  8. Simultaneous quantification of 25 active constituents in the total flavonoids extract from Herba Desmodii Styracifolii by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Guo, Panpan; Yan, Wenying; Han, Qingjie; Wang, Chunying; Zhang, Zijian

    2015-04-01

    A sensitive and selective high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry method has been developed and validated for the simultaneous determination of 25 active constituents, including 21 flavonoids and four phenolic acids in the total flavonoids extract from Herba Desmodii Styracifolii for the first time. Among the 25 compounds, seven compounds including caffeic acid, acacetin, genistein, genistin, diosmetin, diosmin and hesperidin were identified and quantified for the first time in Herba Desmodii Styracifolii. Chromatographic separation was accomplished on a ZORBAX SB-C18 (250 mm×4.6 mm, 5.0 μm) column using gradient elution of methanol and 0.1‰ acetic acid v/v at a flow rate of 1.0 mL/min. The identification and quantification of the analytes were achieved using negative electrospray ionization mass spectrometry in multiple-reaction monitoring mode. The method was fully validated in terms of limits of detection and quantification, linearity, precision and accuracy. The results indicated that the developed method is simple, rapid, specific and reliable. Furthermore, the developed method was successfully applied to quantify the 25 active components in six batches of total flavonoids extract from Herba Desmodii Styracifolii. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Simultaneous quantification of two steroidal glycosides after oral gavage of Marsdenia tenacissima extract in rats using a LC-MS/MS method.

    Science.gov (United States)

    Wang, Wei; Sun, Wei; Dong, Lei; Qu, Xiaotong; Shi, Jin; Li, Ke-Jun; Li, Bing; Ma, Da-Peng

    2015-04-01

    A specific, sensitive and accurate analytical LC-MS/MS assay was developed for the simultaneous determination of two steroidal glycosides, tenacissoside H and tenacissoside I, in rat plasma. An Agilent ZORBAX SB-C18 column was used with an isocratic mobile phase system composed of methanol-water-formic acid (70:30:0.1, v/v/v) at a flow rate of 0.3 mL/min. The analysis was performed on a positive ionization electrospray mass spectrometer via selected reaction monitoring mode scan. One-step protein precipitation with acetonitrile was chosen to extract the analytes from plasma. The lower limits of quantification were 0.9 ng/mL for tenacissoside H and tenacissoside I. The intra- and inter-day precisions were 2.03-11.56 and 3.76-11.62%, respectively, and the accuracies were <110.28% at all quality control levels. The validated method was applied to a pharmacokinetic study in rats after oral gavage of Marsdenia tenacissima extract. Copyright © 2014 John Wiley & Sons, Ltd.

  10. A novel high-throughput method for supported liquid extraction of retinol and alpha-tocopherol from human serum and simultaneous quantitation by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Hinchliffe, Edward; Rudge, James; Reed, Paul

    2016-07-01

    Measurement of vitamin A (retinol) and E (alpha-tocopherol) in UK clinical laboratories is currently performed exclusively by high-performance liquid chromatography with ultraviolet detection. We investigated whether retinol and alpha-tocopherol could be measured simultaneously by liquid chromatography tandem mass spectrometry. Serum samples (100 μL) were extracted using Isolute + Supported Liquid Extraction plates. Chromatography was performed on a Phenomenex Kinetex Biphenyl 2.6 μm, 50 × 2.1 mm column, and liquid chromatography tandem mass spectrometry on a Waters Acquity TQD. Injection-to-injection time was 4.3 min. The assay was validated according to published guidelines. Patient samples were used to compare liquid chromatography tandem mass spectrometry and high-performance liquid chromatography with ultraviolet detection methods. For retinol and alpha-tocopherol, respectively, the assay was linear up to 6.0 and 80.0 μmol/L, and lower limit of quantification was 0.07 and 0.26 μmol/L. Intra and interassay imprecision were within desirable analytical specifications. Analysis of quality control material aligned to NIST SRM 968e, and relative spiked recovery from human serum, both yielded results within 15% of target values. Method comparison with high-performance liquid chromatography with ultraviolet detection methodology demonstrated a negative bias for retinol and alpha-tocopherol by the liquid chromatography tandem mass spectrometry method. Analysis of United Kingdom National External Quality Assurance Scheme samples yielded mean bias from the target value of +3.0% for retinol and -11.2% for alpha-tocopherol. We have developed a novel, high-throughput method for extraction of retinol and alpha-tocopherol from human serum followed by simultaneous quantitation by liquid chromatography tandem mass spectrometry. The method offers a rapid, sensitive, specific and cost-effective alternative to high-performance liquid chromatography with

  11. Transdermal iontophoretic delivery of timolol maleate

    Directory of Open Access Journals (Sweden)

    Mayur Patni

    2012-12-01

    Full Text Available Transdermal iontophoresis would be a promising method for the systemic delivery of water soluble and ionic drugs of relatively high molecular size, including peptides. The objective of the present study was to investigate the effect of biological variable such as guinea pig and human cadaver skin and other variables like drug concentration, current density on the transdermal iontophoretic transport of timolol maleate. The permeation profile of drug using solution and gel formulation was studied and compared. For better bioavailability, better patient compliance, and enhanced delivery, an iontophoretic drug delivery system of a timolol maleate matrix gel was formulated using Carbopol 974P. The study was conducted using silver-silver chloride electrodes across the guinea pig and human cadaver skin. Viscosity measurements and flux calculations indicated the suitability of the Carbopol 974P gel for transdermal iontophoretic delivery of timolol maleate. Anodal iontophoresis with silver-silver chloride electrode significantly increased the timolol maleate skin permeation as compared with the passive permeation study. The amount of timolol maleate transported during iontophoresis was significantly different among the different skins. However, iontophoretic gel formulations provided required flux of drug through human cadaver skin.A iontoforese transdérmica seria um método promissor para a liberação sistêmica de fármacos solúveis em água e iônicos de relativamente elevado tamanho molecular, incluindo peptídeos. O objetivo do presente estudo foi investigar o efeito da variável biológica, tais como cobaia e pele de cadáver humano, e outras variáveis como concentração do fármaco, densidade de corrente sobre o transporte transdérmico iontoforético de maleato de timolol. Comparou-se o perfil de permeação do fármaco usando a formulação de solução e de gel. Para melhor biodisponibilidade, melhor adesão do paciente e libera

  12. Current advances in the fabrication of microneedles for transdermal delivery.

    Science.gov (United States)

    Indermun, Sunaina; Luttge, Regina; Choonara, Yahya E; Kumar, Pradeep; du Toit, Lisa C; Modi, Girish; Pillay, Viness

    2014-07-10

    The transdermal route is an excellent site for drug delivery due to the avoidance of gastric degradation and hepatic metabolism, in addition to easy accessibility. Although offering numerous attractive advantages, many available transdermal systems are not able to deliver drugs and other compounds as desired. The use of hypodermic needles, associated with phobia, pain and accidental needle-sticks has been used to overcome the delivery limitation of macromolecular compounds. The means to overcome the disadvantages of hypodermic needles has led to the development of microneedles for transdermal delivery. However, since the initial stages of microneedle fabrication, recent research has been conducted integrating various fabrication techniques for generating sophisticated microneedle devices for transdermal delivery including progress on their commercialization. A concerted effort has been made within this review to highlight the current advances of microneedles, and to provide an update of pharmaceutical research in the field of microneedle-assisted transdermal drug delivery systems. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Synthesis and transdermal properties of acetylsalicylic acid and selected esters.

    Science.gov (United States)

    Gerber, Minja; Breytenbach, Jaco C; Hadgraft, Jonathan; du Plessis, Jeanetta

    2006-03-09

    The primary aim of this study was to determine the transdermal penetration of acetylsalicylic acid and some of its derivatives, to establish a correlation, if any, with selected physicochemical properties and to determine if transdermal application of acetylsalicylic acid and its derivatives will give therapeutic drug concentrations with respect to transdermal flux. Ten derivatives of acetylsalicylic acid were prepared by esterification of acetylsalicyloyl chloride with ten different alcohols. The experimental aqueous solubility, logD and transdermal flux values were determined for acetylsalicylic acid and its derivatives at pH 4.5. In vitro penetration was measured through excised female human abdominal skin in diffusion cells. The experimental aqueous solubility of acetylsalicylic acid (6.56 mg/ml) was higher than that of the synthesised acetylsalicylate derivatives (ranging from 1.76 x 10(-3) to 3.32 mg/ml), and the logD of acetylsalicylic acid (-0.85) was lower than that of its derivatives (ranging from -0.25 to 1.95). There was thus an inverse correlation between the aqueous solubility data and the logD values. The experimental transdermal flux of acetylsalicylic acid (263.83 nmol/cm(2)h) was much higher than that of its derivatives (ranging from 0.12 to 136.02 nmol/cm(2)h).

  14. A new tunable dispersive liquid-liquid micro extraction method developed for the simultaneous preconcentration of lead and cadmium from lakes water: a multivariate study

    Science.gov (United States)

    Bilal, Muhammad; Kazi, Tasneem Gul; Afridi, Hassan Imran; Ali, Jamshed; Baig, Jameel Ahmed; Arain, Mohammad Balal; Khan, Mustafa

    2017-08-01

    A green tunable dispersive liquid-liquid micro extraction (TDLLME) technique was established for the simultaneous enrichment of lead (Pb) and cadmium (Cd) from different lakes water before analysis by flame atomic absorption spectrometry (FAAS). A solvent known as tunable polarity solvent (TPS), mixture of 1,8-diazabicyclo-[5.4.0]-undec-7-ene (DBU) and 1-decanol, has been employed as extractant in aqueous medium. In first step this mixture can be made polar by slowly bubbling the antisolvent trigger (CO2) through the solution, which makes a monophasic solution. During this step hydrophobic complexes of the metals with 8-hydroxy quinoline (8-HQ) were extracted by TPS. Then the mixture was switched back to hydrophobic one by heating and/or bubbling nitrogen, turning the mixture into two phases again. In second phase the metals were leached out from the complexes entrapped in TPS, by treating with a solution of nitric acid and exposing the mixture to CO2, which switched the mixture into single phase. Then N2 purging and/or heating again turned the mixture into two phases. The acidic aqueous phase containing the metals was introduced to FAAS for analysis, whereas TPS was recycled for next experiment. Different parameters, affecting the efficiency the technique, were optimized by multivariate approach. The method was applied to certified reference material of water and to a real sample spiked with standards of known concentration, to confirm its validity and accuracy. LOD obtained for Pb and Cd were 0.560 and 0.056 μg L- 1 respectively. The developed method was applied successfully to the real water samples of two lakes of Sindh, Pakistan.

  15. Simultaneous Determination of 11 Aminoglycoside Residues in Honey, Milk, and Pork by Liquid Chromatography with Tandem Mass Spectrometry and Molecularly Imprinted Polymer Solid Phase Extraction.

    Science.gov (United States)

    Yang, Bixia; Wang, Lian; Luo, Chunying; Wang, Xixi; Sun, Chengjun

    2017-08-08

    An analytical method was developed for the simultaneous determination of 11 aminoglycoside (AG) antibiotics, including amikacin, paromomycin, dihydrostreptomycin, gentamicin C1a, hygromycin, kanamycin, netilmicin, spectinomycin, sisomicin, streptomycin, and tobramycin in honey, milk, and pork samples by LC with tandem MS and molecularly imprinted polymer (MIP) SPE. The AG antibiotics in milk and homogenated meat samples were extracted with a solution composed of 10 mmol/L potassium dihydrogen phosphate, 0.4 mmol/L EDTA-Na₂, and 2% trichloroacetic acid. For honey samples, the extractant was 50 mmol/L potassium dihydrogen phosphate. The extracts were cleaned up with MIP SPE cartridges. The separation was performed on a zwitter ionic-HILIC column (50 × 2.1 mm, 3.5 μm), with the mobile phase consisting of methanol, 0.3% formic acid, and 175 mmol/L ammonium formate at 0.50 mL/min in gradient elution. A triple-quadrupole mass spectrometer equipped with an electrospray ionization source, which was operated in positive mode, was used for detection. The quantification was based on matrix-matched calibration curves. The method was applied to real samples with three different matrixes. The LODs of the method were 2-30 μg/kg and the LOQs were 7-100 μg/kg; the average recovery ranged from 78.2 to 94.8%; intraday RSDs and interday RSDs were ≤15 and ≤18%, respectively; and the absolute values of matrix effect for all AGs were RSDs ≤23%.

  16. Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up.

    Science.gov (United States)

    Helaleh, Murad I H; Al-Rashdan, Amal; Ibtisam, A

    2012-05-30

    An automated pressurized liquid extraction (PLE) method followed by Power Prep™ clean-up was developed for organochlorinated pesticide (OCP) and polychlorinated biphenyl (PCB) analysis in environmental marine samples of fish, squid, bivalves, shells, octopus and shrimp. OCPs and PCBs were simultaneously determined in a single chromatographic run using gas chromatography-mass spectrometry-negative chemical ionization (GC-MS-NCI). About 5 g of each biological marine sample was mixed with anhydrous sodium sulphate and placed in the extraction cell of the PLE system. PLE is controlled by means of a PC using DMS 6000 software. Purification of the extract was accomplished using automated Power Prep™ clean-up with a pre-packed disposable silica column (6 g) supplied by Fluid Management Systems (FMS). All OCPs and PCBs were eluted from the silica column using two types of solvent: 80 mL of hexane and a 50 mL mixture of hexane and dichloromethane (1:1). A wide variety of fish and shellfish were collected from the fish market and analyzed using this method. The total PCB concentrations were 2.53, 0.25, 0.24, 0.24, 0.17 and 1.38 ng g(-1) (w/w) for fish, squid, bivalves, shells, octopus and shrimp, respectively, and the corresponding total OCP concentrations were 30.47, 2.86, 0.92, 10.72, 5.13 and 18.39 ng g(-1) (w/w). Lipids were removed using an SX-3 Bio-Beads gel permeation chromatography (GPC) column. Analytical criteria such as recovery, reproducibility and repeatability were evaluated through a range of biological matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. A salting out-acetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics.

    Science.gov (United States)

    Dong, Hao; Guo, Xindong; Xian, Yanping; Luo, Haiying; Wang, Bin; Wu, Yuluan

    2015-11-27

    A sensitive gas chromatography-mass spectrometry method was established for the simultaneous determination of thirteen N-nitrosamines (NAs) in skin care cosmetics. The cosmetics samples were firstly dispersed by water and subsequently extracted and purified using salting out-acetonitrile homogeneous extraction method. Finally, the extracting solution was concentrated by slow nitrogen gas blowing. All of the samples were separated by INNOWAX capillary chromatographic column, and detected by selected ion monitoring (SIM) mode of gas chromatography-mass spectrometry (GC-MS) and quantified by isotope internal standard method. The method was validated for linearity and range, accuracy, precision and sensitivity. Under the optimized condition, the calibration curves were linear over the selected concentration ranges of 2-500μg/L for all the thirteen analytes, with calculated coefficients of determination (R(2)) of greater than 0.996. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 3-15μg/kg and 10-50μg/kg, respectively. Recoveries were calculated at three levels of concentration spiked in two kinds of cosmetics (skin care cream and water). The values were found between 93.8% and 121.0% with relative standard deviation (RSD) values of 2.5-7.2% for intra-day precision (n=6) and 3.3-6.7% for inter-day precision (n=5). The method was successfully applied to analyze twenty-two cosmetics samples and N-nitrosodimethylamine (NDMA) was detected in one sample with the concentration of 207μg/kg. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Effect of borneol on the transdermal permeation of drugs with differing lipophilicity and molecular organization of stratum corneum lipids.

    Science.gov (United States)

    Yi, Qi-Feng; Yan, Jin; Tang, Si-Yuan; Huang, Hui; Kang, Li-Yang

    2016-01-01

    The aim of the present paper was to investigate the promoting activity of borneol on the transdermal permeation of drugs with differing lipophilicity, and probe its alterations in molecular organization of stratum corneum (SC) lipids. The toxicity of borneol was evaluated in epidermal keratinocyte HaCaT and dermal fibroblast CCC-HSF-1 cell cultures and compared to known enhancers, and its irritant profile was also assessed by transepidermal water loss (TEWL) evaluation. The promoting effect of borneol on the transdermal permeation of five model drugs, namely 5-fluorouracil, antipyrine, aspirin, salicylic acid and ibuprofen, which were selected based on their lipophilicity denoted by logp value, were performed using in vitro skin permeation studies. Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) was employed to monitor the borneol-induced alteration in molecular organization of SC lipids. The enhancer borneol displayed lower cytotoxicity or irritation in comparison to the well-established and standard enhancer Azone. Borneol could effectively promote the transdermal permeation of five model drugs, and its enhancement ratios were found to be parabolic curve with the logp values of drugs, which exhibited the optimum permeation activity for relatively hydrophilic drugs (an estimated logp value of -0.5 ∼0.5). The molecular mechanism studies suggested that borneol could perturb the structure of SC lipid alkyl chains, and extract part of SC lipids, resulting in the alteration in the skin permeability barrier.

  19. Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography.

    Science.gov (United States)

    Djozan, Djavanshir; Farajzadeh, Mir Ali; Sorouraddin, Saeed Mohammad; Baheri, Tahmineh

    2012-07-27

    In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1 μL of the settled organic phase was injected into gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10-1500 ng mL(-1) (MAMP) and 50-1500 ng mL(-1) (MDMA), and the detection limits (LODs) were 2 and 18 ng mL(-1), respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100 ng mL(-1) of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80-88%. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Nanotechnology approaches for pain therapy through transdermal drug delivery.

    Science.gov (United States)

    Peptu, Cristian; Rotaru, Razvan; Ignat, Leonard; Humelnicu, Andra Cristina; Harabagiu, Valeria; Peptu, Catalina Anisoara; Leon, Maria-Magdalena; Mitu, Florin; Cojocaru, Elena; Boca, Andreea; Tamba, Bogdan Ionel

    2015-01-01

    The paper focuses on the advances in the field of pain treatment by transdermal delivery of specific drugs. Starting from a short description of the skin barrier, the pharmacodynamics and pharmacokinetics including absorption, distribution, action mechanism, metabolism and toxicity, aspects related to the use of pain therapy drugs are further discussed. Most recent results on topical anesthetic agents as well as the methods proved to overcome the skin barrier and to provide efficient delivery of the drug are also discussed. The present review is proposing to summarize the recent literature on the pharmacotherapeutic principles of local anesthetics and non-steroidal anti-inflammatory drugs, generally used to alleviate pain but also the drugs as nanoformulations with potential applications in transdermal delivery. A special attention is given to efficient formulations meant for transdermal penetration enhancement of anesthetics where the drug is encapsulated into macrocyclic molecules (cyclodextrins, cyclodextrin derivatives), liposomes or polymer nanoparticles and hydrogels.

  1. Ethosomes as delivery system for transdermal administration of vinpocetine.

    Science.gov (United States)

    Mao, Yan-Ting; Hua, Hai-Ying; Zhang, Xiang-Guo; Zhu, Dong-Xue; Li, Feng; Gui, Zhen-Hua; Zhao, Yong-Xing

    2013-05-01

    The purpose of the present study was to develop a novel transdermal vinpocetine patch containing a stable formulation and with good entrapment efficiency, and percutaneous absorption which via ethosome. Ethosome was found to be a more efficient delivery carrier with high encapsulation capacities (79.5% +/- 1.8%) and nanometric size (180.7 +/- 1.5 nm). In vitro percutaneous permeation experiments demonstrated that the permeation of vinpocetine through abdominal skin of Sprague Dawley was significantly increased when ethosome was used. The vinpocetine transdermal fluxes from ethosome gel (3.56 +/- 0.13 microg/cm2/h) were 6.72 and 3.10 times higher than that of vinpocetine gel solution and vinpocetine aueous solution, respectively. Furthermore, the AUC(0 --> infinity), and eliminiation half-life by the transdermal administration were significantly higher than those by the intragastric administration (P ethosome is a promising vesicular carrier for enhancing percutaneous absorption of vinpocetine.

  2. Transdermal Delivery of Drugs with Microneedles—Potential and Challenges

    Directory of Open Access Journals (Sweden)

    Kevin Ita

    2015-06-01

    Full Text Available Transdermal drug delivery offers a number of advantages including improved patient compliance, sustained release, avoidance of gastric irritation, as well as elimination of pre-systemic first-pass effect. However, only few medications can be delivered through the transdermal route in therapeutic amounts. Microneedles can be used to enhance transdermal drug delivery. In this review, different types of microneedles are described and their methods of fabrication highlighted. Microneedles can be fabricated in different forms: hollow, solid, and dissolving. There are also hydrogel-forming microneedles. A special attention is paid to hydrogel-forming microneedles. These are innovative microneedles which do not contain drugs but imbibe interstitial fluid to form continuous conduits between dermal microcirculation and an attached patch-type reservoir. Several microneedles approved by regulatory authorities for clinical use are also examined. The last part of this review discusses concerns and challenges regarding microneedle use.

  3. Transdermal Delivery of Drugs with Microneedles—Potential and Challenges

    Science.gov (United States)

    Ita, Kevin

    2015-01-01

    Transdermal drug delivery offers a number of advantages including improved patient compliance, sustained release, avoidance of gastric irritation, as well as elimination of pre-systemic first-pass effect. However, only few medications can be delivered through the transdermal route in therapeutic amounts. Microneedles can be used to enhance transdermal drug delivery. In this review, different types of microneedles are described and their methods of fabrication highlighted. Microneedles can be fabricated in different forms: hollow, solid, and dissolving. There are also hydrogel-forming microneedles. A special attention is paid to hydrogel-forming microneedles. These are innovative microneedles which do not contain drugs but imbibe interstitial fluid to form continuous conduits between dermal microcirculation and an attached patch-type reservoir. Several microneedles approved by regulatory authorities for clinical use are also examined. The last part of this review discusses concerns and challenges regarding microneedle use. PMID:26131647

  4. Transdermal Delivery of Drugs with Microneedles-Potential and Challenges.

    Science.gov (United States)

    Ita, Kevin

    2015-06-29

    Transdermal drug delivery offers a number of advantages including improved patient compliance, sustained release, avoidance of gastric irritation, as well as elimination of pre-systemic first-pass effect. However, only few medications can be delivered through the transdermal route in therapeutic amounts. Microneedles can be used to enhance transdermal drug delivery. In this review, different types of microneedles are described and their methods of fabrication highlighted. Microneedles can be fabricated in different forms: hollow, solid, and dissolving. There are also hydrogel-forming microneedles. A special attention is paid to hydrogel-forming microneedles. These are innovative microneedles which do not contain drugs but imbibe interstitial fluid to form continuous conduits between dermal microcirculation and an attached patch-type reservoir. Several microneedles approved by regulatory authorities for clinical use are also examined. The last part of this review discusses concerns and challenges regarding microneedle use.

  5. [Simultaneous analysis of 14 short- and long-chain perfluorinated compounds in water by liquid chromatography-tandem mass spectrometry using solid phase extraction].

    Science.gov (United States)

    Wang, Chao; Lü, Yibing; Chen, Haijun; Tan, Li; Teng, Enjiang

    2014-09-01

    A solid phase extraction (SPE)-ultrahigh pressure liquid chromatography (UPLC) method coupled with tandem mass spectrometry was developed for the simultaneous analysis of the 14 short- and long-chain perfluorinated compounds (PFCs) in water. Water sample was concentrated and purified through WAX mixed-mode SPE cartridges. The separation of PFCs was performed on a BEH C18 column with gradient elution using methanol-5 mmol/L ammonium acetate as mobile phases. The PFCs were quantified by internal standard method in multiple-reaction monitoring mode. The calibration curves of the 14 PFCs were linear in the range of 0.1-50 μg/L with the correlation coefficients > 0.99. The limits of detection (S/N = 3) and quantitation (S/N = 10) of the method were 0.09-1.15 ng/L and 0.29-3.85 ng/L, respectively. The average recoveries of eight PFCs at three spiked levels of 2, 10 and 20 ng/L were 85.0%, 120.2% and 117.4%, with the relative standard deviations of 9.2%, 9.0% and 6.6%, respectively. The recoveries of the rest six PFCs were low due to unavoidable strong adsorption on the bottle/tube walls during sample pretreatment. The method was applied in the determination of PFCs in real samples of a lake in South China. Four short-chain and five long-chain PFCs were detected with mass concentrations of 41.29-49.05 ng/L and 98.43-111.02 ng/L, respectively. The results show that the method is suitable for the simultaneous analysis of short- and long-chain perfluorinated compounds in environmental water.

  6. Transdermal testosterone replacement therapy in men

    Science.gov (United States)

    Ullah, M Iftekhar; Riche, Daniel M; Koch, Christian A

    2014-01-01

    Androgen deficiency syndrome in men is a frequently diagnosed condition associated with clinical symptoms including fatigue, decreased libido, erectile dysfunction, and metabolic syndrome. Serum testosterone concentrations decline steadily with age. The prevalence of androgen deficiency syndrome in men varies depending on the age group, known and unknown comorbidities, and the respective study group. Reported prevalence rates may be underestimated, as not every man with symptoms of androgen deficiency seeks treatment. Additionally, men reporting symptoms of androgen deficiency may not be correctly diagnosed due to the vagueness of the symptom quality. The treatment of androgen deficiency syndrome or male hypogonadism may sometimes be difficult due to various reasons. There is no consensus as to when to start treating a respective man or with regards to the best treatment option for an individual patient. There is also lack of familiarity with treatment options among general practitioners. The formulations currently available on the market are generally expensive and dose adjustment protocols for each differ. All these factors add to the complexity of testosterone replacement therapy. In this article we will discuss the general indications of transdermal testosterone replacement therapy, available formulations, dosage, application sites, and recommended titration schedule. PMID:24470750

  7. Simultaneous analysis of nine aromatic amines in mainstream cigarette smoke using online solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Jie; Bai, Ruoshi; Zhou, Zhaojuan; Liu, Xingyu; Zhou, Jun

    2017-04-01

    A fully automated analytical method was developed and validated by this present study. The method was based on two-dimensional (2D) online solid-phase extraction liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) to determine nine aromatic amines (AAs) in mainstream smoke (MSS) simultaneously. As a part of validation process, AAs yields for 16 top-selling commercial cigarettes from China market were evaluated by the developed method under both Health Canada Intensive (HCI) and ISO machine smoking regimes. The gas phase of MSS was trapped by 25 mL 0.6 M hydrochloric acid solution, while the particulate phase was collected on a glass fiber filter. Then, the glass fiber pad was extracted with hydrochloric acid solution in an ultrasonic bath. The extract was analyzed with 2D online SPE-LC-MS/MS. In order to minimize the matrix effects of sample on each analyte, two cartridges with different extraction mechanisms were utilized to cleanup disturbances of different polarity, which were performed by the 2D SPE. A phenyl-hexyl analytical column was used to achieve a chromatographic separation. Under the optimized conditions, the isomers of p-toluidine, m-toluidine and o-toluidine, 3-aminobiphenyl and 4-aminobiphenyl, and 1-naphthylamine and 2-naphthylamine were baseline separated with good peak shapes for the first time. The limits of detection for nine AAs ranged from 0.03 to 0.24 ng cig-1. The recovery of the measurement of nine AAs was from 84.82 to 118.47%. The intra-day and inter-day precisions of nine AAs were less than 10 and 16%, respectively. Compared with ISO machine smoking regime, the AAs yields in MSS were 1.17 to 3.41 times higher under HCI machine smoking regime. Graphical abstract New method using online SPE-LC/MS/MS for analysis of aromatic amines in mainstream cigarette smoke.

  8. Maintaining Breast Cancer Specimen Integrity and Individual or Simultaneous Extraction of Quality DNA, RNA, and Proteins from Allprotect-Stabilized and Nonstabilized Tissue Samples

    LENUS (Irish Health Repository)

    Mee, Blanaid C.

    2011-12-29

    The Saint James\\'s Hospital Biobank was established in 2008, to develop a high-quality breast tissue BioResource, as a part of the breast cancer clinical care pathway. The aims of this work were: (1) to ascertain the quality of RNA, DNA, and protein in biobanked carcinomas and normal breast tissues, (2) to assess the efficacy of AllPrep® (Qiagen) in isolating RNA, DNA, and protein simultaneously, (3) to compare AllPrep with RNEasy® and QIAamp® (both Qiagen), and (4) to examine the effectiveness of Allprotect® (Qiagen), a new tissue stabilization medium in preserving DNA, RNA, and proteins. One hundred eleven frozen samples of carcinoma and normal breast tissue were analyzed. Tumor and normal tissue morphology were confirmed by frozen sections. Tissue type, tissue treatment (Allprotect vs. no Allprotect), extraction kit, and nucleic acid quantification were analyzed by utilizing a 4 factorial design (SPSS PASW 18 Statistics Software®). QIAamp (DNA isolation), AllPrep (DNA, RNA, and Protein isolation), and RNeasy (RNA isolation) kits were assessed and compared. Mean DNA yield and A260\\/280 values using QIAamp were 33.2 ng\\/μL and 1.86, respectively, and using AllPrep were 23.2 ng\\/μL and 1.94. Mean RNA yield and RNA Integrity Number (RIN) values with RNeasy were 73.4 ng\\/μL and 8.16, respectively, and with AllPrep were 74.8 ng\\/μL and 7.92. Allprotect-treated tissues produced higher RIN values of borderline significance (P=0.055). No discernible loss of RNA stability was detected after 6 h incubation of stabilized or nonstabilized tissues at room temperature or 4°C or in 9 freeze-thaw cycles. Allprotect requires further detailed evaluation, but we consider AllPrep to be an excellent option for the simultaneous extraction of RNA, DNA, and protein from tumor and normal breast tissues. The essential presampling procedures that maintain the diagnostic integrity of pathology specimens do not appear to compromise the quality of molecular isolates.

  9. Transdermal fentanyl matrix patches Matrifen and Durogesic DTrans are bioequivalent

    DEFF Research Database (Denmark)

    Kress, Hans G; Boss, Hildegard; Delvin, Thomas

    2010-01-01

    AIM: The pharmacokinetic profiles of the two commercially available transdermal fentanyl patches Matrifen (100 microg/h) and Durogesic DTrans (100 microg/h), used to manage severe chronic pain, were compared regarding their systemic exposure, rate of absorption, and safety. METHODS: Transdermal...... matrix fentanyl patches [Matrifen or Durogesic DTrans (100 microg/h)] were applied for 72 h to 30 healthy male subjects in a randomized, four-period (two replicated treatment sequences), crossover study; 28 subjects completed the study. The pharmacokinetic parameters of fentanyl were determined for 144 h...

  10. New and emerging contraceptive options: a focus on transdermal contraception

    Directory of Open Access Journals (Sweden)

    Böttcher B

    2014-01-01

    Full Text Available Bettina Böttcher, Ludwig WildtDepartment of Gynecologic Endocrinology and Reproductive Medicine, Innsbruck Medical University, Innsbruck, AustriaAbstract: Transdermal contraception is a convenient way of hormonal contraception that allows weekly application of a patch for 3 consecutive weeks followed by a patch-free week. Efficacy, side effects, advantages, and disadvantages as well as patient satisfaction with this formulation are discussed in this short review. The first patch, introduced in 2002, contained ethinylestradiol and norelgestromin. Recently, a new patch containing gestodene as the gestagen component has been developed. Early data for this formulation are presented.Keywords: transdermal contraception, skin patch

  11. Transdermal carbamate poisoning – a case of misuse

    Directory of Open Access Journals (Sweden)

    Lalit Kumar Rajbanshi

    2017-01-01

    Full Text Available Acute pesticide poisoning is a common mode of intentional self harm. Oral ingestion is the usual mode of poisoning. However, inhalation, accidental or occupational transdermal exposure leading to acute or chronic poisoning can be the other route of poisoning. It has been seen that the purpose of poising is suicidal intensity in most of the cases. We report an unusual case where the victim had acute pesticide poisoning through transdermal route that was intended for non suicidal purpose. The patient was managed successfully with immediate decontamination and adequate antidote.

  12. Microfluidic-enabled liposomes elucidate size-dependent transdermal transport.

    Directory of Open Access Journals (Sweden)

    Renee R Hood

    Full Text Available Microfluidic synthesis of small and nearly-monodisperse liposomes is used to investigate the size-dependent passive transdermal transport of nanoscale lipid vesicles. While large liposomes with diameters above 105 nm are found to be excluded from deeper skin layers past the stratum corneum, the primary barrier to nanoparticle transport, liposomes with mean diameters between 31-41 nm exhibit significantly enhanced penetration. Furthermore, multicolor fluorescence imaging reveals that the smaller liposomes pass rapidly through the stratum corneum without vesicle rupture. These findings reveal that nanoscale liposomes with well-controlled size and minimal size variance are excellent vehicles for transdermal delivery of functional nanoparticle drugs.

  13. Simultaneous Determination and Pharmacokinetic Study of Quercetin, Luteolin, and Apigenin in Rat Plasma after Oral Administration of Matricaria chamomilla L. Extract by HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiaoxv Dong

    2017-01-01

    Full Text Available A simple and sensitive HPLC-UV method has been developed for the simultaneous determination of quercetin, luteolin, and apigenin in rat plasma after oral administration of Matricaria chamomilla L. extract. The flow rate was set at 1.0 ml/min and the detection wavelength was kept at 350 nm. The calibration curves were linear in the range of 0.11–11.36 μg/ml for quercetin, 0.11–11.20 μg/ml for luteolin, and 0.11–10.60 μg/ml for apigenin, respectively. The intraday and interday precisions (RSD were less than 8.32 and 8.81%, respectively. The lower limits of quantification (LLOQ of the three compounds were 0.11 μg/ml. The mean recoveries for quercetin, luteolin, and apigenin were 99.11, 95.62, and 95.21%, respectively. Stability studies demonstrated that the three compounds were stable in the preparation and analytical process. The maximum plasma concentration (Cmax was 0.29 ± 0.06, 3.04 ± 0.60, and 0.42 ± 0.10 μg/ml, respectively. The time to reach the maximum plasma concentration (Tmax was 0.79 ± 0.25, 0.42 ± 0.09, and 0.51 ± 0.13 h, respectively. The validated method was successfully applied to investigate the pharmacokinetics study of quercetin, luteolin, and apigenin in rat plasma after oral administration of M. chamomilla extract.

  14. High-throughput salting-out assisted liquid/liquid extraction with acetonitrile for the simultaneous determination of simvastatin and simvastatin acid in human plasma with liquid chromatography.

    Science.gov (United States)

    Zhang, Jun; Rodila, Ramona; Gage, Eric; Hautman, Mathew; Fan, Leimin; King, Linda L; Wu, Huaiqin; El-Shourbagy, Tawakol A

    2010-02-28

    Simvastatin (SS) is an effective cholesterol-lowering medicine, and is hydrolyzed to simvastatin acid (SSA) after oral administration. Due to SS and SSA inter-conversion and its pH and temperature dependence, SS and SSA quantitation is analytically challenging. Here we report a high-throughput salting-out assisted liquid/liquid extraction (SALLE) method with acetonitrile and mass spectrometry compatible salts for simultaneous LC-MS/MS analysis of SS and SSA. The sample preparation of a 96-well plate using SALLE was completed within 20 min, and the SALLE extract was diluted and injected into an LC-MS/MS system with a cycle time of 2.0 min/sample. The seamless interface of SALLE and LC-MS eliminated drying down step and thus potential sample exposure to room or higher temperature. The stability of SS and SSA in various concentration ratios in plasma was evaluated at room and low (4 degrees C) temperature and the low temperature (4 degrees C) was found necessary to maintain sample integrity. The short sample preparation time along with controlled temperature (2-4 degrees C) and acidity (pH 4.5) throughout sample preparation minimized the conversion of SS-->SSA to SS to 0.00% The method was validated with a lower limit of quantitation (LLOQ) of 0.094 ng mL(-1) for both SS and SSA and a sample volume of 100 microL. The method was used for a bioequivalence study with 4048 samples. Incurred sample reproducibility (ISR) analysis of 362 samples from the study exceeded ISR requirement with 99% re-analysis results within 100+/-20% of the original analysis results. Copyright 2010 Elsevier B.V. All rights reserved.

  15. Simultaneous determination nucleosides in marine organisms using ultrasound-assisted extraction followed by hydrophilic interaction liquid chromatography-electrospray ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhao, Hengqiang; Chen, Junhui; Shi, Qian; Li, Xin; Zhou, Wenhui; Zhang, Daolai; Zheng, Li; Cao, Wei; Wang, Xiaoru; Lee, Frank Sen-Chun

    2011-10-01

    A new method has been developed based on ultrasound-assisted extraction (UAE) followed by hydrophilic interaction chromatography (HILIC) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) for the simultaneous determination of 16 nucleosides and nucleobases in medicinal extracts of various marine organisms. The separation was achieved on a Venusil HILIC column (250×4.6 mm id, 5 μm) and gradient elution using a solution of acetonitrile and buffer (0.20% formic acid and 20 mmol/L ammonium acetate) as the mobile phase. Identification of the 16 target nucleosides and nucleobases was based on the retention time, UV spectra, and mass measurements of the protonated molecules ([M+H](+)) and main fragment ions (ESI-TOF/MS). In addition, non-target compounds of 2'-deoxyinosine and four other amino acids were also tentatively identified by ESI-TOF/MS. The 16 target compounds were quantified by HILIC-ESI-TOF/MS under optimized mass conditions. All calibration curves showed good linearity (r(2)>0.9951). The recoveries were 84.72-124.10%, and the limits of detection of the 16 target compounds were 0.6-130.0 ng/mL. The developed method was applied to quantify the target compounds in 15 batches of various marine organisms. The method has potential applicability for the identification and determination of highly polar and low-concentration active compounds in marine organisms. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Simultaneous determination of sugars and picrosides in Picrorhiza species using ultrasonic extraction and high-performance liquid chromatography with evaporative light scattering detection.

    Science.gov (United States)

    Bhandari, Pamita; Kumar, Neeraj; Singh, Bikram; Kaul, Vijay K

    2008-06-20

    Sugars play a critical role in regulating overall cellular metabolism in high altitude growing plants. These plants are shown to have high levels of sugars to enhance their tolerance to abiotic stresses such as drought and freezing temperature. In the present study, a simple, sensitive, selective and reliable HPLC method based on ultrasonic extraction and evaporative light scattering detection (ELSD) has been developed and validated for the simultaneous determination of important sugars (xylose, xylitol, mannitol, glucose and sucrose) and picrosides (picroside-I and picroside-II) in two species Picrorhiza kurroa and P. scrophulariiflora. The analysis was carried out on a Zorbax amino column (250 mm x 4.6 mm i.d., 5 microm) with isocratic elution of acetonitrile:water (78:22, v/v). The method was validated for accuracy, precision, limit of detection and quantification according to International Conference on Harmonization (ICH) guidelines. The drift tube temperature of the ELSD system was set to 81 degrees C and nitrogen flow rate was 2.0 standard liter per minute (SLM). The regression equation revealed a good linear relationship (r(2)=0.9997+/-0.0012) within test ranges. The limit of detection and quantification for seven analytes in ELSD were less than 0.98 and 2.95 microg, respectively. The method showed good reproducibility for the quantification of seven analytes in Picrorhiza species with intra- and inter-day variation of less than 2.0%.

  17. Simultaneous determination of 14 disinfection by-products in meat products using microwave-assisted extraction and static headspace coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cardador, Maria Jose; Gallego, Mercedes

    2017-08-04

    This paper described the first analytical method to simultaneously determine 14 disinfection by-products (DBPs) in meat products using microwave-assisted extraction (MAE) and static headspace (SHS) followed by gas chromatography-mass spectrometry (GC-MS). The DBPs included were 4 trihalomethanes, 7 haloacetic acids, 2 haloacetonitriles and trichloronitromethane, which are commonly formed as a consequence of the disinfection process of water. The combination of the MAE and SHS techniques allows meat samples to be analysed in two sequential steps into the same HS vial in spite of the sample's complexity. Detection limits were obtained within the range of 0.06-0.70ng/g, and the average relative standard deviation was 7.4%. Recoveries throughout the whole process were between 86 and 95%. The SHS-GC-MS method was applied to determine DBPs in meat products with different industrial processing which could be contaminated through contact with disinfectants and/or treated water employed in the factory either for washing or for the cooking of meat. Up to 5 DBPs were found at ng/g levels in about 36% of the samples analysed, cooked ham being the most contaminated meat product because of the brine solutions employed in its manufacturing process. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Simultaneous Determination and Pharmacokinetic Study of Six Components in Rat Plasma by HPLC-MS/MS after Oral Administration of Acanthopanax sessiliflorus Fruit Extract

    Directory of Open Access Journals (Sweden)

    Peng Du

    2016-12-01

    Full Text Available A specific and reliable HPLC-MS/MS method was developed and validated for the simultaneous determination of protocatechuic acid (PCA, scopolin, (−-pinoresinol-4,4′-di-O-β-d-glucopyranoside (PDG, acanthoside D, acanthoside B and hyperin in rat plasma for the first time. The analytes were separated on a C18 column (50 × 2.1 mm, 1.8 µm and a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI source was used for detection. The rat plasma sample was prepared using the protein precipitation procedure. The calibration curves were linear over a concentration range of 1.2–1200.0 ng/mL for PCA, 0.96–960.0 ng/mL for scopolin, 1.12–1120.0 ng/mL for PDG, 1.32–1320.0 ng/mL for acanthoside D, 0.99–990.0 ng/mL for acanthoside B and 1.01–1010.0 ng/mL for hyperin. The intra-day and inter-day precision was less than 11.4% and the relative error (RE was all within ±15%. The validated method was successfully applied to assess the pharmacokinetics characteristics after the extracts of Acanthopanax sessiliflorus fruits were orally administered to the Sprague-Dawley rat.

  19. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  20. Analgesic and anti-inflammatory activity and pharmacokinetics of alkaloids from seeds of Strychnos nux-vomica after transdermal administration: effect of changes in alkaloid composition.

    Science.gov (United States)

    Chen, Jun; Wang, Xuan; Qu, Yan-Ge; Chen, Zhi-Peng; Cai, Hao; Liu, Xiao; Xu, Fei; Lu, Tu-Lin; Cai, Bao-Chang

    2012-01-06

    Strychnos nux-vomica L. (Loganiaceae) is grown extensively in southern Asian countries. The dried seed of this plant, nux vomica, has been clinically used in Chinese folk medicine for improving blood circulation, relieving rheumatic pain, reducing swelling and treating cancer. This study was carried out to investigate the effect of removing most strychnine from the total alkaloid fraction (TAF) extracted from nux vomica on analgesic and anti-inflammatory activity and pharmacokinetics after transdermal administration. Most strychnine was removed from TAF and the resulted modified total alkaloid fraction (MTAF) was obtained. The contents of strychnine and brucine in TAF and MTAF were determined. Then the analgesic and anti-inflammatory activity of TAF, MTAF, brucine and strychnine dissolved in hydrogel was compared after transdermal administration. Furthermore, in vitro and in vivo transdermal absorption profiles of brucine after administration of TAF, MTAF and brucine dissolved in hydrogel were also compared. In contrast to TAF, most strychnine was removed from MTAF and the ratio of brucine to strychnine was adjusted from 1:1.8 to 2.7:1. MTAF showed significant analgesic activity in all the chemical-, thermal- and physical- induced nociception models, which indicated the presence of both centrally and peripherally mediated activities. MTAF also showed significant anti-inflammatory activity against xylene-induced ear edema. But TAF and strychnine demonstrated little activity in all those pharmacological tests. Brucine showed to be effective in acetic acid-induced writhing and xylene-induced ear edema test. Brucine in MTAF was absorbed more completely than it alone at the same dosage of brucine after transdermal administration. The results from the present study appeared to support the viewpoint that most strychnine should be removed from TAF to improve analgesic and anti-inflammatory activity. The relatively higher pharmacological activity of MTAF compared to brucine

  1. Formulation and Development of Dendrimer-Based Transdermal ...

    African Journals Online (AJOL)

    Purpose: To develop transdermal patches of meloxicam (MLX) using chitosan and hydroxypropyl methylcellulose (HPMC) and polyvinyl alcohol (PVA) as hydrophilic polymers, polyamido amine (PAMAM) dendrimer as a permeation enhancer, and dibutyl pthalate as a plasticizer. Methods: The patches were prepared by ...

  2. Penetration Enhancement Effect of Turpentine Oil on Transdermal ...

    African Journals Online (AJOL)

    irritation/discomfort, no drug-drug interaction, prolonged drug release, controlled therapeutic responses and improved patient compliance [6-. 8]. Transdermal films/patches are a practical and feasible dosage form in that there is better patient compliance and are very suited for chronic pain and inflammation management in.

  3. Design and Development of a Proniosomal Transdermal Drug ...

    African Journals Online (AJOL)

    Patrick Erah

    Design and Development of a Proniosomal. Transdermal Drug Delivery System for Captopril. Ankur Gupta*, Sunil Kumar Prajapati, M Balamurugan, Mamta. Singh .... beadlets 12, microcapsules 13 bioadhesive system 14, floating tablets and capsules 15, semisolid matrix systems16, and microspheres17. Proniosomes ...

  4. Diclofenac transdermal patch versus the sustained release tablet: A ...

    African Journals Online (AJOL)

    therapeutic advantages over conventional oral tablets in terms of prolonged release and improvement of ... arthritic therapy. Non-steroidal anti-inflammatory drugs (NSAIDs) are prescribed frequently for the management of pain and local inflammation. (similar to gout) [5]. ... systems, transdermal films/patches are the most.

  5. Formulation and In vitro Evaluation of Carvedilol Transdermal ...

    African Journals Online (AJOL)

    Table I: Optimization designs for the development of carvedilol transdermal drug delivery system. (TDDS). Formulation code. Treatment. Level of PMMA, ... Low oral bioavailability (25 %) due to extensive first pass metabolism, a short ..... Implantable therapeutic systems. In: Robinson, J.R.; Vincent HL. Editors. Controlled.

  6. Silicon micromachined hollow microneedles for transdermal liquid transfer

    NARCIS (Netherlands)

    Gardeniers, Johannes G.E.; Berenschot, Johan W.; de Boer, Meint J.; Yeshurun, Y.; Hefetz, M.; van 't Oever, R.; van den Berg, Albert

    2002-01-01

    This paper presents an improved design and fabrication process [ 13 for hollow micro needles with the proper mechanical strength and sharpness to be applied for painless transdermal transfer of liquids. Tests have shown that liquids like blood are drawn into the needle by capillary forces, reducing

  7. Design and Development of a Proniosomal Transdermal Drug ...

    African Journals Online (AJOL)

    Purpose: The aim of the study was to develop a proniosomal carrier system for captopril for the treatment of hypertension that is capable of efficiently delivering entrapped drug over an extended period of time. Method: The potential of proniosomes as a transdermal drug delivery system for captopril was investigated by ...

  8. Microneedles: a valuable physical enhancer to increase transdermal drug delivery.

    Science.gov (United States)

    Escobar-Chávez, José Juan; Bonilla-Martínez, Dalia; Villegas-González, Martha Angélica; Molina-Trinidad, Eva; Casas-Alancaster, Norma; Revilla-Vázquez, Alma Luisa

    2011-07-01

    Transdermal drug delivery offers an attractive alternative to the conventional drug delivery methods of oral administration and injection. However, the stratum corneum acts as a barrier that limits the penetration of substances through the skin. Recently, the use of micron-scale needles in increasing skin permeability has been proposed and shown to dramatically increase transdermal delivery. Microneedles have been fabricated with a range of sizes, shapes, and materials. Most in vitro drug delivery studies have shown these needles to increase skin permeability to a broad range of drugs that differ in molecular size and weight. In vivo studies have demonstrated satisfactory release of oligonucleotides and insulin and the induction of immune responses from protein and DNA vaccines. Microneedles inserted into the skin of human subjects were reported to be painless. For all these reasons, microneedles are a promising technology to deliver drugs into the skin. This review presents the main findings concerning the use of microneedles in transdermal drug delivery. It also covers types of microneedles, their advantages and disadvantages, enhancement mechanisms, and trends in transdermal drug delivery.

  9. MICRONEEDLES AS A WAY TO INCREASE THE TRANSDERMAL INSULIN DELIVERY

    Directory of Open Access Journals (Sweden)

    E. G. Kuznetsova

    2016-01-01

    Full Text Available Aim: to prove the possibility of increasing the diffusion of insulin through the skin in vitro with pre-applying microneedles.Materials and methods. Microemulsion for transdermal therapeutic system of insulin has been used in vitro studies. Genetically engineered human insulin has been used in this research. Applicators with silicon microneedles (40 and 150 microns long have been used to enhance the diffusion fl ux of drug substance. The dynamics of insulin release from the transdermal therapeutic systems through the rabbit skin has been studied in glass Franz diffusion cells in analyzer diffusion of drugs HDT 1000 (Copley Scientifi c Ltd., UK. Insulin has been labeled with fl uorescein isothiocyanate to separate the insulin absorption spectrum from the spectra of native skin proteins at spectrophotometer measurements.Results. The amounts of insulin delivered through the skin in vitro after previous application of microneedles of 40 and 150 microns are 282.5 ± 61.1 and 372.3 ± 7.0 microgram, respectively. This is 1.4 and 1.9 times more than in the transdermal system without microneedles.Conclusion. The conditions for increasing the diffusion of insulin through the skin in a model transdermal therapeutic system with microneedles (length – 150 microns, duration of pre-application – 1 hour have been found.

  10. Formulation effects of topical emulsions on transdermal and dermal delivery.

    Science.gov (United States)

    Otto, A; du Plessis, J; Wiechers, J W

    2009-02-01

    It has been recognized that the vehicle in which a permeant is applied to the skin has a distinctive effect on the dermal and transdermal delivery of active ingredients. The cutaneous and percutaneous absorptions can be enhanced, e.g. by an increase in thermodynamic activity, supersaturation and penetration modifiers. Furthermore, dermal and transdermal delivery can be influenced by the interactions that may occur between the vehicle and the skin on the one hand, and interactions between the active ingredient and the skin on the other hand. Emulsions are widely used as cosmetic and pharmaceutical formulations because of their excellent solubilizing capacities for lipophilic and hydrophilic active ingredients and application acceptability. This review focuses, in particular, on the effect of emulsions on the dermal and transdermal delivery of active ingredients. It is shown that the type of emulsion (w/o vs. o/w emulsion), the droplet size, the emollient, the emulsifier as well as the surfactant organization (micelles, lyotropic liquid crystals) in the emulsion may affect the cutaneous and percutaneous absorption. Examples substantiate the fact that emulsion constituents such as emollients and emulsifiers should be selected carefully for optimal efficiency of the formulation. Moreover, to understand the influence of emulsion on dermal and transdermal delivery, the physicochemical properties of the formulation after application are considered.

  11. Transferosomes - A vesicular transdermal delivery system for enhanced drug permeation

    Directory of Open Access Journals (Sweden)

    Reshmy Rajan

    2011-01-01

    Full Text Available Transdermal administration of drugs is generally limited by the barrier function of the skin. Vesicular systems are one of the most controversial methods for transdermal delivery of active substances. The interest in designing transdermal delivery systems was relaunched after the discovery of elastic vesicles like transferosomes, ethosomes, cubosomes, phytosomes, etc. This paper presents the composition, mechanisms of penetration, manufacturing and characterization methods of transferosomes as transdermal delivery systems of active substances. For a drug to be absorbed and distributed into organs and tissues and eliminated from the body, it must pass through one or more biological membranes/barriers at various locations. Such a movement of drug across the membrane is called as drug transport. For the drugs to be delivered to the body, they should cross the membranous barrier. The concept of these delivery systems was designed in an attempt to concentrate the drug in the tissues of interest, while reducing the amount of drug in the remaining tissues. Hence, surrounding tissues are not affected by the drug. In addition, loss of drug does not happen due to localization of drug, leading to get maximum efficacy of the medication. Therefore, the phospholipid based carrier systems are of considerable interest in this era.

  12. Avanafil Liposomes as Transdermal Drug Delivery for Erectile ...

    African Journals Online (AJOL)

    Purpose: To formulate avanafil, a recently approved phosphodiesterase-5 enzyme inhibitor, in liposomal form for enhanced transdermal permeation and bioavailability. Methods: Two preparation procedures were employed, leading to the formation of multilamellar vesicles (MLVs) and reverse-phase evaporation unilamellar ...

  13. Transferosomes - A vesicular transdermal delivery system for enhanced drug permeation

    Science.gov (United States)

    Rajan, Reshmy; Jose, Shoma; Mukund, V. P. Biju; Vasudevan, Deepa T.

    2011-01-01

    Transdermal administration of drugs is generally limited by the barrier function of the skin. Vesicular systems are one of the most controversial methods for transdermal delivery of active substances. The interest in designing transdermal delivery systems was relaunched after the discovery of elastic vesicles like transferosomes, ethosomes, cubosomes, phytosomes, etc. This paper presents the composition, mechanisms of penetration, manufacturing and characterization methods of transferosomes as transdermal delivery systems of active substances. For a drug to be absorbed and distributed into organs and tissues and eliminated from the body, it must pass through one or more biological membranes/barriers at various locations. Such a movement of drug across the membrane is called as drug transport. For the drugs to be delivered to the body, they should cross the membranous barrier. The concept of these delivery systems was designed in an attempt to concentrate the drug in the tissues of interest, while reducing the amount of drug in the remaining tissues. Hence, surrounding tissues are not affected by the drug. In addition, loss of drug does not happen due to localization of drug, leading to get maximum efficacy of the medication. Therefore, the phospholipid based carrier systems are of considerable interest in this era. PMID:22171309

  14. Development of Chitosan Acetate Films for Transdermal Delivery of ...

    African Journals Online (AJOL)

    Erah

    KSY Hemant* and HG Shivakumar. Department of Pharmaceutics, J.S.S. College of Pharmacy, JSS University, S.S. Nagar, Mysore-570 015, Karnataka,. India. Abstract. Purpose: To formulate and evaluate chitosan acetate films designed for transdermal delivery of propranolol hydrochloride. Methods: Chitosan acetate was ...

  15. Enhanced transdermal delivery of salbutamol sulfate via ethosomes

    OpenAIRE

    Bendas, Ehab R.; Tadros, Mina I.

    2007-01-01

    The main objective of the present work was to compare the transdermal delivery of salbutamol sulfate (SS), a hydrophilic drug used as a bronchodilator, from ethosomes and classic liposomes containing different cholesterol and dicetylphosphate concentrations. All the systems were characterized for shape, particle size, and entrapment efficiency percentage, by image analysis optical microscopy or transmission electron microscopy, laser diffraction, and ultracentrifugation, respectively. In vitr...

  16. Communication: Matrix type transdermal drug delivery systems of ...

    African Journals Online (AJOL)

    Communication: Matrix type transdermal drug delivery systems of metoprolol tartrate: skin toxicity and in vivo characterization. ... The statistical analysis was performed using GraphPad Instat 3 software. All the treatment groups showed significant (P < 0.05) and constant fall in BP up to 48 h. Formulation MT-4 was found to ...

  17. Efficacy and transdermal absorption of permethrin in scabies patients

    NARCIS (Netherlands)

    van der Rhee, H.J.; Farquhar, J A; Vermeulen, N P

    1989-01-01

    The clinical efficacy and transdermal absorption of permethrin, a new synthetic insecticide was investigated in ten scabies patients. All patients were successfully treated with one application of a cream, containing 5% permethrin. Apart from mild postscabies dermatitis no side-effects were

  18. Swellable silk fibroin microneedles for transdermal drug delivery.

    Science.gov (United States)

    Yin, Zhuping; Kuang, Dajiang; Wang, Shiyi; Zheng, Zhaozhu; Yadavalli, Vamsi K; Lu, Shenzhou

    2017-08-01

    In this paper, a swelling-modified silk fibroin (SF) microneedle for transdermal drug delivery is presented. The microneedles undergo a phase transition from a dried and rigid state to a semi-solid, acerose hydrogel state with a controlled 3-dimensional (3D) porous network structure. Different micromolecular reagents have been studied for mixing with aqueous silk fibroin to endow a swellable and insoluble capacity to the SF. The aqueous SF composite is poured on a polydimethylsiloxane (PDMS) mold with arranged micropores on its surface to fabricate SF microneedles with high fidelity and mechanical robustness. The results demonstrate that 2-ethoxyethanol (ECS) modified SF microneedles can easily pierce porcine skin with a depth of ∼200μm in vitro, and transform into semi-solid hydrogels with 50-700nm porous network inside. These swelling-modified microneedles can accomplish a significantly enhanced transdermal drug release capacity in proportion to their swelling characteristics. The better swelling capacity of the microneedles produces larger pores, resulting in higher transdermal drug release kinetics. There is also a relationship between swollen pore dimensions and the molecular weights of encapsulated therapeutics. The controllable properties of these SF microneedles coupled with their high biocompatibility, render swell-to-release ECS/SF composites as viable transdermal delivery devices. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Development of Chitosan Acetate Films for Transdermal Delivery of ...

    African Journals Online (AJOL)

    Purpose: To formulate and evaluate chitosan acetate films designed for transdermal delivery of propranolol hydrochloride. Methods: Chitosan acetate was chemically modified with acetaldehyde and the solution was prepared with 1 % acetic acid, in which was dissolved propranolol hydrochloride, was cast as films in Petri ...

  20. Simultaneous determination of three estrogens in human saliva without derivatization or liquid-liquid extraction for routine testing via miniaturized solid phase extraction with LC-MS/MS detection.

    Science.gov (United States)

    Li, Xiaoguang Sunny; Li, Shu; Kellermann, Gottfried

    2018-02-01

    Accurate quantitation of estrogens (i.e, estrone (E1), estradiol (E2) and estriol (E3)) is valuable for clinical assessment of human health and disease. Alterations in estrogen levels have been implicated in numerous pathological conditions. However, inadequacies in sensitivity and specificity, cumbersome sample preparation and invasive specimen collection hamper the usability of available methods for clinical applications. Herein, a simple, rapid, highly sensitive and specific LC-MS/MS method was developed and validated for the simultaneous determination of three estrogens in human saliva providing a non-invasive alternative to conventional blood samples. For the first time, a 96-well hydrophilic-lipophilic-balanced (HLB) microplate was employed for clean-up and enrichment of estrogens in a single extraction without the requirements of derivatization, evaporation, liquid-liquid extraction and online extraction. A rapid LC chromatographic separation with a turnaround time of 5.0min was achieved on a BEH C18 XP column. The use of 0.1mM ammonium fluoride (NH4F) as LC additive, and integration of summated and scheduled multiple reaction monitoring (MRM) transitions substantially improved the sensitivity to 1pg/mL, allowing the accurate quantitation of trace levels of three estrogens in one run. The assay was fully validated with good performance for extraction efficiency (67.0-85.6%), matrix effect (89.6-100.2%), linearity (from 1.0pg/mL up to 1000pg/mL), accuracy (98.9-112.4%) and precision (≤7.4%). Additionally, the assay was unaffected by 34 structurally-similar, potentially interfering substances tested at high clinical concentrations. The applicability of the assay was demonstrated by assessing the reference intervals of authentic saliva samples from healthy adult males, pre- and post-menopausal females. The easy sample preparation, fast LC and multi-analyte MS/MS detection utilizing noninvasive saliva as a specimen delivers a simple, practical, sensitive and

  1. An optmized protocol for simultaneous extraction of DNA and RNA from soils Protocolo otimizado para extração simultanea de DNA e RNA de solo

    Directory of Open Access Journals (Sweden)

    Rodrigo Costa

    2004-09-01

    Full Text Available In this work we report an optimized protocol for simultaneous extraction of DNA and RNA from soil matrices. Treatment of soil matrices with ethanol followed by bead-beating worked as a successful strategy to lyse the cells without considerable degradation of nucleic acids, resulting in DNA and RNA of good yield and integrity. The reverse transcribed RNA could be amplified with primers targeting a glutamine synthetase (glnA gene fragment. From both DNA and cDNA, 16S rDNA fragments were amplified and analyzed by Denaturing Gradient Gel Electrophoresis (DGGE. The method was applied to soil and rhizosphere (strawberry and oilseed rape samples. Two other protocols for the extraction of nucleic acids from soil were applied to the same set of samples in order to compare the methods in terms of efficiency and reproducibility. The DGGE profiles indicated no relevant differences between the patterns obtained. The method described here is suitable for rapid processing of many samples and therefore appropriate for ecological studies.Nesse trabalho descrevemos um protocolo otimizado para extração simultânea de DNA e RNA de solo. O tratamento das amostras de solo com etanol e posterior agitação com partículas foi uma estratégia bem sucedida para lise das células sem degradação significativa dos ácidos nucléicos, resultando em bom rendimento de DNA e RNA íntegros. O RNA transcrito pode ser amplificado com iniciadores com alvo no fragmento do gene da glutamina sintetase (glnA. Os fragmentos 16S rDNA, tanto do DNA como do cDNA, foram amplificados e analisados por DGGE. O método foi aplicado para amostras de solo e rizosfera (morango e canola. Dois outros protocolos para extração de ácidos nucléicos de solo foram aplicados para o mesmo lote de amostras, de forma a comparar os métodos quanto à eficiência e reprodutibilidade. Os perfis de DGGE mostraram não haver diferença relevante nos padrões obtidos. O método descrito é apropriado para

  2. Risk assessment of heavy metals in Vembanad Lake sediments (south-west coast of India), based on acid-volatile sulfide (AVS)-simultaneously extracted metal (SEM) approach.

    Science.gov (United States)

    Shyleshchandran, Mohanachandran Nair; Mohan, Mahesh; Ramasamy, Eswara Venkatesaperumal

    2017-12-23

    Contamination of estuarine system due to heavy metals is a severe issue in tropical countries, especially in India. For the evaluation of the risk due to heavy metals, the current study assessed spatial and temporal variation of acid-volatile sulfide (AVS), simultaneously extracted metal (SEM), and total metal concentration as toxicity indicator of aquatic sediments in Vembanad Lake System (VLS), India. Surface sediment samples collected from 12 locations from the northern portion of VLS for 4 years during different seasons. The results suggest, in post-monsoon season, 91% of the sampling locations possessed high bioavailability of metals and results in toxicity to aquatic biota. The average seasonal distribution of SEM during the period of observations was in the order post-monsoon > pre-monsoon > monsoon (1.76 ± 2.00 > 1.35 ± 0.60 > 0.80 ± 0.54 μmol/g). The concentration of individual metals on ∑SEM are in the order SEM Zn > SEM Cu> SEM Cd ≈ SEM Pb > SEM Hg. Considering annual ΣSEM/AVS ratio, 83% of the sites cross the critical value of 'One,' reveals that active sulfide phase of the sediment for fixing the metals is saturated. The molar ratio (differences between SEM and AVS) and its normalized organic carbon ratio reveals that in the post-monsoon season, about 42% of the sites are in the category of adverse effects are possible. The study suggests the toxicity and mobility of the metals largely depend on the available AVS, and the current situation may pose harm to benthic organisms.

  3. Statistical design-principal component analysis optimization of a multiple response procedure using cloud point extraction and simultaneous determination of metals by ICP OES.

    Science.gov (United States)

    Bezerra, Marcos A; Bruns, Roy E; Ferreira, Sergio L C

    2006-11-24

    A procedure has been developed for the simultaneous determination of traces amounts of Cd, Cr, Cu, Mn, Ni and Pb from saline oil-refinery effluents and digested vegetable samples using inductively coupled plasma optical emission spectrometry (ICP OES). The procedure is based on cloud point extraction (CPE) of these metals as 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) complexes into a micellar phase of octylphenoxypolyethoxyethanol (Triton X-114). Optimization of the procedure was performed by response surface methodology (RSM) using a Doehlert design. Principal components (PC) were used to simplify the multiple response analysis. A response surface for the first PC score is useful in determining the optimum conditions for the Cd, Cr, Cu, Mn and Pb determinations whereas the second PC is highly correlated with the Ni response. Improvement factors of 22, 36, 46, 25, 65 and 39, along with limits of detection (3sigma(B)) of 0.081, 0.79, 0.38, 0.83, 0.28 and 0.69 microg L(-1), and precision expressed as relative standard deviation (%R.S.D., n=8, 20.0 microg L(-1)) of 1.5, 2.2, 3.5, 2.6, 2.5 and 2.5 were achieved for Cd, Cr, Cu, Mn, Ni and Pb, respectively. The accuracy was evaluated by spike tests in oil-refinery effluent samples and analysis of a vegetable certified reference material (NIST 1571, orchard leaves). Results found were in agreement with certified values.

  4. Development and optimization of a novel sample preparation method cored on functionalized nanofibers mat-solid-phase extraction for the simultaneous efficient extraction of illegal anionic and cationic dyes in foods.

    Science.gov (United States)

    Qi, Feifei; Jian, Ningge; Qian, Liangliang; Cao, Weixin; Xu, Qian; Li, Jian

    2017-09-01

    A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg-1, and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.

  5. Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in seawater samples by membrane-assisted solvent extraction combined with gas chromatography-electron capture detector and gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Shi, Xizhi; Tang, Zigang; Sun, Aili; Zhou, Lei; Zhao, Jian; Li, Dexiang; Chen, Jiong; Pan, Daodong

    2014-12-01

    A highly efficient and environment-friendly membrane-assisted solvent extraction system combined with gas chromatography-electron capture detector was applied in the simultaneous determination of 17 polychlorinated biphenyls and organochlorine pesticides in seawater samples. Variables affecting extraction efficiency, including extraction solvent used, stirring rate, extraction time, and temperature, were optimized extensively. Under optimal extraction conditions, recoveries between 76.9% and 104.6% in seawater samples were achieved, and relative standard deviation values below 10% were obtained. The limit of detection (signal-to-noise ratio=3) and limit of quantification (signal-to-noise ratio=10) of 17 polychlorinated biphenyls and organochlorine pesticides in seawater ranged from 0.14ngL(-1) to 0.36ngL(-1) and 0.46ngL(-1) to 1.19ngL(-1), respectively. Matrix effects on extraction efficiency were evaluated by comparing with the results obtained using tap water. The extraction effect of developed membrane-assisted solvent extraction method was further demonstrated by gas chromatography-tandem mass spectrometry which can provide structural information of the analytes for more accurate identification, and results identical to those produced by gas chromatography-electron capture detector were obtained. These findings demonstrate the applicability of the developed membrane-assisted solvent extraction determination method for coupling to gas chromatography-electron capture detector or tandem mass spectrometry for determining polychlorinated biphenyls and organochlorine pesticides in seawater samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. All-in-one solid-phase microextraction: Development of a selective solid-phase microextraction fiber assembly for the simultaneous and efficient extraction of analytes with different polarities.

    Science.gov (United States)

    Gharari, Hossein; Farjaminezhad, Manoochehr; Marefat, Abdolrahim; Fakhari, Ali Reza

    2016-05-01

    In the present work, for the first time, an all-in-one solid-phase microextraction technique was developed for the simultaneous and efficient extraction of analytes within a vast polarity range. A novel fiber assembly composed of two different steel components each coated with different coatings (polydimethylsiloxane and polyethylene glycol) in terms of polarity by sol-gel technology was employed for the extraction of model compounds of different polarity in a single run followed by gas chromatography with mass spectrometry. Effective parameters in the extraction step and gas chromatography with mass spectrometry analysis were optimized for all model compounds. The detection limits of the developed method for model compounds were below 0.2 ng/L. The repeatability and reproducibility of the proposed method, explained by relative standard deviation, varied between 7.22 and 9.15% and between 7.95 and 14.90 (n = 5), respectively. Results showed that, under random conditions, compared to separate extractions performed by two other differently end-coated components that had not been assembled as the final dual fiber, as two individual fibers; simultaneous, efficient and relatively selective extraction of all model compounds was obtained in a single run by the proposed all-in-one technique. Finally, the optimized procedure was applied to extraction and determination of the model compounds in spiked water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Simultaneous determination of seven anthraquinones in rat plasma by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry and pharmacokinetic study after oral administration of Semen Cassiae extract.

    Science.gov (United States)

    Yang, Chunjuan; Wang, Shuhong; Guo, Xiaowei; Sun, Jiahui; Liu, Lu; Wu, Lijun

    2015-07-01

    Semen Cassiae, called Juemingzi in China, is the seed of the annual Cassia obtusifolia L., of the leguminosae family. It has been used as healthy drinks to alleviate constipation and improve eyesight for many years in China. A simple sensitive UHPLC-MS/MS method has been developed and validated for the simultaneous determination and pharmacokinetic study of chrysophanol, emodin, aloe-emodin, rhein, physcion, obtusifolin and aurantio-obtusin in rat plasma. Chromatographic separation was accomplished on a C18 column with a 5min gradient elution. A tandem mass spectrometric detection was conducted using multiple reaction monitoring (MRM) via an electrospray ionization (ESI) source and operating in the negative ionization mode. The samples were prepared by LLE with ethyl acetate after being spiked with an internal standard (butylparaben). The current UHPLC-MS/MS assay was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery and stability. The method was linear for all analytes over investigated range with all correlation coefficients greater than 0.9900. The lower limit of quantification (LLOQ) of each analyte was lower than 5ng/mL. Intra-day and inter-day precisions were less than 14.99%. The relative errors of accuracies were in the range of -14.60% to 5.11%. The mean recoveries and matrix effects of anthraquinones were higher than 65.54% and 93.26%, respectively. After oral administration 1.25g/kg of Semen Cassiae extract, the maximum plasma concentration (Cmax) was 1189.25±333.40ng/mL for chrysophanol, 38.48±3.15ng/mL for emodin, 79.20±34.76ng/mL for aloe-emodin, 152.70±23.91ng/mL for rhein, 461.85±266.77ng/mL for physcion, 243.59±22.71ng/mL for obtusifolin and 1950.44±638.86ng/mL for aurantio-obtusin, respectively. The time to reach the maximum plasma concentration (Tmax) was 0.333±0.071h for chrysophanol, 0.333±0.059h for emodin, 0.333±0.009h for aloe-emodin, 0.333±0.09h for rhein, 0.167±0.002h for physcion, 0.5

  8. Hydrosoluble, UV-crosslinkable and injectable chitosan for patterned cell-laden microgel and rapid transdermal curing hydrogel in vivo.

    Science.gov (United States)

    Li, Baoqiang; Wang, Lei; Xu, Feng; Gang, Xiaomin; Demirci, Utkan; Wei, Daqing; Li, Ying; Feng, Yujie; Jia, Dechang; Zhou, Yu

    2015-08-01

    Natural and biodegradable chitosan with unique amino groups has found widespread applications in tissue engineering and drug delivery. However, its applications have been limited by the poor solubility of native chitosan in neutral pH solution, which subsequently fails to achieve cell-laden hydrogel at physiological pH. To address this, we incorporated UV crosslinking ability in chitosan, allowing fabrication of patterned cell-laden and rapid transdermal curing hydrogel in vivo. The hydrosoluble, UV crosslinkable and injectable N-methacryloyl chitosan (N-MAC) was synthesized via single-step chemoselective N-acylation reaction, which simultaneously endowed chitosan with well solubility in neutral pH solution, UV crosslinkable ability and injectability. The solubility of N-MAC in neutral pH solution increased 2.21-fold with substitution degree increasing from 10.9% to 28.4%. The N-MAC allowed fabrication of cell-laden microgels with on-demand patterns via photolithography, and the cell viability in N-MAC hydrogel maintained 96.3 ± 1.3% N-MAC allowed rapid transdermal curing hydrogel in vivo within 60s through minimally invasive clinical surgery. Histological analysis revealed that low-dose UV irradiation hardly induced skin injury and acute inflammatory response disappeared after 7 days. N-MAC would allow rapid, robust and cost-effective fabrication of patterned cell-laden polysaccharide microgels with unique amino groups serving as building blocks for tissue engineering and rapid transdermal curing hydrogel in vivo for localized and sustained protein delivery. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  9. Transdermal and intradermal delivery of therapeutic agents: application of physical technologies

    National Research Council Canada - National Science Library

    Banga, Ajay K

    2011-01-01

    .... Commercialization of transdermal drug delivery requires technology from many disciplines beyond pharmaceutical sciences, such as polymer chemistry, adhesion sciences, mass transport, web film coating...

  10. Liquid-liquid extraction combined with high performance liquid chromatography-diode array-ultra-violet for simultaneous determination of antineoplastic drugs in plasma

    Directory of Open Access Journals (Sweden)

    Ananda Lima Sanson

    2011-06-01

    Full Text Available A liquid-liquid extraction (LLE combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v, which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.Um método de extração líquido-líquido (ELL combinado com cromatografia líquida de alta eficiência-detector de arranjo de diodos foi desenvolvido para análise simultânea de quatro fármacos antineoplásicos quimicamente e estruturalmente diferentes (ciclofosfamida, doxorrubicina, fluoruracila e ifosfamida. O estudo foi realizado sob condições isocráticas, com coluna C18 (5µm, 250 x 4.6 mm e fase móvel constituída por água pH 4.0-acetonitrila-metanol (68:19:13, v/v/v, que permitiu separação satisfatória dos analitos de interesse. A ELL, com acetato de etila, foi utilizada para limpeza da amostra, com recuperação variando de 60 a 98%. As faixas foram lineares de 0,5 a 100 µg mL-1 para doxorrubicina e 1 a 100 µg mL-1 para os outros compostos. O desvio padrão relativo variou de 5,5 a 17,7%. Este método é uma alternativa rápida e simples que pode ser usado, simultaneamente, para a determinação dos

  11. Use of pressurized liquid extraction for the simultaneous analysis of 28 polar and 94 non-polar pesticides in agricultural soils by GC/QqQ-MS/MS and UPLC/QqQ-MS/MS.

    Science.gov (United States)

    Martínez Vidal, José Luis; Padilla Sánchez, Juan Antonio; Plaza-Bolaños, Patricia; Garrido Frenich, Antonia; Romero-González, Roberto

    2010-01-01

    Due to the wide range of pesticides that can be used in agriculture, the development of fast multiresidue methods that simultaneously determine polar and non-polar pesticides is greatly demanded. This study shows the development and validation of a multiresidue method for the analysis of 98 non-polar pesticides and 28 polar pesticides in soil. A simultaneous extraction step by pressurized liquid extraction was utilized. The optimum results were obtained using ethyl acetate-methanol (3:1, v/v) with 2 min of preheat time and 85 degrees C as the extraction temperature. The final determination of non-polar pesticides was performed by GC, whereas polar pesticides were determined by ultra-performance liquid chromatography (UPLC). Both GC and UPLC were coupled to triple-quadrupole analyzers operating in tandem MS. The optimized extraction procedure was validated. The average extraction recoveries were in the range 72-108% (10 microg/kg) and 71-106% (50 microg/kg), with RSD values < or = 26%. The matrix effect was also evaluated, and matrix-matched standard calibration was finally applied for quantification. The suitability of the method was also checked by the analysis of a certified reference material. Furthermore, 26 real soil samples were analyzed by the proposed methods in order to assess their applicability. Several pesticides (e.g., bifenthrin, triadimefon, or endosulfan) were found in the samples.

  12. Simultaneous Analysis of 3-MCPD and 1,3-DCP in Asian Style Sauces Using QuEChERS Extraction and Gas Chromatography–Triple Quadrupole Mass Spectrometry

    Science.gov (United States)

    Genualdi, Susan; Nyman, Patricia; DeJager, Lowri

    2017-01-01

    Acid hydrolyzed vegetable protein (aHVP) is used for flavoring a wide variety of foods and also in the production of nonfermented soy sauce. During the production of aHVP, chloropropanols including 3-monochloropropane-1,2-diol (3-MCPD) and 1,3 dichloropropane-2-ol (1,3-DCP) can be formed through the reaction of the hydrochloric acid catalyst and residual fat and the reaction of 3-MCPD with acetic acid, respectively. 3-MCPD is a carcinogen, and 1,3-DCP has been classified as a genotoxic carcinogen. The European Union (EU) has set a maximum concentration of 0.02 mg/kg of 3-MCPD in aHVP, and the Food and Drug Administration (FDA) set a guidance limit of 1 mg/kg of 3-MCPD in aHVP. 1,3-DCP is not an approved food additive, and the Joint FAO/WHO Expert Committee on Food Additives (JEFCA) has set a limit at 0.005 mg/kg, which is close to the estimated method detection limit. Currently there are few analytical methods for the simultaneous determination of 3-MCPD and 1,3-DCP without derivatization due to differences in their physical chemical properties and reactivity. A new method was developed using QuEChERS (quick, easy, cheap, effective, rugged, and safe) with direct analysis of the extract without derivatization using gas chromatography–triple quadrupole mass spectrometry (GC-QQQ). Additionally, a market sampling of 60 soy sauce samples was performed in 2015 to determine if concentrations have changed since the FDA limit was set in 2008. The sampling results were compared between the new QuEChERS method and a method using phenylboronic acid (PBA) as a derivatizing agent for 3-MCPD analysis. The concentrations of 3-MCPD detected in soy sauce samples collected in 2015 (

  13. NMR characterisation and transdermal drug delivery potential of microemulsion systems

    DEFF Research Database (Denmark)

    Kreilgaard, Mads; Pedersen, E J; Jaroszewski, J W

    2000-01-01

    The purpose of this study was to investigate the influence of structure and composition of microemulsions (Labrasol/Plurol Isostearique/isostearylic isostearate/water) on their transdermal delivery potential of a lipophilic (lidocaine) and a hydrophilic model drug (prilocaine hydrochloride......), and to compare the drug delivery potential of microemulsions to conventional vehicles. Self-diffusion coefficients determined by pulsed-gradient spin-echo NMR spectroscopy and T(1) relaxation times were used to characterise the microemulsions. Transdermal flux of lidocaine and prilocaine hydrochloride through...... rat skin was determined in vitro using Franz-type diffusion cells. The formulation constituents enabled a broad variety of microemulsion compositions, which ranged from water-continuous to oil-continuous aggregates over possible bicontinuous structures, with excellent solubility properties for both...

  14. Inkjet printing of insulin microneedles for transdermal delivery.

    Science.gov (United States)

    Ross, Steven; Scoutaris, Nicolaos; Lamprou, Dimitrios; Mallinson, David; Douroumis, Dennis

    2015-08-01

    Inkjet printing technology was used to apply insulin polymeric layers on metal microneedles for transdermal delivery. A range of various polymers such as gelatin (GLN), polyvinyl caprolactame-polyvinyl acetate-polyethylene glycol (SOL), poly(2-ethyl-2-oxazoline) (POX) and trehalose (THL) were assessed for their capacity to form thin uniform and homogeneous layers that preserve insulin intact. Atomic force microscopy (AFM) showed homogeneous insulin-polymer layers without any phase separation while SOL demonstrated the best performance. Circular discroism (CD) analysis of rehydrated films showed that insulin's alpha helices and β-sheet were well preserved for THL and SOL. In contrast, GLN and POX insulin layers revealed small band shifts indicating possible conformational changes. Insulin release in Franz diffusion cells from MNs inserted into porcine skin showed rapid release rates for POX and GLN within the first 20 min. Inkjet printing was proved an effective approach for transdermal delivery of insulin in solid state.

  15. Current advances in transdermal delivery of drugs for Alzheimer's disease.

    Science.gov (United States)

    Nguyen, Thuy Trang; Giau, Vo Van; Vo, Tuong Kha

    2017-01-01

    Alzheimer's disease (AD) is a common, progressive, fatal neurodegenerative disorder, which will play an increasingly important role both socially and financially in the aging populations. Treatments for AD show modest improvements in cognition and global functioning among patients. Furthermore, the oral administration of treating AD has had some drawbacks that decrease the medication adherence and efficacy of the therapy. Transdermal drugs are proposed as an alternative remedy to overcome the disadvantages of current pharmaceutical dosage options for this chronic disorder. They could have different strengths, such as offering a stable diffusion of active substance, avoiding the first pass metabolism, and reducing system adverse reactions. This article reviews the technical principles, novel techniques of transdermal delivery drug, and prospects for future development for the management of cognitive and behavioral dysfunctions in AD patients.

  16. Laser microporation: A promising field in transdermal drug delivery

    OpenAIRE

    Mozhdeh Sepaskhah

    2017-01-01

    Topical therapy is an expanding field not only in dermatology but also in other fields of medicine. An expanding list of systemic medications have been applied topically in several dermatologic conditions. Drugs applied topically have the advantage of fewer side effects, and bypassing the first-pass effect. Also, painless drug delivery which is especially encouraging in children, makes transdermal drug delivery even more appealing.

  17. Laser microporation: A promising field in transdermal drug delivery

    Directory of Open Access Journals (Sweden)

    Mozhdeh Sepaskhah

    2017-03-01

    Full Text Available Topical therapy is an expanding field not only in dermatology but also in other fields of medicine. An expanding list of systemic medications have been applied topically in several dermatologic conditions. Drugs applied topically have the advantage of fewer side effects, and bypassing the first-pass effect. Also, painless drug delivery which is especially encouraging in children, makes transdermal drug delivery even more appealing.

  18. MICRONEEDLES IN TRANSDERMAL DRUG DELIVERY: AN UNIQUE PAINLESS OPTION

    OpenAIRE

    Tiwari Raj Kumar; Bagga Manish; Chanda Silpi

    2011-01-01

    The outermost layer of skin, the stratum corneum, has developed unnerving physical and immunological barrier properties that prevent infiltration of noxious chemicals and pathogens. Consequently, transdermal delivery of medicaments is currently restricted to a limited number of low molecular weight drugs to enter the skin at successful therapeutic rates. As a result, there has been significant recent interest in providing strategies that disrupt or dodge the principal physical barrier, the st...

  19. Design and evaluation of transdermal patches of timolol maleate.

    Science.gov (United States)

    Hiremath, S P; Jujjuri, J; Jamakandi, V J

    2017-10-02

    Continuous intravenous infusion of controlled drug delivery has certain risks. This could be diligently duplicated devoid of its hassles by using the skin as the port of drug entry. Transdermal drug delivery system is the main route with discrete, self-contained dosage forms when placed on the skin transports the medicament through the skin into the systemic circulation in a well-controlled manner. The rationale of the current work was to formulate and evaluate a transdermal patch of an antihypertensive drug by using different grades of polymers with a view to circumvent the hepatic first pass metabolism and also to escalate its bioavailability. Solvent-casting method was used to prepare transdermal patches of timolol maleate using Eudragit RL100, Eudragit RS100, ethyl cellulose as polymers, and dibutyl phthalate as the plasticizer. The formulated patches were evaluated for its physiochemical parameters such as folding endurance, percentage moisture content, thickness, and water vapour transmission. The formulated patches were subjected to in-vitro permeation studies by using a Franz diffusion cell with a dialysis sac. The optimized formulation chosen based on physiochemical characteristics and in-vitro studies was subjected to in-vivo studies on methyl prednisolone acetate-induced hypertensive rats. The data from release kinetics disclosed that the Korsmayer-Peppas could be the best fitting model. The results obtained from in-vitro studies disclosed that formulation with high proportion of Eudragit grade RL100 in acetone solvent system exhibited better drug release compared to rest of the formulations. The output obtained from in-vivo studies performed on rats revealed that, the optimized formulation showed decrease in blood pressure from 158.53 ± 0.39 to 128.91 ± 0.50 mmHg. Our study concludes that timolol maleate patch could be formulated into a matrix-type transdermal patch for the management of hypertension. Copyright© Bentham Science Publishers; For any

  20. Synthesis and transdermal properties of acetylsalicylic acid derivates / Minja Gerber

    OpenAIRE

    Gerber, Minja

    2003-01-01

    The skin is an amazing elastic and relatively impermeable barrier that provides protective, perceptive and communication functions to the body. The stratum corneum is widely accepted as the barrier of the skin - limiting the transport of molecules into and across the skin. It is evident that the transdermal permeation of drugs depend on a number of factors of which the physicochemical properties play the most prevalent role. The potential of using intact skin as the site of adm...

  1. Current advances in transdermal delivery of drugs for Alzheimer's disease

    OpenAIRE

    Thuy Trang Nguyen; Vo Van Giau; Tuong Kha Vo

    2017-01-01

    Alzheimer's disease (AD) is a common, progressive, fatal neurodegenerative disorder, which will play an increasingly important role both socially and financially in the aging populations. Treatments for AD show modest improvements in cognition and global functioning among patients. Furthermore, the oral administration of treating AD has had some drawbacks that decrease the medication adherence and efficacy of the therapy. Transdermal drugs are proposed as an alternative remedy to overcome the...

  2. Evaluation of mesotherapy as a transdermal drug delivery tool.

    Science.gov (United States)

    Kim, S; Kye, J; Lee, M; Park, B

    2016-05-01

    There has been no research about the exact mechanism of transdermal drug delivery during mesotherapy. We aimed to evaluate whether the commercial mesogun can be an appropriate technique for a transdermal drug delivery. We injected blue ink into the polyurethane foam or pig skin with three types of mesotherapy using a commercial mesogun, or local made intradermal injector, or a manual injection of syringe. To assess the internal pressure of the cylinder and drug delivery time, we designed the evaluation setup using a needle tip pressure transducer. All types of injectors induced adequate penetration of blue ink into the polyurethane foam without backflow. In the pig skin, blue ink leaked out rapidly with the backward movement of the needle in the commercial mesogun in contrast to the local made injector or the manual injection of syringe. When the time for backward movement of the syringe approaches 1000 ms, the cylinder pressure of the syringe is saturated at around 25 mmHg which can be translated into the dermal pressure of the pig skin. There should be sufficient time between the insertion and withdrawal of the needle of injector for the adequate transdermal drug delivery and it must be considered for mesotherapy. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  3. Microneedles for enhanced transdermal and intraocular drug delivery.

    Science.gov (United States)

    Moffatt, Kurtis; Wang, Yujing; Raj Singh, Thakur Raghu; Donnelly, Ryan F

    2017-10-01

    Microneedle mediated delivery based research has garnered great interest in recent years. In the past, the initial focus was delivery of macromolecules of biological origin, however the field has now broadened its scope to include transdermal delivery of conventional low molecular weight drug molecules. Great success has been demonstrated utilising this approach, particularly in the field of vaccine delivery. Current technological advances have permitted an enhancement in design formulation, allowing delivery of therapeutic doses of small molecule drugs and biomolecules, aided by larger patch sizes and scalable manufacture. In addition, it has been recently shown that microneedles are beneficial in localisation of drug delivery systems within targeted ocular tissues. Microneedles have the capacity to modify the means in which therapeutics and formulations are delivered to the eye. However, further research is still required due to potential drawbacks and challenges. Indeed, no true microneedle-based transdermal or ocular drug delivery system has yet been marketed. Some concerns have been raised regarding regulatory issues and manufacturing processes of such systems, and those in the field are now actively working to address them. Microneedle-based transdermal and ocular drug delivery systems have the potential to greatly impact not only patient benefits, but also industry, and through diligence, innovation and collaboration, their true potential will begin to be realised within the next 3-5 years. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Infrared free electron laser enhanced transdermal drug delivery

    Science.gov (United States)

    Awazu, Kunio; Uchizono, Takeyuki; Suzuki, Sachiko; Yoshikawa, Kazushi

    2005-08-01

    It is necessary to control enhancement of transdermal drug delivery with non-invasive. The present study was investigated to assess the effectivity of enhancing the drug delivery by irradiating 6-μm region mid infrared free electron laser (MIR-FEL). The enhancement of transdermal drug (lidocaine) delivery of the samples (hairless mouse skin) irradiated with lasers was examined for flux (μg/cm2/h) and total penetration amount (μg/cm2) of lidocaine by High performance Liquid Chromatography (HPLC). The flux and total amount penatration date was enhanced 200-300 fold faster than the control date by the laser irradiation. FEL irradiating had the stratum corneum, and had the less thermal damage in epidermis. The effect of 6-μm region MIR-FEL has the enhancement of transdermal drug delivery without removing the stratum corneum because it has the less thermal damage. It leads to enhancement drug delivery system with non-invasive laser treatment.

  5. Noninvasive measurement of transdermal drug delivery by impedance spectroscopy.

    Science.gov (United States)

    Arpaia, Pasquale; Cesaro, Umberto; Moccaldi, Nicola

    2017-03-24

    The effectiveness in transdermal delivery of skin permeation strategies (e.g., chemical enhancers, vesicular carrier systems, sonophoresis, iontophoresis, and electroporation) is poorly investigated outside of laboratory. In therapeutic application, the lack of recognized techniques for measuring the actually-released drug affects the scientific concept itself of dosage for topically- and transdermally-delivered drugs. Here we prove the suitability of impedance measurement for assessing the amount of drug penetrated into the skin after transdermal delivery. In particular, the measured amount of drug depends linearly on the impedance magnitude variation normalized to the pre-treated value. Three experimental campaigns, based on the electrical analysis of the biological tissue behavior due to the drug delivery, are reported: (i) laboratory emulation on eggplants, (ii) ex-vivo tests on pig ears, and finally (iii) in-vivo tests on human volunteers. Results point out that the amount of delivered drug can be assessed by reasonable metrological performance through a unique measurement of the impedance magnitude at one single frequency. In particular, in-vivo results point out sensitivity of 23 ml-1, repeatability of 0.3%, non-linearity of 3.3%, and accuracy of 5.7%. Finally, the measurement resolution of 0.20 ml is compatible with clinical administration standards.

  6. Chitosan microneedle patches for sustained transdermal delivery of macromolecules.

    Science.gov (United States)

    Chen, Mei-Chin; Ling, Ming-Hung; Lai, Kuan-Ying; Pramudityo, Esar

    2012-12-10

    This paper introduces a chitosan microneedle patch for efficient and sustained transdermal delivery of hydrophilic macromolecules. Chitosan microneedles have sufficient mechanical strength to be inserted in vitro into porcine skin at approximately 250 μm in depth and in vivo into rat skin at approximately 200 μm in depth. Bovine serum albumin (BSA, MW=66.5 kDa) was used as a model protein to explore the potential use of chitosan microneedles as a transdermal delivery device for protein drugs. In vitro drug release showed that chitosan microneedles can provide a sustained release of BSA for at least 8 days (approximately 95% of drugs released in 8 days). When the Alexa Fluor 488-labeled BSA (Alexa 488-BSA)-loaded microneedles were applied to the rat skin in vivo, confocal microscopic images showed that BSA can gradually diffuse from the puncture sites to the dermal layer and the fluorescence of Alexa 488-BSA can be observed at the depth of 300 μm. In addition, encapsulation of BSA within the microneedle matrix did not alter the secondary structure of BSA, indicating that the gentle nature of the fabrication process allowed for encapsulation of fragile biomolecules. These results suggested that the developed chitosan microneedles may serve as a promising device for transdermal delivery of macromolecules in a sustained manner.

  7. Statistically optimised ethosomes for transdermal delivery of tolterodine tartrate.

    Science.gov (United States)

    Prasanthi, D; Lakshmi, P K

    2013-11-01

    The aim of the current investigation is to optimize ethosomes statistically for enhancing transdermal potential of Tolterodine Tartrate (TT). Ethosomes bearing TT were prepared by cold method and characterized for various parameters like vesicle size, vesicle shape, surface morphology and % drug entrapment. Microscopic examinations suggest ethosomes as spherical unilamellar vesicles with a smooth surface. Optimized ethosomal vesicles were of 890±2.67nm size and showed 79.83±3.18% drug entrapment. Ex-vivo permeation studies across rat skin resulted in increased flux of 4.69±0.24μg/cm(2)/hr and decreased lag time of 0.13±0.05 hr when compared with drug solution (0.546±0.05μg/cm(2)/hr, 3±0.2 hr).This shows enhancement of transdermal delivery by 8.82 times. Anatomical changes in skin samples due to vesicle-skin interaction were observed on histological examination. Optimized formulation on storage at 4°C for 120 days showed insignificant growth in vesicular size revealing low aggregation of vesicles. The results collectively suggest ethosomes as carriers for accentuated transdermal delivery of TT.

  8. Microneedles array with biodegradable tips for transdermal drug delivery

    Science.gov (United States)

    Iliescu, Ciprian; Chen, Bangtao; Wei, Jiashen; Tay, Francis E. H.

    2008-12-01

    The paper presented an enhancement solution for transdermal drug delivery using microneedles array with biodegradable tips. The microneedles array was fabricated by using deep reactive ion etching (DRIE) and the biodegradable tips were made to be porous by electrochemical etching process. The porous silicon microneedle tips can greatly enhance the transdermal drug delivery in a minimum invasion, painless, and convenient manner, at the same time; they are breakable and biodegradable. Basically, the main problem of the silicon microneedles consists of broken microneedles tips during the insertion. The solution proposed is to fabricate the microneedle tip from a biodegradable material - porous silicon. The silicon microneedles are fabricated using DRIE notching effect of reflected charges on mask. The process overcomes the difficulty in the undercut control of the tips during the classical isotropic silicon etching process. When the silicon tips were formed, the porous tips were then generated using a classical electrochemical anodization process in MeCN/HF/H2O solution. The paper presents the experimental results of in vitro release of calcein and BSA with animal skins using a microneedle array with biodegradable tips. Compared to the transdermal drug delivery without any enhancer, the microneedle array had presented significant enhancement of drug release.

  9. Simultaneous determination of polar and apolar compounds in environmental samples by a polyaniline/hydroxyl multi-walled carbon nanotubes composite-coated stir bar sorptive extraction coupled with high performance liquid chromatography.

    Science.gov (United States)

    Hu, Cong; He, Man; Chen, Beibei; Hu, Bin

    2015-05-15

    Developing novel coatings for stir bar sorptive extraction (SBSE) is essential for extending the application of SBSE. Herein, a polyaniline/hydroxyl multi-walled carbon nanotubes (PANi/MWCNTs-OH) composite-coated stir bar was prepared via the adhesion technique for the simultaneous extraction of polar and apolar compounds, and a novel method of PANi/MWCNTs-OH-coated SBSE coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was proposed. To test the extraction performance of PANi/MWCNTs-OH-coated stir bar, phenols, non-steroidal anti-inflammatory drugs, and polychlorinated biphenyls were selected as representatives for polar, semi-polar and apolar compounds, respectively. High enrichment factors (EFs) ranged from 20.4 to 60.4-fold (theoretical EF, 100-fold) for target analytes were achieved, indicating that the proposed method is applicable in simultaneous analysis of the compounds with different polarities. The prepared PANi/MWCNTs-OH-coated stir bar has a good preparation reproducibility and can be reused for 20 times. The limits of detection (LODs, S/N=3) were found to be in the range of 0.09-0.81μg/L. To validate the applicability, the proposed method was successfully applied to the analysis of eight target analytes in Yangtze River water after filtration and in the extract from sediment samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Development and Evaluation of Naproxen Sodium Gel Using Piper cubeba for Enhanced Transdermal Drug Delivery and Therapeutic Facilitation.

    Science.gov (United States)

    Patwardhan, Sunetra; Patil, Manohar; Sockalingam, Anbazhagan

    2017-01-01

    The absorption of drug through skin avoids many side effects of oral route like gastric irritation, nausea, systemic toxicity etc and thus improves patient compliance. Naproxen sodium (NPRS) is one of the potent NSAID agents. The present study was aimed to develop and evaluate the gel formulation containing NPRS for transdermal drug delivery reducing the side effects and improving patient compliance. The patents on topical delivery of NSAIDS (US 9012402 B1, US 9072659 B2, US 20150258196 A1) and patents indicating use of herbal penetration enhancers (US 20100273746A1, WO 2005009510 A2, US 6004969 A) helped in selecting the drug, excipients. Current protocol employs various extracts of Piper cubeba fruit to evaluate its role in absorption of NPRS. Various batches containing 1% NPRS and varying concentrations of synthetic permeation enhancers or the extracts were formulated in carbopol gel. Gel was evaluated for parameters like organoleptic parameters, pH, viscosity and spreadability. An ex-vivo percutaneous absorption of NPRS from gel was investigated and compared with best performing synthetic enhancer, transcutol P (TP). The batch containing 2% n-hexane extract (NHE) of Piper cubeba showed higher permeation than TP and Chloroform (CE), Methanolic (ME) and aqueous (AE) extracts as well. It showed improved % cumulative release (85.09%) and flux (278.61μg/cm2.h), as compared to TP and other extracts. Histopathology indicated the formulation safer as compared to that with synthetic enhancer. It suggests P. cubeba as effective and safer tool for transdermal delivery and acts as therapeutic facilitator for naproxen. GC-MS analysis indicates lignans & terpenes in NHE to which this permeation enhancement activity may be attributed. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  11. Transdermal administration of radiolabelled [14C]rotigotine by a patch formulation: A mass balance trial

    NARCIS (Netherlands)

    Cawello, W.; Wolff, H.M.; Meuling, W.J.A.; Horstmann, R.; Braun, M.

    2007-01-01

    Background and objective: The dopamine agonist rotigotine has been formulated in a silicone-based transdermal system for once-daily administration. The objective of the present study was to characterise the mass balance of rotigotine in humans after administration of a single transdermal patch

  12. Transdermal permeation of Zanthoxylum bungeanum essential oil on TCM components with different lipophilicity

    Directory of Open Access Journals (Sweden)

    Yi Lan

    2016-07-01

    Conclusion: Z. bungeanum oil facilitated transdermal permeation of drugs with different lipophilicity, including the extremely hydrophilic and lipophilic drugs, whereas it exhibited greater enhancement activity for strongly hydrophilic drugs. The mechanisms of transdermal permeation enhancement by the oil could be explained with SC/vehicle partition coefficient, saturation solubility, and the interactions with SC lipids.

  13. Effect of transdermal hormone therapy on platelet haemostasis in menopausal women

    Directory of Open Access Journals (Sweden)

    Grzegorz Stachowiak

    2015-02-01

    1 Transdermal HT in the form of combined, estrogen-progestogen patches favourably modifies platelets haemostasis, reversing the adverse effects that occur after menopause. 2 The use of low ASA doses as a thromboprophylaxis in short-term transdermal HT is not necessary.

  14. Multicriteria optimisation of a simultaneous supercritical fluid extraction and clean-up procedure for the determination of persistent organohalogenated pollutants in aquaculture samples.

    Science.gov (United States)

    Rodil, R; Carro, A M; Lorenzo, R A; Cela, R

    2007-04-01

    A useful tool based on a single-step extraction and clean-up procedure for the determination of 15 organohalogenated pollutants (including brominated flame retardants) in aquaculture samples, using aluminium oxide basic and acidic silica gel in the supercritical extraction cell followed by gas chromatography with electron capture detection or mass spectrometry has been developed. This effective clean-up step ensures a minimum of chromatographic difficulties related to complex matrix components such as aquaculture feed. The extraction procedure has been screened by a fractional factorial design for the preliminary statistically significant parameters. The factors selected were extraction temperature, pressure, static extraction time, dynamic extraction time and carbon dioxide flow rate. The Doehlert design, followed by a multicriteria decision-making strategy, was then performed in order to determine the optimum conditions for the two most significant factors: pressure (165 bar) and dynamic extraction time (27 min). Under optimal conditions, the procedure developed with GC-MS/MS provides an excellent linearity, detection (0.01-0.2 ng g(-1)) and quantification limits (0.05-0.8 ng g(-1)) for most of the analytes investigated. The feasibility of the proposed supercritical fluid extraction method was validated by analysing two reference materials and fish feed and shellfish samples with satisfactory results.

  15. Simultaneous Microwave Extraction and Separation of Volatile and Non-Volatile Organic Compounds of Boldo Leaves. From Lab to Industrial Scale

    Directory of Open Access Journals (Sweden)

    Loïc Petigny

    2014-04-01

    Full Text Available Microwave extraction and separation has been used to increase the concentration of the extract compared to the conventional method with the same solid/liquid ratio, reducing extraction time and separate at the same time Volatile Organic Compounds (VOC from non-Volatile Organic Compounds (NVOC of boldo leaves. As preliminary study, a response surface method has been used to optimize the extraction of soluble material and the separation of VOC from the plant in laboratory scale. The results from the statistical analysis revealed that the optimized conditions were: microwave power 200 W, extraction time 56 min and solid liquid ratio of 7.5% of plants in water. Lab scale optimized microwave method is compared to conventional distillation, and requires a power/mass ratio of 0.4 W/g of water engaged. This power/mass ratio is kept in order to upscale from lab to pilot plant.

  16. Effect of the type and level of hydration of alcoholic solvents on the simultaneous extraction of oil and chlorogenic acids from sunflower seed press cake.

    Science.gov (United States)

    Scharlack, Nayara K; Aracava, Keila K; Rodrigues, Christianne Ec

    2017-10-01

    The present study aimed to evaluate the replacement of hexane by alcoholic solvents in oil extraction from sunflower seed press cake. The use of ethanol and isopropanol has important advantages, including low toxicity and good operational safety. Thus, in the present study, solid-liquid extractions were performed in a single stage from 60 to 90 °C and in consecutive extractions in three stages at 90 °C. Solvent hydration negatively affected the extraction of oil but favored the extraction of chlorogenic acids (CAs), especially when ethanol was used. Regarding oxidative stability, the oils extracted using ethanol presented long induction times, which could be related to the high levels of not only CAs and tocopherols, but also phospholipids. Alcoholic solvents can be used for extraction to produce sunflower seed oil containing minor compounds that give it greater oxidative stability. In addition, the results obtained using hydrous ethanol showed that this solvent can yield defatted sunflower seed meal with a low content of CAs, enabling future use of the protein fraction. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  17. A new beta-glucosidase producing yeast for lower-cost cellulosic ethanol production from xylose-extracted corncob residues by simultaneous saccharification and fermentation

    Science.gov (United States)

    Conventional cellulose-to-ethanol conversion by simultaneous saccharification and fermentation (SSF)requires enzymatic saccharification using both cellulase and ß-glucosidase allowing cellulose utilization by common ethanologenic yeast. Here we report a new yeast strain of Clavispora NRRL Y-50464 th...

  18. Investigating the potential of essential oils as penetration enhancer for transdermal losartan delivery: Effectiveness and mechanism of action

    Directory of Open Access Journals (Sweden)

    Indu Vashisth

    2014-10-01

    Full Text Available The effect of tea tree oil (TTO, cumin oil (CO, rose oil (RO and aloe vera oil (AVO on the skin permeation of losartan potassium (LP was investigated. In vitro skin permeation studies were carried out using rat skin. The mechanism of skin permeation enhancement of LP by essential oils treatment was evaluated by FTIR, DSC, activation energy measurement and histopathological examination. Both concurrent ethanol/enhancer treatment and neat enhancer pretreatment of rat SC with all the oils produced significance increase in the LP flux over the control. The effectiveness of the oils as the penetration enhancers was found to be in the following descending order: AVO > RO > CO > TTO. However, only AVO was the only enhancer to provide target flux required to deliver the therapeutic transdermal dose of LP. FTIR and DSC spectra of the enhancer treated SC indicated that TTO, CO, RO and AVO increased the LP permeation by extraction of SC lipids. The results of thermodynamic studies and histopathological examination of AVO treated SC suggested additional mechanisms for AVO facilitated permeation i.e. transient reduction in barrier resistance of SC and intracellular transport by dekeratinization of corneocytes which may be attributed to the presence of triglycerides as constituents of AVO. It is feasible to deliver therapeutically effective dose of LP via transdermal route using AVO as penetration enhancer.

  19. Optimisation of a headspace-solid-phase micro-extraction method for simultaneous determination of organometallic compounds of mercury, lead and tin in water by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Beceiro-González, E; Guimaraes, A; Alpendurada, M F

    2009-07-17

    In this work, a headspace-solid-phase micro-extraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) method for multielemental speciation of organometallic compounds of mercury, lead and tin in water samples was upgraded by the introduction of tandem mass spectrometry (MS/MS) as detection technique. The analytical method is based on the ethylation with NaBEt(4) and simultaneous headspace-solid-phase micro-extraction of the derivative compounds followed by GC-MS/MS analysis. The main experimental parameters influencing the extraction efficiency such as derivatisation time, extraction time and extraction temperature were optimized. The overall optimum extraction conditions were the following: a 50 microm/30 microm divinyl-benzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) SPME fibre, 150 min derivatisation time, 15 min extraction time, sample agitation at 250 rpm and 40 degrees C extraction temperature. The analytical characteristics of the HS-SPME method combined with GC-MS and GC-MS/MS were evaluated. The combination of both techniques HS-SPME and GC-MS/MS allowed to attain lower limits of detection (4-33 ng l(-1)) than those obtained by HS-SPME-GC-MS (17-45 ng l(-1)). The proposed method presented good linear regression coefficients (r(2)>0.9970) and repeatability (4.8-21.0%) for all the compounds under study. The accuracy of the method measured as the average percentage recovery of the compounds in spiked river water and seawater samples was higher than 80% for all the compounds studied, except for monobutyltin in the river water sample. A study of the uncertainty associated with the analytical results was also carried out.

  20. Simultaneous optimization of the ultrasound-assisted extraction for phenolic compounds content and antioxidant activity of Lycium ruthenicum Murr. fruit using response surface methodology.

    Science.gov (United States)

    Chen, Shasha; Zeng, Zhi; Hu, Na; Bai, Bo; Wang, Honglun; Suo, Yourui

    2018-03-01

    Lycium ruthenicum Murr. (LR) is a functional food that plays an important role in anti-oxidation due to its high level of phenolic compounds. This study aims to optimize ultrasound-assisted extraction (UAE) of phenolic compounds and antioxidant activities of obtained extracts from LR using response surface methodology (RSM). A four-factor-three-level Box-Behnken design (BBD) was employed to discuss the following extracting parameters: extraction time (X1), ultrasonic power (X2), solvent to sample ratio (X3) and solvent concentration (X4). The analysis of variance (ANOVA) results revealed that the solvent to sample ratio had a significant influence on all responses, while the extraction time had no statistically significant effect on phenolic compounds. The optimum values of the combination of phenolic compounds and antioxidant activities were obtained for X1=30min, X2=100W, X3=40mL/g, and X4=33% (v/v). Five phenolic acids, including chlorogenic acid, caffeic acid, syringic acid, p-coumaric acid and ferulic acid, were analyzed by HPLC. Our results indicated that optimization extraction is vital for the quantification of phenolic compounds and antioxidant activity in LR, which may be contributed to large-scale industrial applications and future pharmacological activities research. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Dimethyl carbonate-mediated lipid extraction and lipase-catalyzed in situ transesterification for simultaneous preparation of fatty acid methyl esters and glycerol carbonate from Chlorella sp. KR-1 biomass.

    Science.gov (United States)

    Jo, Yoon Ju; Lee, Ok Kyung; Lee, Eun Yeol

    2014-04-01

    Fatty acid methyl esters (FAMEs) and glycerol carbonate were simultaneously prepared from Chlorella sp. KR-1 containing 40.9% (w/w) lipid using a reactive extraction method with dimethyl carbonate (DMC). DMC was used as lipid extraction agent, acyl acceptor for transesterification of the extracted triglycerides, substrate for glycerol carbonate synthesis from glycerol, and reaction medium for the solvent-free reaction system. For 1g of biomass, 367.31 mg of FAMEs and 16.73 mg of glycerol carbonate were obtained under the optimized conditions: DMC to biomass ratio of 10:1 (v/w), water content of 0.5% (v/v), and Novozyme 435 to biomass ratio of 20% (w/w) at 70°C for 24h. The amount of residual glycerol was only in the range of 1-2.5mg. Compared to conventional method, the cost of FAME production with the proposed technique could be reduced by combining lipid extraction with transesterification and omitting the extraction solvent recovery process. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. A high-throughput liquid chromatography/tandem mass spectrometry method for simultaneous quantification of a hydrophobic drug candidate and its hydrophilic metabolite in human urine with a fully automated liquid/liquid extraction.

    Science.gov (United States)

    Wang, Perry G; Zhang, Jun; Gage, Eric M; Schmidt, Jeffrey M; Rodila, Ramona C; Ji, Qin C; El-Shourbagy, Tawakol A

    2006-01-01

    ABT-869 (A-741439) is an investigational new drug candidate under development by Abbott Laboratories. ABT-869 is hydrophobic, but is oxidized in the body to A-849529, a hydrophilic metabolite that includes both carboxyl and amino groups. Poor solubility of ABT-869 in aqueous matrix causes simultaneous analysis of both ABT-869 and its metabolite within the same extraction and injection to be extremely difficult in human urine. In this paper, a high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) method has been developed and validated for high-speed simultaneous quantitation of the hydrophobic ABT-869 and its hydrophilic metabolite, A-849529, in human urine. The deuterated internal standards, A-741439D(4) and A-849529D(4), were used in this method. The disparate properties of the two analytes were mediated by treating samples with acetonitrile, adjusting pH with an extraction buffer, and optimizing the extraction solvent and mobile phase composition. For a 100 microL urine sample volume, the lower limit of quantitation was approximately 1 ng/mL for both ABT-869 and A-849529. The calibration curve was linear from 1.09 to 595.13 ng/mL for ABT-869, and 1.10 to 600.48 ng/mL for A-849529 (r2 > 0.9975 for both ABT-869 and A-849529). Because the method employs simultaneous quantification, high throughput is achieved despite the presence of both a hydrophobic analyte and its hydrophilic metabolite in human urine. Copyright 2006 John Wiley & Sons, Ltd.

  3. Evaluation of paeonol-loaded transethosomes as transdermal delivery carriers.

    Science.gov (United States)

    Chen, Z X; Li, B; Liu, T; Wang, X; Zhu, Y; Wang, L; Wang, X H; Niu, X; Xiao, Y; Sun, Q

    2017-03-01

    Paeonol shows effective anti-allergic, anti-inflammatory and analgesic activities. However, because of its poor solubility in water and high volatility at room temperature, the application of this drug is restricted in the clinic. The objective of this research was to develop a biocompatible paeonol formulation with improved stability, skin delivery and pharmacokinetic efficiency. In this paper, paeonol-loaded vesicles were prepared using an ethanol injection method. Nano-vesicles were characterized for their physical properties and encapsulation efficiency (EE). Drug permeation behavior in vitro and deposition quantity in porcine ear skin were measured with a Valia-Chien (V-C) diffusion device. Additionally, a validated and sensitive high performance liquid chromatography (HPLC) method was developed to analyze paeonol concentrations in rat plasma after transdermal administration. The results showed that the particle-size order of the nano-vesicles was the following: transethosomes (122.5±7.5nm)transethosomes had a higher EE (85.5±5.2%), and they showed a spherical morphology with a smooth surface when viewed under a transmission electron microscope (TEM). In an in vitro permeation study, the paeonol transethosomes showed an enhanced transdermal flux of 95.7±8.8μg/cm2/h and a higher deposition quantity in porcine ear skin compared to the transfersomes. A one-compartment first-order absorption model could be used to describe the pharmacokinetics of paeonol in rats after transdermal administration. The AUC of the paeonol transethosomes was approximately 1.57- and 3.52-fold higher than those of the transfersomes and a saturated solution of paeonol in 35% ethanol, respectively. The results demonstrated that the paeonol transethosomes had a narrow size distribution, high encapsulation efficiency, and long residence in the plasma. This formulation remarkably enhanced the bioavailability of paeonol. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Transdermal Lipid Nanocarriers: A Potential Delivery System for Lornoxicam.

    Science.gov (United States)

    Dasgupta, Sandipan; Ray, Subhabrata; Dey, Sanjay; Pal, Paulami; Mazumder, Bhaskar

    2017-01-01

    Lornoxicam, is a NSAID of the oxicam class. Its short duration of action owing to rapid elimination and gastrointestinal side effects limits its usefulness when administered orally. The primary objective of the proposed work is to develop suitable lipid nanocarriers for transdermal delivery of Lornoxicam with increased drug residence time at local site of inflamation and in systemic circulation, overcoming undesired gastrointestinal side effects. Lornoxicam loaded lipid nanocarriers like solid lipid nanocarriers (SLN), nano-structured lipid carriers (NLC) & nanoemulsions (NE) were prepared by high-speed homogenization technique. The particle size, zeta potential, and polydispersity index as obtained, were in the range of 140- 193 nm, -22 to -32 mV, and 0.354-0.301 for SLN formulations and 146-201 nm, -23 to -30 mV, and 0.355-0.354 for NLC formulations respectively. Characterization of stable NE revealed that globule size, zeta potential and polydispersity index were within the range of 138 to 195 nm, -26.1±0.123 mV and 0.195 ± 1.231 respectively. It was also observed that entrapment efficacy and drug loading improved as the lipid concentration was increased. The results obtained from the in vitro permeation study and in vivo anti-inflammatory study showed controlled drug permeation, increased bioavailability, longer retention and better therapeutic potential of Lornoxicam after transdermal application of lipid nanoparticles as compared to conventional gel. It can be concluded that the developed lipid nanoparticle loaded gel was found to be a suitable drug delivery carrier for transdermal delivery of Lornoxicam to increase the residence time of drug in systemic circulation and to combat the gastrointestinal side effects. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  5. Diclofenac Transdermal Patch: A Potential Ingress to Maxillofacial Surgery.

    Science.gov (United States)

    Perepa, Anisha; Sinha, Brig Ramen; Uppada, Uday Kiran; Kumar, Avss Subramanya

    2017-06-01

    To evaluate the analgesic efficacy of a diclofenac transdermal patch with diclofenac intra muscular injection in the immediate postoperative period in patients undergoing major oral surgical procedures. Subjects who underwent bijaw surgeries for surgical correction of various dentofacial deformities were included. Sixty such patients who belonged to the above entity were randomly categorized into two groups from Jan 2012-Aug 2015. Group A (study group) received a single dose of 100 mg transdermal diclofenac patch, Group B (control group) received 75 mg intramuscular diclofenac and tramadol HCl 2 mg/kg body wt was used as rescue analgesic in the immediate post operative phase. The analgesic efficacy of the drugs are evaluated on periodic patient's perception of pain in the immediate postoperative phase of 2nd, 6th, 12th, 24th and 48 hours. The mean VAS score in Group A was 2, mean duration of analgesia was 16 h 9 min, and in Group B the mean VAS score was 4, duration of analgesia was 8 h and 4 min. Tramadol HCl was given as rescue analgesia in 22 % (6) of patients belonging to Group A. None of the patients from both the groups reported local complications. A noninvasive application of a single dose of 100 mg transdermal diclofenac patch is more effective than intramuscular diclofenac (75 mg) in the immediate post operative phase, without any significant side-effects is a novel ingress into the field of oral and maxillofacial surgery for post operative pain management.

  6. Development of an Ionic Liquid-Based Ultrasonic/Microwave-Assisted Simultaneous Distillation and Extraction Method for Separation of Camptothecin, 10-Hydroxycamptothecin, Vincoside-Lactam, and Essential Oils from the Fruits of Camptotheca acuminata Decne

    Directory of Open Access Journals (Sweden)

    Chunjian Zhao

    2016-10-01

    Full Text Available An ionic liquid-based ultrasonic/microwave-assisted simultaneous distillation and extraction (IL-UMASDE method for isolating camptothecin (CPT, 10-hydroxycamptothecin (HCPT, vincoside-lactam (VCS-LT, and essential oils (EOs from Camptotheca acuminata Decne fruits was developed. The important parameters were optimized using single-factor and central composite design experiments. The optimum conditions were 0.75 M 1-octyl-3-methylimidazolium ([C8mim]Br as the extraction solvent, a liquid–solid ratio of 13.7 mL/g, an extraction time of 33.2 min, a microwave power of 582 W, and a fixed ultrasonic power of 50 W. The yields of CPT, HCPT, and VCS-LT obtained under the optimum conditions were 2.463, 0.164, and 0.297 mg/g, respectively; these are 1.08-, 1.12-, and 1.04-fold higher, respectively, than those obtained by conventional 55% ethanol heat reflux extraction (HRE. The extraction time for the equilibrium yields of CPT, HCPT and VCS-LT using IL-UMASDE was 33.6%, 58.5%, 63.1%, and 66.8%, respectively, less than the corresponding times using IL-MASDE, IL-ultrasonic-assisted extraction (IL-UAE, 55% ethanol UAE and 55% ethanol HRE. The yield of EOs obtained using IL-UMASDE was 0.793 mg/g, i.e., 1.31-fold higher than that obtained by conventional hydrodistillation extraction (HDE. The components of the EOs obtained using IL-UMASDE and HDE were similar. The extraction time for the equilibrium yields of EOs using IL-UMASDE is 33.6%, 58.5%, 52.6%, and 72.3% lower than those for IL-MASDE, water-UMASDE, water-MASDE, and HDE, respectively. Compared with other extraction methods, IL-UMASDE gave the highest yields of CPT, HCPT, VCS-LT, and EOs and also had the shortest extraction time. IL-UMASDE is a potential green and highly efficient technique for the extraction of CPT, HCPT, VCS-LT, and EOs from Camptotheca acuminata Decne fruits.

  7. Treatment of Severe Cancer Pain by Transdermal Fentanyl

    Directory of Open Access Journals (Sweden)

    Dženita Ljuca

    2010-05-01

    Full Text Available The goal of research was to determine the frequency, intensity, time of occurrence, duration and causes of breakthrough pain (BTP in patients whose carcinoma pain was treated by transdermal fentanyl. (TDF. A prospective study was conducted in a hospice for recumbent patients of the Centre for Palliative Care (hospice University Clinical Centre Tuzla from October 2009 to December 2010. 33 patients in terminal stage of carcinoma, who had been treated by transdermal fentanyl due to their excruciating pain (7-10 mark on numerica! scale with initial dosage of 25 μg as a strong opiate analgesic, were monitored within the time period of 10 days. In the statistics we used the even T - test, the Wilcox test and Mann -Whitney test. The difference was seen to be significant at p < 0,05. Treatment by transdermal fentanyl significantly reduces the intensity of strong carcinoma pain (p < 0.0001, with a frequent requirement for dose increase with bone metastasis. The intensity of BTP is higher compared to the pain experienced upon reception. The frequency and intensity of BTP are significantly reduced already in the second day of treatment by transdermal fentanyl (p = 0,0024. The BTP is most intense in patients with neck and head tumours (9,26 ± 0,66, and most frequent with abdomen and pelvic tumour. The biggest number of BTP (68.3 % occurs within first three days of treatment. BTP most frequently occurs in the evening or at night (between 18:00 and 06:00 h in 62,2 % of the cases, with the duration of usually less than 15 minutes (65,2% of the cases. In 61,6 % cases the occurrence of BTP is related to physical activities or psychosocial incidents, while the cause is undetermined in 38,4 % of examinees.BTP is most frequent within first three days of treatment by TDF. Using the optimal dosage a good control of carcinoma pain is enabled, regardless of the occurrence of bone metastasis, while it also helps reduce the frequency and intensity of BTP.

  8. The preventive effect of Mangifera foetida L. leaf extract administered simultaneously to excess iron on markers of iron overload in Spraque-Dawley rats

    Directory of Open Access Journals (Sweden)

    Purnama Fajri

    2018-02-01

    Full Text Available Background: Recently, there is no agent available for the prevention of iron overload (IO in thalassemia patients. Previous studies showed that Mangifera foetida L. leaf extracts reduced the levels of iron in IO in vitro and in vivo models. The present study aimed to determine the efficacy of Mangifera foetida L. leaf extract in the prevention of IO induced in rats.Methods: Thirty male Sprague-Dawley rats were divided into 5 groups: control (untreated, IO, 3 treatment groups with leaf extract equivalent to 50, 100, and 200 mg of mangiferin per kg BW. Fe-dextran (15 mg was administered intraperitoneally twice a week for 4 weeks to all groups except control (IO, DSM50, DSM100, and DSM200. Urine and blood samples were taken before and after treatments. After 4 weeks of treatment, rats were terminated, and samples of spleen, liver, and heart were taken. Ferritin and mangiferin levels and SOD activities were determined in plasma. Iron levels were measured in plasma, urine, and spleen.Results: Experimental IO increased plasma Fe content 4.23 times and plasma ferritin levels 6.9 times vs normal. Mangifera foetida L. leaf extract DSM50 resulted in the highest blood levels of 212 ng mangiferin per mL and moderately, although not significant, prevented increased plasma ferritin levels and IO in organs and protected against oxidative stress.Conclusion: Aqueous Mangifera foetida L. leaf extract may be useful to prevent IO and oxidative stress in thalassemia patients.

  9. Transdermal hormone therapy in postmenopausal women: A review of metabolic effects and drug delivery technologies

    Directory of Open Access Journals (Sweden)

    Nathan W Kopper

    2008-10-01

    Full Text Available Nathan W Kopper, Jennifer Gudeman, Daniel J ThompsonKV Pharmaceutical, St. Louis, MO, USAAbstract: Vasomotor symptoms (VMS associated with menopause can cause significant discomfort and decrease the quality of life for women in the peri-menopausal and post-menopausal stages of life. Hormone therapy (HT is the mainstay of treatment for menopausal symptoms and is currently the only therapy proven effective for VMS. Numerous HT options are available to treat VMS, including estrogen-only and estrogen-progestogen combination products to meet the needs of both hysterectomized and nonhysterectomized women. In addition to selecting an appropriate estrogen or estrogen-progestogen combination, consideration should be given to the route of administration to best suit the needs of the patient. Delivery systems for hormone therapy include oral tablets, transdermal patches, transdermal topical (nonpatch products, and intravaginal preparations. Oral is currently the most commonly utilized route of administration in the United States. However, evidence suggests that oral delivery may lead to some undesirable physiologic effects caused by significant gut and hepatic metabolism. Transdermal drug delivery may mitigate some of these effects by avoiding gut and hepatic first-pass metabolism. Advantages of transdermal delivery include the ability to administer unmetabolized estradiol directly to the blood stream, administration of lower doses compared to oral products, and minimal stimulation of hepatic protein production. Several estradiol transdermal delivery technologies are available, including various types of patches, topical gels, and a transdermal spray.Keywords: estradiol, hormone therapy, menopause, transdermal drug delivery, vasomotor symptoms

  10. Active enhancement methods for intra- and transdermal drug delivery: a review

    Directory of Open Access Journals (Sweden)

    Barbara Zorec

    2013-05-01

    Full Text Available Transdermal route has some advantages over other drug administration routes. These include avoidance of first pass effect (hepatic metabolism, better pharmacokinetic profile, reduction of side effects and good patient compliance. The greatest obstacle for the drugs to be delivered through the skin is overcoming the impermeable outermost layer of the skin – the stratum corneum. Quite a few enhancement techniques can be used to overcome the stratum corneum barrier and facilitate transdermal drug delivery. These include various passive (penetration enhancers, liposomes and active approaches (electroporation, iontophoresis, microneedles, which are of prime interest for transdermal drug delivery research area.

  11. Kinetic Study of Copper(II Simultaneous Extraction/Stripping from Aqueous Solutions by Bulk Liquid Membranes Using Coupled Transport Mechanisms

    Directory of Open Access Journals (Sweden)

    Loreto León

    2016-09-01

    Full Text Available Heavy metals removal/recovery from industrial wastewater has become a prime concern for both economic and environmental reasons. This paper describes a comparative kinetic study of the removal/recovery of copper(II from aqueous solutions by bulk liquid membrane using two types of coupled facilitated transport mechanisms and three carriers of different chemical nature: benzoylacetone, 8-hydroxyquinoline, and tri-n-octylamine. The results are analyzed by means of a kinetic model involving two consecutive irreversible first-order reactions (extraction and stripping. Rate constants and efficiencies of the extraction (k1, EE and the stripping (k2, SE reactions, and maximum fluxes through the membrane, were determined for the three carriers to compare their efficiency in the Cu(II removal/recovery process. Counter-facilitated transport mechanism using benzoylacetone as carrier and protons as counterions led to higher maximum flux and higher extraction and stripping efficiencies due to the higher values of both the extraction and the stripping rate constants. Acceptable linear relationships between EE and k1, and between SE and k2, were found.

  12. Development of a UFLC-MS/MS method for the simultaneous determination of seven tea catechins in rat plasma and its application to a pharmacokinetic study after administration of green tea extract.

    Science.gov (United States)

    Huo, Yanshuang; Zhang, Qian; Li, Qing; Geng, Bingjie; Bi, Kaishun

    2016-06-05

    A rapid, sensitive and selective ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method was developed and validated for simultaneous determination of seven green tea catechins including catechin (C), (-)-epicatechin (EC), gallocatechin (GC), (-)-epigallocatechin (EGC), (-)-epicatechin-3-gallate (ECG), gallocatechin-3-gallate (GCG) and (-)-epigallocatechin-3-gallate (EGCG) in rat plasma. The plasma samples were firstly hydrolysed with the mixture of β-glucuronidase and sulfatase, which were then extracted by liquid-liquid extraction with ethyl acetate-isopropanol (1:1, v/v). The analytes were separated on a Venusil MP C18 column (Venusil, China) with a gradient elution at a flow rate of 0.4mL/min. The detection was performed in negative ionization and multiple reaction monitoring (MRM) mode. All the calibration curves exhibited good linearity (r>0.9943) with intra- and inter-day precisions of less than 14.3% and the accuracy deviations ranging from -8.8% to 7.5%. The extraction recoveries of the analytes and ethyl gallate (internal standard) were all more than 72%. The validated method was successfully applied to a pharmacokinetic study of seven catechins in rat plasma after oral administration of the green tea extract at different doses of 0.4, 1.2 and 2.0g/kg. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Rapid simultaneous determination of eperisone, tolperisone, and tizanidine in human serum by using a MonoSpin® C18 extraction column and liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Miura, Naoya; Saito, Takeshi; Taira, Takayuki; Yamagiwa, Takeshi; Morita, Sein; Inokuchi, Sadaki

    2014-01-01

    A method was developed for rapid toxicological analysis of eperisone, tolperisone, and tizanidine in human serum using a MonoSpin® C18 extraction column and LC/MS/MS. The method was validated for LOD, linearity, precision, and extraction recovery. This method was rapid with an LOD of 0.5 ng/mL, linearity range 1-500.0 ng/mL (r2 = 0.999), and RSD value below 14.6%. Extraction recovery from the sample was greater than 98.6, 98.8, and 88.5% for eperisone, tolperisone, and tizanidine, respectively. Results showed that combination of the MonoSpin C18 extraction column and LC/MS/MS is a simple and rapid method for the analysis of these three analytes, and a method is described for simultaneous quantitative determination of the analytes in human serum by LC/MSIMS. This method was used to determine the serum levels of eperisone in a patient with eperisone poisoning, and could be successfully applied for screening analyses in clinical cases other than poisoning.

  14. Effective extraction and simultaneous determination of Sudan dyes from tomato sauce and chili-containing foods using magnetite/reduced graphene oxide nanoparticles coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Zhang, Ming-Yue; Wang, Man-Man; Hao, Yu-Lan; Shi, Xin-Ran; Wang, Xue-Sheng

    2016-05-01

    A simple, effective, and robust magnetic solid-phase extraction method was developed using magnetite/reduced graphene oxide nanoparticles as the adsorbent for the simultaneous determination of Sudan dyes (I, II, III, and IV) in foodstuffs. The magnetite/reduced graphene oxide nanoparticles were characterized by X-ray diffraction, scanning electron microscopy, and vibrating sample magnetometry. The extraction parameters including extraction time, elution solution, and elution time and volume were investigated in detail. Such magnetite/reduced graphene oxide nanoparticles based magnetic solid-phase extraction in combination with high-performance liquid chromatography and variable wavelength detection gave the detection limits of 3-6 μg/kg for Sudan I-IV in chili sauce, tomato sauce, chili powder, and chili flake samples. The recoveries were 79.6-108% at three spiked levels with the intra- and inter-day relative standard deviations of 1.2-8.6 and 4.5-9.6%, respectively. The feasibility was further performed by a comparison with commercial alumina-N. This method is suitable for the routine analysis of Sudan dyes due to its sensitivity, simplicity, and low cost. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Simultaneous determination of senkyunolide I and senkyunolide H in rat plasma by LC-MS: application to a comparative pharmacokinetic study in normal and migrainous rats after oral administration of Chuanxiong Rhizoma extract.

    Science.gov (United States)

    Zhao, Xu; Ma, Tiancheng; Zhang, Chenning; Shi, Shaohuai; Cui, Sijiao; Bi, Kaishun; Jia, Ying

    2015-09-01

    A selective liquid chromatographic-mass spectrometric method has been developed and validated for simultaneous determination of senkyunolide I (SEI) and senkyunolide H (SEH) from Chuanxiong Rhizoma in rat plasma. Plasma samples were extracted by liquid-liquid extraction with ethyl acetate and separated on a Kromasil C18 column (250 × 4.6 mm, 5 µm), with methanol-water (55:45, v/v) as mobile phase. The linear range was 0.05-25 µg/mL for SEI and 0.01-5.0 µg/mL for SEH, with lower limits of quantitation of 0.05 and 0.01 µg/mL, respectively. Intra- and inter-day precision were within 10.0 and 9.8%, and the accuracies (relative errors) were rats after oral administration of Chuanxiong Rhizoma extract. The results indicated that there were obvious differences between normal and migrainous rats in the pharmacokinetic behavior after oral administration of Chuanxiong Rhizoma extract. The absorption of SEI and SEH were significantly increased in migrainous rats compared with normal rats. Copyright © 2015 John Wiley & Sons, Ltd.

  16. Lecithin/chitosan nanoparticles for transdermal delivery of melatonin.

    Science.gov (United States)

    Hafner, Anita; Lovrić, Jasmina; Pepić, Ivan; Filipović-Grčić, Jelena

    2011-01-01

    In this study, the potential of lecithin/chitosan nanoparticles (NPs) as colloidal nanosystem for transdermal melatonin delivery was investigated. Mean diameter and zeta-potential of NPs differing in lecithin type (Lipoid S45 and S100) and chitosan content ranged between 113.7 and 331.5 nm and 4.6 and 31.2 mV, respectively. Melatonin loadings were up to 7.2%. The potential of lecithin/chitosan NPs to enhance transdermal melatonin delivery was investigated by determining the drug flux across dermatomed porcine skin and its skin deposition. Lecithin/chitosan NPs provided 1.3-2.3-fold higher flux compared to melatonin solution. The highest flux, 9.0 ± 0.21 µg/cm²/h, was observed for S45 lecithin/chitosan NPs with lecithin/chitosan weight ratio of 20:1. NP possible cytotoxicity in vitro was evaluated using human skin keratinocytes and fibroblasts. It was demonstrated that lecithin/chitosan NPs can be applied to skin cells at concentrations up to 200 µg/mL without inducing plasma membrane damage or cell viability decrease.

  17. Carbon Nanotube Micro-Needles for Rapid Transdermal Drug Delivery

    Science.gov (United States)

    Lyon, Bradley; Aria, Adrianus Indrat; Gat, Amir; Cosse, Julia; Montemayor, Lauren; Beizaie, Masoud; Gharib, Morteza

    2012-11-01

    By catalyst patterning, bundles of vertically-aligned carbon nanotubes (CNT) can be assembled to create 2D arrays of hollow micro-needles with feature size as small as a few microns. For transdermal drug delivery, the most challenging mechanical requirement is to make the CNT micro-needle small enough so that delivery is painless yet large enough so that the micro-needle can achieve skin penetration. By taking advantage of capillary action and the nanoporosity of CNT bundles, we can wick high strength polymer into the inter-spacing between nanotubes to augment the stiffness of our micro-needles. For low viscous polymers, the large ratio between the micron sized center hole of the micro-needle and the nanopores of the surrounding CNT allow us to wick polymer through the nanotubes while maintaining an open central hole for drug transport. For a transdermal patch prototype with a delivery area less than 1cm x 1cm square, we can fabricate 50 CNT micro-needles that produces a total flow rate up to 100 uL/s with actuation pressure provided by a mere finger tap. From in vitro experiments, we will demonstrate that CNT micro-needles provide a much faster convective delivery of drugs than conventional topical diffusion based patches. We acknowledge Zcube s.r.l for their support of this work.

  18. A novel microparticulate vaccine for melanoma cancer using transdermal delivery.

    Science.gov (United States)

    Bhowmik, Tuhin; D'Souza, Bernadette; Shashidharamurthy, Rangaiah; Oettinger, Carl; Selvaraj, Periasamy; D'Souza, Martin J

    2011-01-01

    In this study, we formulated a microparticulate melanoma cancer vaccine via the transdermal route. The vaccine was delivered using microneedle-based Dermaroller® which is available for cosmetic purposes. Unlike subcutaneous injections, administration using microneedles is painless and in general can increase the permeability of many compounds ranging in size from small molecules to proteins and microparticles that do not normally penetrate the skin. The vaccine microparticles were taken up by the antigen presenting cells which demonstrated a strong IgG titre level of 930 ug/mL in serum samples. The formulation increased the immunogenicity of the vaccine by incorporating the antigen into an albumin matrix having a size range of around 0.63-1.4 µm which acted as a synthetic adjuvant. The animals were vaccinated with 1 prime and 4 booster doses administered every 14 days over 8 weeks duration, followed by challenge with live tumour cells which showed protection after transdermal vaccination.

  19. Rapidly dissolvable microneedle patches for transdermal delivery of exenatide.

    Science.gov (United States)

    Zhu, Zhuangzhi; Luo, Huafei; Lu, Wangding; Luan, Hansen; Wu, Yubo; Luo, Jing; Wang, Youjie; Pi, Jiaxin; Lim, Chee Yen; Wang, Hao

    2014-12-01

    To assess the feasibility of transdermal delivery of exenatide (EXT) using low-molecular-weight sodium hyaluronate (HA) dissolving microneedles (MNs) patches for type 2 diabetes mellitus therapy. Micromold casting method was used to fabricate EXT-loaded dissolving MNs. The characteristics of prepared MNs including mechanical strength, in vitro/in vivo insertion capacity, dissolution profile and storage stability were then investigated. Finally, the in vivo pharmacokinetics and hypoglycemic effects were compared with traditional subcutaneous (SC) injection. EXT-loaded dissolving MNs made of HA possessed sufficient mechanical strength and the strength could be weakened as the water content increases. The EXT preserved its pharmacological activity during fabrication and one-month storage. With the aid of spring-operated applicator, dissolving MNs could be readily penetrated into the skin in vitro/in vivo, and then rapidly dissolved to release encapsulated drug within 2 min. Additionally, transepidermal water loss (TEWL) determinations showed that skin's barrier properties disrupted by MNs recovered within 10-12 h. Transdermal pharmacokinetics and antidiabetic effects studies demonstrated that fabricated EXT MNs induced comparable efficacy to SC injection. Our rapidly dissolving MNs patch appears to an excellent, painless alternative to conventional SC injection of EXT, and this minimally invasive device might also be suitable for other biotherapeutics.

  20. Microneedle arrays as medical devices for enhanced transdermal drug delivery.

    Science.gov (United States)

    Garland, Martin J; Migalska, Katarzyna; Mahmood, Tuan Mazlelaa Tuan; Singh, Thakur Raghu Raj; Woolfson, A David; Donnelly, Ryan F

    2011-07-01

    In order to exploit the transdermal route for systemic delivery of a wide range of drug molecules, including peptide/protein molecules and genetic material, a means of disrupting the excellent barrier properties of the uppermost layer of the skin, the stratum corneum, must be sought. The use of microneedle (MN) arrays has been proposed as a method to temporarily disrupt the barrier function of the skin and thus enable enhanced transdermal drug delivery. MN arrays consist of a plurality of micron-sized needles, generally ranging from 25 to 2000 µm in height, of a variety of different shapes and composition (e.g., silicon, metal, sugars and biodegradable polymers). The application of such MN arrays to the skin results in the creation of aqueous channels that are orders of magnitude larger than molecular dimensions and, therefore, should readily permit the transport of macromolecules. This article will focus on recent and future developments for MN technology, focusing on the materials used for MN fabrication, the forces required for MN insertion and potential safety aspects that may be involved with the use of MN devices.

  1. Magnetophoresis in combination with chemical enhancers for transdermal drug delivery.

    Science.gov (United States)

    Sammeta, Srinivasa M; Repka, Michael A; Narasimha Murthy, S

    2011-09-01

    The objective of the present work was to investigate the effect of combination of a novel physical permeation enhancement technique, magnetophoresis with chemical permeation enhancers on the transdermal delivery of drugs. The in vitro drug transport studies were carried out across the freshly excised abdominal skin of Sprague-Dawley rats using transdermal patch systems (magnetophoretic and non-magnetophoretic) of lidocaine hydrochloride (LH). LH gel prepared using hydroxypropyl methylcellulose (HPMC) was spread over the magnets as a thin layer. To investigate the effect of chemical permeation enhancers, menthol, dimethyl sulfoxide, sodium lauryl sulfate and urea (5% w/v) were incorporated in the gels prior to loading on the patch system. The flux of lidocaine from magnetophoretic patch was ~3-fold higher (3.07 ± 0.43 µg/cm(2)/h) than that of the control (non-magnetophoretic patch) (0.94 ± 0.13 µg/cm(2)/h). Incorporation of chemical permeation enhancers in the gel enhanced the magnetophoretic delivery flux by ~4 to 7-fold. The enhancement factor due to combination of chemical permeation enhancer was additive and not synergistic. Mechanistic studies indicated that magnetophoresis mediated drug delivery enhancement was via appendageal pathway.

  2. Nanosized ethosomes bearing ketoprofen for improved transdermal delivery.

    Science.gov (United States)

    Chourasia, Manish K; Kang, Lifeng; Chan, Sui Yung

    2011-05-01

    The potential of ethosomes for delivering ketoprofen via skin was evaluated. The ethosomes were prepared, optimized and characterized. Vesicular shape, size and entrapment efficiency were determined by transmission electron microscopy, dynamic light scattering and minicolumn centrifugation technique, respectively. Vesicle sizes varied from 120.3±6.1 to 410.2±21.8 nm depending on the concentrations of soya phosphatidyl choline (SPC) and ethanol. Entrapment efficiency increased with concentrations of SPC and ethanol. The formulations exhibited entrapment efficiencies of 42-78%. In vitro release through cellophane membrane showed sustained release of drug from ethosomal formulations in contrast to hydroalcoholic drug solution (HA), which released most of the drug within 2-3 h. In vitro drug permeation across human skin revealed improved drug permeation and higher transdermal flux with ethosomal formulations compared to hydroethanolic drug solution. Kinetics of in vitro skin permeation showed zero order drug release from formulations. Based on in vitro transdermal flux, the estimated steady state in vivo plasma concentration from ethosomes attained therapeutic drug levels whereas hydroalcoholic drug solution exhibited sub therapeutic drug concentration with a patch size of 50 cm(2). Skin permeation of ethosomal formulations assessed by confocal microscopy revealed enhanced permeation of Rhodamine 123 loaded formulation in comparison to the hydroalcoholic solution.

  3. [Preparation and transdermal diffusion of ursolic acid ethosomes].

    Science.gov (United States)

    Chen, Yan; Wiu, Qingqing; Zhang, Zhenhai; Zhou, Lei; Liu, Xuan; Du, Meng; Jia, Xiaobin

    2011-04-01

    To prepare ursolic acid ethosomes and investigate the penetration characteristics of ursolic ethosomes as a transdermal vehicle. Ursolic acid ethosomes were prepared by injection method, and the shape and particle size of the ethosomes were analyzed. Ursolic acid permeation tests in vitro through the skin of rats were performed in TP-3 diffusion cell. The accumulated permeation amounts of ursolic acid 10% isopropanol solution, ursolic acid liposomes, ursolic acid ethosomes were compared. The average encapsulation percentage, particle size, and Zeta potential of the ethosomes were (95.83 +/- 0.86)%, (87.5 +/- 7.5) nm and - (38.4 +/- 3.6) mV, respectively. The accumulated permeation amount of the ethosomes in 12 h was 146.49 microg x cm(-2), and its transdermal permeability in 12 h was 12.17 microg x cm(-2) x h(-1). The encapsulation percentage of the ethosomes is good, and the stability of the ursolic acid ethosomes is fine. Ethosomes can significantly enhance the diffusion rate of ursolic acid through the skin of rats.

  4. Starch nanocrystals based hydrogel: Construction, characterizations and transdermal application.

    Science.gov (United States)

    Bakrudeen, Haja Bava; Sudarvizhi, C; Reddy, B S R

    2016-11-01

    Bio-based nanocomposites were prepared using starch nanocrystals obtained by acid hydrolysis of native starches using different acid sources. In recent times, focuses on starch nanocrystals (SNCs) have been increasing in number of research works dedicated to the development of bio-nanocomposites by blending with different biopolymeric matrices. The work mainly deals with the preparation of starch nanocrystals using different native starches by acid hydrolysis using hydrochloric acid and trifluroacetic acid. The as-prepared starch nanocrystals are having high crystallinity and more platelet morphologies, and used as a drug carrying filler material in the hydrogel formulations with the care of different polymer matrices. The condensed work also concentrates on the dispersion of antiviral drug in the hydrogels, which are applied onto biocompatible bio-membrane to be formulating a complete transdermal patch. The acid hydrolysed starch nanocrystals were thoroughly characterized using TEM, SEM, particle size analysis and zeta potential. Their thermal stability and the crystalline properties were also characterized using TG-DSC and XRD respectively. The physiochemical interaction and compatibility between the drug and the SNCs filler in the polymeric hydrogels were evaluated using FT-IR analysis. The formulated hydrogels were subjected to evaluation of in vitro permeation studies using Franz diffusion studies. The in vitro study was indicated substantial guarantee for the fabrication of drug dispersed in polymeric hydrogels using SNCs as filler matrices for a successful transdermal drug delivery. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Plasma Concentrations of Fentanyl Achieved With Transdermal Application in Chickens.

    Science.gov (United States)

    Delaski, Kristina M; Gehring, Ronette; Heffron, Brendan T; Negrusz, Adam; Gamble, Kathryn C

    2017-03-01

    Providing appropriate analgesia is an important concern in any species. Fentanyl, a μ-receptor specific opioid, use is common in mammalian species but has been incompletely evaluated for this purpose in avian species. Transdermal fentanyl patches were applied to domestic chickens (n = 10) of varying breeds for 72 hours. Repeated blood samples were collected from the birds to assess time-concentration of fentanyl and norfentanyl in plasma, as assayed by liquid chromatography-mass spectrometry, throughout patch application and for 48 hours after patch removal. Compartmental modeling was used to characterize the elimination profiles. Evaluation as a large bolus, followed by slower elimination rates over the remaining time, best fit the data as a one-compartment open model. Although maximum plasma fentanyl concentrations varied substantially by individual birds, chickens trended into 2 general groups of maximum plasma concentration, clearance, and volume of distribution, which was attributed to absorption variability. For all birds, harmonic mean of elimination half-life was 7.2 ± 3.7 hours and showed less individual variation than the other pharmacokinetic parameters. Because the application of transdermal fentanyl patches in the chickens achieved plasma fentanyl concentrations considered therapeutic in people, this approach could provide an additional analgesic option for avian patients.

  6. Fatty acid vesicles acting as expanding horizon for transdermal delivery.

    Science.gov (United States)

    Kumar, Lalit; Verma, Shivani; Kumar, Sanjeev; Prasad, Deo Nandan; Jain, Amit Kumar

    2017-03-01

    The body is protected against the external environment by the skin due to its physical barrier nature. Stratum corneum composed of corneocytes surrounded by lipid region performs a major barrier function as it lies in the uppermost area of skin. Alteration in barrier function, increase in permeability, and disorganization of stratum corneum represent diseased skin. Drugs applied to the diseased skin should induce a local effect at the site of application or area close to it along with cutaneous absorption rather than percutaneous absorption. Conventional formulations like ointments, gels, and creams suffer from the drawback of limited local activity. For the enhancement of drug penetration and localization of the drug at the site of action approaches explored are liposomes, niosomes, ethosomes microparticles, and solid lipid nanoparticles. Vesicles composed of fatty acids like oleic acid and linoleic acid represent the new approach used for transdermal penetration and localization. In this review article, our major aim was to explore the applications of fatty acid vesicles for transdermal delivery of various bioactives.

  7. In vivo transdermal delivery of leuprolide using microneedles and iontophoresis.

    Science.gov (United States)

    Sachdeva, Vishal; Zhou, Yingcong; Banga, Ajay K

    2013-01-01

    The objective of this study was to investigate the use of iontophoresis and/or microneedles to enhance transdermal delivery of leuprolide acetate in vivo in hairless rats. Microporation was achieved using 500 μm long maltose microneedles and pore formation was confirmed using dye binding studies, histology studies, calcein imaging studies, pore permeability index calculation and trans-epidermal water loss measurement. Iontophoresis was performed using liquid reservoir patch with inbuilt silver wire electrode and a current density of 0.1 mA/cm2 was applied for 4 hours. Delivery studies were performed using microneedles and iontophoresis alone and in combination. Passive studies involving delivery through intact skin and injections of drug solution administered subcutaneously served as controls. Blood samples were collected at predetermined time points and plasma samples were analyzed for drug using ELISA. Significantly higher drug levels were detected at the end of 6 hours treatment by microneedles alone treatment (0.98 ± 0.08 ng/ml) as compared to passive (0.36 ± 0.22 ng/ml) delivery (p microneedles alone treatment (p microneedles and/or iontophoresis seems promising for the transdermal delivery of peptide like leuprolide acetate.

  8. Biocompatible 5-Aminolevulinic Acid/Au Nanoparticle-Loaded Ethosomal Vesicles for In Vitro Transdermal Synergistic Photodynamic/Photothermal Therapy of Hypertrophic Scars

    Science.gov (United States)

    Zhang, Zheng; Chen, Yunsheng; Ding, Jiayue; Zhang, Chunlei; Zhang, Amin; He, Dannong; Zhang, Yixin

    2017-12-01

    Biocompatible 5-aminolevulinic acid/Au nanoparticle-loaded ethosomal vesicle (A/A-ES) is prepared via ultrasonication for synergistic transdermal photodynamic/photothermal therapy (PDT/PTT) of hypertrophic scar (HS). Utilizing ultrasonication, Au nanoparticles (AuNPs) are synthesized and simultaneously loaded in ethosomal vesicles (ES) without any toxic agents, and 5-aminolevulinic acid (ALA) is also loaded in ES with 20% of the entrapment efficiency (EE). The prepared A/A-ES displays strong absorbance in 600-650 nm due to the plasmonic coupling effect between neighboring AuNPs in the same A/A-ES, which can simultaneously stimulate A/A-ES to produce heat and enhance quantum yields of reactive oxygen species (ROS) by using 632 nm laser. In vitro transdermal penetrability study demonstrates that A/A-ES acts as a highly efficient drug carrier to enhance both ALA and AuNPs penetration into HS tissue . Taking human hypertrophic scar fibroblasts (HSF) as therapeutic targets, synergistic PDT/PTT of HS indicates that A/A-ES could enhance quantum yields of ROS by photothermal effect and localized surface plasmon resonance (LSPR) of AuNPs, resulting in a high level of apoptosis or necrosis. In a word, the prepared A/A-ES shows a better synergistic PDT/PTT efficiency for HSF than the individual PDT and PTT, encouraging perspective for treatment of HS.

  9. Effectively simultaneous naked-eye detection of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin extracted from red cabbage as chelating agent.

    Science.gov (United States)

    Khaodee, Warangkhana; Aeungmaitrepirom, Wanlapa; Tuntulani, Thawatchai

    2014-05-21

    Simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin as a chelating agent was investigated in terms of both quantitative and qualitative detections. Cyanidin was extracted and purified from red cabbage which is a local plant in Thailand. The selectivity of this method was examined by regulating the pH of cyanidin solution operated together with masking agents. It was found that Cu(II), Pb(II), Al(III) and Fe(III) simultaneously responded with the color change at pH 7, pH 6, pH 5 and pH 4, respectively. KF, DMG and the mixture of KF and DMG were used as masking agents for the determination of Fe(III), Al(III) and Pb(II), respectively. Results from naked-eye detection were evaluated by comparing with those of inductively coupled plasma (ICP), and there was no significant difference noticed. Cyanidin using as a multianalyte reagent could be employed for simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) at the lowest concentration at 50, 80, 50 and 200μM, respectively, by slightly varying pHs. Moreover, the proposed method could be potentially applied for real water samples with simplicity, rapidity, low cost and environmental safety. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. An LC-MS/MS method for the simultaneous determination and pharmacokinetic studies of bergenin, chlorogenic acid and four flavonoids in rat plasma after oral administration of a QingGanSanJie decotion extract.

    Science.gov (United States)

    Zhao, Liang; Qian, Xian; Li, Wuhong; Lv, Lei; Zhang, Hai; Chai, Yifeng; Zhang, Guoqing

    2014-12-01

    A rapid, simple and sensitive, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of bergenin, chlorogenic acid and four flavonoids in a QingGanSanJie preparation in rat plasma. Puerarin was selected as the internal standard (IS). Plasma samples were precipitated with methanol and separated with a reverse phase Agilent Poroshell 120 EC-C18 column using a gradient mobile phase of methanol-water containing 0.1% formic acid (v/v). A triple quadruple mass spectrometer was used for quantification (limit of detection 0.36-5.55 ng/mL). Intra-day and inter-day precisions were within 15% and the average extraction recoveries ranged from 85 to 115% for each analyte. The method allowed simultaneous quantification for the first time of the pharmacokinetics of bergenin, chlorogenic acid and four flavonoids after intragastric administration of a QingGanSanJie extract in Sprague-Dawley rats. It was found that bergenin and chlorogenic acid had typical extravascular administration concentration-time curves; flavonoids had a bimodal distribution improving bioavailability and extending the pharmacodynamics period. Copyright © 2014 John Wiley & Sons, Ltd.

  11. Simultaneous determination of thirteen flavonoids from Xiaobuxin-Tang extract using high-performance liquid chromatography coupled with electrospray ionization mass spectrometry.

    Science.gov (United States)

    Cen, Meifeng; Ruan, Jinxiu; Huang, Lihua; Zhang, Zhenqing; Yu, Nengjiang; Zhang, Youzhi; Cheng, Xuange; Xiong, Xiaohong; Wang, Guixiang; Zang, Linquan; Wang, Sujun

    2015-11-10

    A simple and reliable high performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS) analysis method was established to simultaneously determine thirteen flavonoids of Xiaobuxing-Tang in intestine perfusate, namely onpordin, 3'-O-methylorobol, glycitein, patuletin, genistein, luteolin, quercetin, nepitrin, quercimeritrin, daidzin, patulitrin, quercetagitrin and 3-glucosylisorhamnetin. Detection was performed on a quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source operating in negative ionization mode. Negative ion ESI was used to form deprotonated molecules at m/z 315 for onpordin, m/z 299 for 3'-O-methylorobol, m/z 283 for glycitein, m/z 331 for patuletin, m/z 269 for genistein, m/z 285 for luteolin, m/z 301 for quercetin, m/z 477 for nepitrin, m/z 463 for quercimeritrin, m/z 461 for daidzin, m/z 493 for patulitrin, m/z 479 for quercetagitrin, m/z 477 for 3-glucosylisorhamnetin and m/z 609.2 for rutin. The linearity, sensitivity, selectivity, repeatability, accuracy, precision, recovery and matrix effect of the assay were evaluated. The proposed method was successfully applied to simultaneous determination of these thirteen flavonoids, and using this method, the intestinal absorption profiles of thirteen flavonoids were preliminarily predicted. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

    Directory of Open Access Journals (Sweden)

    Abdulrahman Bahrami

    2017-02-01

    Full Text Available This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD (% values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens.

  13. Evaluation of alternative environmentally friendly matrix solid phase dispersion solid supports for the simultaneous extraction of 15 pesticides of different chemical classes from drinking water treatment sludge.

    Science.gov (United States)

    Soares, Karina Lotz; Cerqueira, Maristela Barnes Rodrigues; Caldas, Sergiane Souza; Primel, Ednei Gilberto

    2017-09-01

    This study describes the development, optimization and validation of a method for the extraction of 15 pesticides of different chemical classes in drinking water treatment sludge (DWTS) by vortex-assisted Matrix Solid Phase Dispersion (MSPD) with determination by gas chromatography coupled to mass spectrometry. It focused on the application of alternative and different solid supports to the extraction step of the MSPD. The main parameters that influenced the extraction were studied in order to obtain better recovery responses. Recoveries ranged from 70 to 120% with RSD below 20% for all analytes. Limits of quantification (LOQ) of the method ranged from 5 to 500 μg kg-1 whereas the analytical curves showed correlation coefficients above 0.997. The method under investigation used low volume of solvent (5 mL), low sample mass (1.5 g) and low mass of chitin (0.5 g), an environmentally friendly support. It has advantages, such as speed, simplicity and low cost material, over other methods. When the method was applied, 4 out of 15 pesticides were detected in the DWTS samples in concentrations below the LOQ. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Simultaneous determination of four phenolic compounds in extracts of aerial parts of Ipomoea pes-caprae (L. R. Br. (Convolvulaceae by HPLC-UV

    Directory of Open Access Journals (Sweden)

    Daniela Maes Dutra

    2014-01-01

    Full Text Available Among other applications, Ipomoea pes-caprae is popularly used to treat jellyfish stings, supporting the development of a product for dermatological use. Hydroethanolic spray-dried extract was chosen for the further development of phytomedicines, and a stability-indicative HPLC-UV method was developed and validated for the determination of isoquercitrin and isochlorogenic acids A, B and C. The method was developed using a C18 column (250 x 4.6 mm, 5 µm with an acetonitrile:water mobile phase at pH 3.0 in a gradient run. The four constituents and other unidentified components of the extract were appropriately resolved without interference of degradation products after stress tests (acid, alkali, neutral, oxidant, photolysis. The method showed linearity in the isoquercitrin concentration range from 5.0-50.0 µg mL-1, with adequate precision (RSD% < 2.5% for the intra- and inter-day studies, accuracy (recovery of 100.0 ± 2.0%, and robustness. Both the herbal drug and spray-dried extract of I. pes-caprae were subjected to stability studies in accelerated and long-term conditions over four months. The samples maintained their characteristics and marker contents (< 10% of variation.

  15. Simultaneous determination of methamphetamine and amphetamine in human urine using pipette tip solid-phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kumazawa, Takeshi; Hasegawa, Chika; Lee, Xiao-Pen; Hara, Kenji; Seno, Hiroshi; Suzuki, Osamu; Sato, Keizo

    2007-06-28

    Methamphetamine and amphetamine were extracted from human urine samples using pipette tip solid-phase extraction (SPE) with MonoTip C18 tips (pipette tip volume, 200 microl), in which C18-bonded monolithic silica gel was fixed. A sample of human urine (0.5 ml) containing methamphetamine, amphetamine, and N-methylbenzylamine as internal standard (IS), was mixed with 25 microl of 1M sodium hydroxide solution. The mixture was extracted into the C18 phase of the SPE tip by 25 repeated aspirating/dispensing cycles using a manual micropipettor. Analytes retained in the C18 phase were then eluted with methanol by five repeated aspirating/dispensing cycles. After derivatization with trifluoroacetic anhydride, analytes were measured by gas chromatography/mass spectrometry with selected ion monitoring in the positive-ion electron impact mode. Recoveries of methamphetamine, amphetamine, and IS spiked into urine were more than 82.9, 82.2, and 78.2%, respectively. Regression equations for methamphetamine and amphetamine showed excellent linearity in the range of 0.25-200 ng/0.5 ml. Limit of detection was 0.04 ng/0.5 ml for methamphetamine and 0.05 ng/0.5 ml for amphetamine. Intra- and inter-day coefficients of variations for both stimulants were not greater than 10.8%. The data obtained from actual determination of methamphetamine and amphetamine in autopsy urine samples are also presented for validation of the method.

  16. Comparative enhancing effects of electret with chemical enhancers on transdermal delivery of meloxicam in vitro

    Energy Technology Data Exchange (ETDEWEB)

    Cui, L L; Hou, X M; Li, G D [Department of Inorganic Chemistry, College of Pharmacy, Second Military Medical University, Shanghai, 200433 (China); Jiang, J; Liang, Y Y; Xin, X [Department of Physics and Mathematics, College of Basic Medical Sciences, Second Military Medical University, Shanghai, 200433 (China)], E-mail: cuilili39@hotmail.com, E-mail: JJiang0827@hotmail.com

    2008-12-01

    Electret offers enhancing effect in transdermal drug delivery for altering of the arrangement of lipid molecules in the stratum corneum, forming many transient permeable apertures and enhancing the transdermal drug delivery. In this paper, meloxicam patch formulations were developed to make the comparative study of transdermal drug delivery between electret and chemical enhancers. Patches were made into control, electret, chemical enhancer and electret with chemical enhancer ones, according to the preparation procedure. The electret combined with chemical enhancer patch was designed to probe the incorporation between electret and chemical enhancer in transdermal drug delivery. The meloxicam release from the patch was found to increase in order of blank, chemical enhancer, electret and electret with chemical enhancer patch, in general.

  17. Prodrugs of gestodene for matrix-type transdermal drug delivery systems.

    Science.gov (United States)

    Lipp, R; Laurent, H; Günther, C; Riedl, J; Esperling, P; Täuber, U

    1998-09-01

    The aim of this study was to enhance the transdermal absorption of the highly active progestin gestodene from matrix type transdermal delivery systems (TDDS) by formation of prodrugs with improved matrix solubility. Gestodene esters were synthesized via acylation of the drug with the respective carboxylic anhydrides. Subsequently TDDS were produced using the solvent cast method. Selected formulations were examined with in vitro diffusion experiments using skin of nude mice. One prodrug, gestodene caproate proved to be an oil at ambient temperature and showed a very high solubilty of over 10.5% in the TDDS matrix. Within in vitro penetration studies using those systems the prodrug exhibited a significantly higher transdermal penetration rate than gestodene from reference systems. Furthermore, the prodrug was hydrolyzed to the parent drug to a high extent during the passage of the skin. Designing prodrugs to the requirements of matrix TDDS is an efficient way of enhancing the transdermal drug flux rate.

  18. [Synthetical evaluation of promoting effect of some kinds of transdermal enhancers with grey relational cluster method].

    Science.gov (United States)

    Wang, Hui; Li, Xin; Xu, Bi-lian; Xu, Wei-ming

    2004-05-01

    Synthetical evaluation of promoting effect of some kinds of transdermal enhancers was carried through. Diclofenac sodium was used as model, and azone and l-menthol and synthetic borneol and olieic acid and essential oil from Cnidium monnieri were used as transdermal enhancers. Transdermal absorption experimentation of diclofenac sodium on the device of penetrating skins in vitro was done. Cumulation of permeation amount and penetrating rates and steady fluxes and lag times were observed, and grey relational cluster method was used to evaluate the promoting effect of some kinds of transdermal enhancers. As for promoting effect on diclofenac sodium, azone and l-menthol were the best, and synthetic borneol and olieic acid ranked behind. Grey relational cluster method can evaluate promoting effect objectively and fairly.

  19. Efficacy of a single dose of a transdermal diclofenac patch as pre ...

    African Journals Online (AJOL)

    2012-01-25

    Jan 25, 2012 ... Original Research: Efficacy of single dose of transdermal diclofenac patch. 194 ... period. Prevention and establishment of this hypersensitivity ... This clinical ..... International Journal Pharmaceutical Sciences Review and.

  20. [Has the transdermal patch gone up in smoke? A fatal fentanyl intoxication].

    Science.gov (United States)

    Oechsler, Stephanie; Zimmer, Gisela; Pedal, Ingo; Skopp, Gisela

    2009-01-01

    Recently, there has been an increase in fentanyl-related overdoses following administration of transdermal patches by the buccal, oral or intravenous route or via inhalation. A fatal intoxication is reported with clear evidence from toxicological analysis. However, the administration route and the fate of the patch remained elusive at the end of the investigations. Alcohol was present in the blood in small quantity (0.024%), whereas no other drug could be detected by basic strategies. Autopsy and microscopic examination failed to find sufficient evidence for a diagnosis. Fentanyl and norfentanyl were determined from body fluids and tissues by LC/MS/MS following liquid/liquid extraction. Both analytes were detectable in all specimens under investigation except muscle tissue where norfentanyl was absent. While the fentanyl concentration in the blood was considered potentially life-threatening on the basis of data obtained from living persons and fentanyl-related deaths, it was difficult to assess the other values because no comparative data were available. The history and circumstances of the case together with the toxicological findings suggest an intravenous or inhalative application of the patch. The latter assumption is supported by the fact that the body was found holding a cigarillo butt in his right hand. The case underlines the necessity to study fentanyl-related deaths more closely to allow a better interpretation of potential intoxications.

  1. Rapid and Simultaneous Detection of Mycobacterium tuberculosis Complex and Beijing/W Genotype in Sputum by an Optimized DNA Extraction Protocol and a Novel Multiplex Real-Time PCR ▿

    Science.gov (United States)

    Leung, Eric T. Y.; Zheng, L.; Wong, Rity Y. K.; Chan, Edward W. C.; Au, T. K.; Chan, Raphael C. Y.; Lui, Grace; Lee, Nelson; Ip, Margaret

    2011-01-01

    Rapid diagnosis and genotyping of Mycobacterium tuberculosis by molecular methods are often limited by the amount and purity of DNA extracted from body fluids. In this study, we evaluated 12 DNA extraction methods and developed a highly sensitive protocol for mycobacterial DNA extraction directly from sputa using surface-coated magnetic particles. We have also developed a novel multiplex real-time PCR for simultaneous identification of M. tuberculosis complex and the Beijing/W genotype (a hypervirulent sublineage of M. tuberculosis) by using multiple fluorogenic probes targeting both the M. tuberculosis IS6110 and the Rv0927c-pstS3 intergenic region. With reference strains and clinical isolates, our real-time PCR accurately identified 20 non-Beijing/W and 20 Beijing/W M. tuberculosis strains from 17 different species of nontuberculosis Mycobacterium (NTM). Further assessment of our DNA extraction protocol and real-time PCR with 335 nonduplicate sputum specimens correctly identified all 74 M. tuberculosis culture-positive specimens. In addition, 15 culture-negative specimens from patients with confirmed tuberculosis were also identified. No cross-reactivity was detected with NTM specimens (n = 31). The detection limit of the assay is 10 M. tuberculosis bacilli, as determined by endpoint dilution analysis. In conclusion, an optimized DNA extraction protocol coupled with a novel multiprobe multiplex real-time PCR for the direct detection of M. tuberculosis, including Beijing/W M. tuberculosis, was found to confer high sensitivity and specificity. The combined procedure has the potential to compensate for the drawbacks of conventional mycobacterial culture in routine clinical laboratory setting, such as the lengthy incubation period and the limitation to viable organisms. PMID:21593264

  2. Simultaneous determination of bisphenol A and bisphenol B in beverages and powdered infant formula by dispersive liquid-liquid micro-extraction and heart-cutting multidimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cunha, S C; Almeida, C; Mendes, E; Fernandes, J O

    2011-04-01

    The purpose of this study was to establish a reliable, cost-effective, fast and simple method to quantify simultaneously both bisphenol A (BPA) and bisphenol B (BPB) in liquid food matrixes such as canned beverages (soft drinks and beers) and powdered infant formula using dispersive liquid-liquid micro-extraction (DLLME) with in-situ derivatisation coupled with heart-cutting gas chromatography-mass spectrometry (GC-MS). For the optimisation of the DLLME procedure different amounts of various extractive and dispersive solvents as well as different amounts of the derivative reagent were compared for their effects on extraction efficiency and yields. The optimised procedure consisted of the injection of a mixture containing tetrachloroethylene (extractant), acetonitrile (dispersant) and acetic anhydride (derivatising reagent) directly into an aliquot of beverage samples or into an aqueous extract of powdered milk samples obtained after a pretreatment of the samples. Given the compatibility of the solvents used, and the low volumes involved, the procedure was easily associated with GC-MS end-point determination, which was accomplished by means of an accurate GC dual column (heart-cutting) technique. Careful optimisation of heart-cutting GC-MS conditions, namely pressure of front and auxiliary inlets, have resulted in a good analytical performance. The linearity of the matrix-matched calibration curves was acceptable, with coefficients of determination (r2) always higher than 0.99. Average recoveries of the BPA and BPB spiked at two concentration levels into beverages and powdered infant formula ranged from 68% to 114% and the relative standard deviation (RSD) was market.

  3. Multiplex PCR for the simultaneous identification and detection of Meloidogyne incognita, M. enterolobii, and M. javanica using DNA extracted directly from individual galls.

    Science.gov (United States)

    Hu, M X; Zhuo, K; Liao, J L

    2011-11-01

    Meloidogyne incognita, M. enterolobii, and M. javanica are the most widespread species of root-knot nematodes in South China, affecting many economically important crops, ornamental plants, and fruit trees. In this study, one pair of Meloidogyne universal primers was designed and three pairs of species-specific primers were employed successfully to rapidly detect and identify M. incognita, M. enterolobii, and M. javanica by multiplex polymerase chain reaction (PCR) using DNA extracted from individual galls. Multiplex PCR from all M. incognita, M. enterolobii, and M. javanica isolates generated two fragments of ≈500 and 1,000, 500 and 200, and 500 and 700 bp, respectively. The 500-bp fragment is the internal positive control fragment of rDNA 28S D2/D3 resulting from the use of the universal primers. Other Meloidogyne spp. included in this study generated only one fragment of ≈500 bp in size. Using this approach, M. incognita, M. enterolobii, and M. javanica were identified and detected using DNA extracted directly from individual galls containing the Meloidogyne spp. at various stages of their life cycle. Moreover, the percentage of positive PCR amplification increased with nematode development and detection was usually easy after the late stage of the second-stage juvenile. The protocol was applied to galls from naturally infested roots and the results were found to be fast, sensitive, robust, and accurate. This present study is the first to provide a definitive diagnostic tool for M. incognita, M. enterolobii, and M. javanica using DNA extracted directly from individual galls using a one-step multiplex PCR technique.

  4. Simultaneous determination of polyether ionophores, macrolides and lincosamides in hen eggs by liquid chromatography-electrospray ionization tandem mass spectrometry using a simple solvent extraction.

    Science.gov (United States)

    Spisso, Bernardete Ferraz; Ferreira, Rosana Gomes; Pereira, Mararlene Ulberg; Monteiro, Mychelle Alves; Cruz, Tatiana Ávila; da Costa, Rafaela Pinto; Lima, Adélia Mara Belém; da Nóbrega, Armi Wanderley

    2010-12-03

    A liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method was developed and validated for the determination of residues of 6 polyether ionophores (lasalocid, maduramicin, monensin, narasin, salinomycin, semduramicin), 3 macrolides (erythromycin, tylosin, clarithromycin) and 1 lincosamide (lincomycin) in eggs. Nigericin was used as qualitative internal standard. Samples were deproteinizated/extracted with acetonitrile without pH adjustments. Aliquots of the extracts were evaporated and reconstituted for injection in the instrument operated in positive multiple reaction monitoring (MRM) mode. The stability of the antibiotics and the intensity of the formed ions were considered in order to select a suitable solvent for the reconstitution of the obtained dry extracts. No clean-up steps were required and matrix effects were controlled by sample dilution, selection of appropriate chromatographic conditions and reduced injection volume. Good within-laboratory reproducibility was obtained, with relative standard deviations (RSD(R)) from 4.0 (semduramicin at 5 μgkg(-1)) to 18.6 (erythromycin at 25 μgkg(-1)) for the ionophores and macrolides. Lincomycin showed the least precise results, with a maximum RSD(R) of 20.2% at 75 μgkg(-1)). Satisfactory decision limits (CCα) and detection capabilities (CCβ) were also attained. Method limits of detection (LODs) from 0.04 (salinomycin) to 1.6 μgkg(-1) (lincomycin) were achieved. Method limits of quantification (LOQs) were from 0.14 to 5.3 μgkg(-1) for the same drugs, respectively. All the LOQs, except that obtained for maduramicin were remarkably below the lowest validation level. The proposed method is suitable for routine application in commercial egg samples. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Genetic Variation in Nicotine Metabolism Predicts the Efficacy of Extended-Duration Transdermal Nicotine Therapy

    OpenAIRE

    Lerman, C.; Jepson, C.; Wileyto, EP; Patterson, F.; Schnoll, R; Mroziewicz, M; Benowitz, N; Tyndale, RF

    2010-01-01

    In a placebo-controlled trial, we examined the efficacy of a 6-month (“extended”) transdermal nicotine therapy vs. the 8-week (“standard”) therapy in 471 Caucasian smokers with either normal or reduced rates of nicotine metabolism as determined at pretreatment. Extended therapy was superior to standard therapy in genotypic or phenotypic reduced metabolizers (RMs) of nicotine but not in normal metabolizers (NMs). RMs of nicotine are candidates for extended transdermal nicotine therapy, whereas...

  6. GC profiles of volatile constituents from human urine obtained by closed loop stripping, purge and trap technique and simultaneous stem distillation-extraction.

    Science.gov (United States)

    Bestmann, H J; Haberkorn, K; Vostrowsky, O; Ferstl, R; Eggert, F

    1996-01-01

    Different techniques like "closed loop stripping" [CLSA], "purge and trap" [PTI], and continuous steam distillation extraction [SDE] were used to establish GC profiles of major histocompatibility complex-associated volatile constituents of human urine and statistically evaluated for reliability. Of the three methods investigated, PTI appeared to be superior for the detection of very volatile substances, whereas SDE was the most efficient one with respect to yield. A number of short to medium-chain ketones, 4-hydroxy-3-methoxy-styrene, menthol and nicotine were identified in preliminary analyses.

  7. LC-MS/MS method for simultaneous determination of flavonoids and physalins in rat plasma: Application to pharmacokinetic study after oral administration of Physalis alkekengi var. franchetii (Chinese lantern) extract.

    Science.gov (United States)

    Guo, Yaqing; Liu, Hongxia; Ding, Liqin; Oppong, Mahmood; Pan, Guixiang; Qiu, Feng

    2017-10-01

    A rapid and sensitive liquid chromatography with tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous determination of luteolin, luteolin-7-O-β-D-glucopyranoside, physalin A, physalin D and physalin L in rat plasma. Scutellarein and dexamethasone were used as the internal standards (IS). Plasma samples were prepared by liquid-liquid extraction with ethyl acetate. The five constituents were separated on an Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm). A gradient elution procedure was used with acetonitrile (A)-0.1% aqueous formic acid (B). Mass spectrometric detection was performed in negative ion multiple reaction monitoring mode with an electrospray ionization (ESI) source. This method showed good linearity (r2  > 0.997) over a concentration range of 2.0-500 ng/mL with a lower limit of quantification of 2.0 ng/mL for all five compounds. The inter- and intra-day accuracy ranged from 91.7 to 104%, and precisions (RSD) were extraction recoveries of all analytes were >85%. This validated method was successfully applied for the first time to the pharmacokinetic study of five ingredients after oral administration of 70% ethanol extract of Chinese lantern in rats. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

    Science.gov (United States)

    Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

    2016-10-01

    A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

  9. Ultra high performance liquid chromatography with mass spectrometry method for the simultaneous determination of phenolic constituents in honey from various floral sources using multiwalled carbon nanotubes as extraction sorbents.

    Science.gov (United States)

    Wabaidur, Saikh Mohammad; Ahmed, Yacine Badjah Hadj; Alothman, Zeid Abdullah; Obbed, Munir Saeed; AL-Harbi, Nasser Mohamed; AL-Turki, Turki Mohammad

    2015-08-01

    An ultra high performance liquid chromatography with mass spectrometry method has been developed for the simultaneous separation, identification and determination of 22 phenolic constituents in honey from various floral sources from Yemen. Solid-phase extraction was used for extraction of the target phenolic constituents from honey samples, while multiwalled carbon nanotubes were used as solid-phase adsorbent. The chromatographic separation of all phenolic constituents was performed on a BEH C18 column using a linear gradient elution with a binary mobile phase mixture of aqueous 0.1% formic acid and methanol. The quantitation was carried out in selected ion reaction monitoring acquisition mode. The total amount of phenolic acids, flavonoids and other phenols in each analyzed honey was found in the range of 338-3312, 122-5482 and 2.4-1342 μg/100 g of honey, respectively. 4-Hydroxybenzoic acid was found to be the major phenolic acid. The main detected flavonoid was chrysin, while cinnamic acid was found to be the major other phenol compound. The regeneration of solid phase adsorbent to be reused and recovery results confirm that the proposed method could be potentially used for the routine analysis of phenolic constituents in honey extract. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. An UPLC-MS/MS method for simultaneous quantitation of two coumarins and two flavonoids in rat plasma and its application to a pharmacokinetic study of Wikstroemia indica extract.

    Science.gov (United States)

    Wei, Lan; Wang, Xiaobo; Zhang, Peng; Sun, Yangyang; Jia, Lili; Zhao, Jingxin; Dong, Shikai; Sun, Lixin

    2016-01-01

    In this study, an ultra performance liquid chromatography tandem mass spectrometry method (UPLC-MS/MS) was developed for simultaneous determination of umbelliferone, apigenin, daphnoretin and genkwanin in total (free and conjugated) forms in rat plasma using psoralen as internal standard. Plasma samples were protein precipitated with acetonitrile followed by liquid-liquid extracted with ethyl acetate. Four ingredients were separated on an Acquity UPLC(®) BEH C18 column using gradient elution with the mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile, and detected by positive ion electrospray ionization (ESI) in multiple reaction monitoring mode (MRM). The method was linear for all analytes over investigated ranges with all correlation coefficients greater than 0.99. The validated lower limit of quantification was 3ng/mL for umbelliferone, 3ng/mL for apigenin, 12ng/mL for daphnoretin and 2ng/mL for genkwanin, respectively. Intra- and inter-day precisions (RSD%) were less than 15% and accuracy (RE%) ranged from -1.1% to 15%. The mean absolute extraction recoveries of analytes and IS from rat plasma were all more than 75%. The validated method was firstly and successfully applied to investigate the pharmacokinetics of four chemical ingredients after oral administration of Wikstroemia indica extract (WIE) to rats. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Validated UPLC-MS/MS method for simultaneous quantification of eight saikosaponins in rat plasma: Application to a comparative pharmacokinetic study in depression rats after oral administration of extracts of raw and vinegar-baked Bupleuri Radix.

    Science.gov (United States)

    Lei, Tianli; Zhang, Dandan; Guo, Kun; Li, Mingxiao; Lv, Chongning; Wang, Jing; Jia, Lingyun; Lu, Jincai

    2017-08-15

    A sensitive and efficient UPLC-MS/MS method was developed and validated for simultaneous quantification of eight saikosaponins (SSa, SSb1, SSb2, SSb3, SSb4, SSc, SSd and SSf) in rat plasma. Furthermore, comparative pharmacokinetic profiles of these sakosaponins were investigated, following oral administration of extracts of raw and vinegar-baked Bupleuri Radix to depression rats. Biosamples were processed with liquid-liquid extraction technique using ethyl acetate. Chromatographic separation was accomplished on Waters BEH C18 UPLC column. 0.05% formic acid in water and acetonitrile as mobile phase was used at a flow rate of 0.40mL/min. The analytes and internal standard, digoxin, were detected using negative ion electrospray ionization in multiple reaction monitoring mode. The lower limit of quantification was less than 0.62ng/mL for the each analyte. The validation parameters investigated, which were specificity, precision, accuracy, matrix effect, recovery and stability, were well within acceptable limits. Results showed that for some of analytes, AUC0-t and Cmax were significantly different after oral administration of extracts of raw and vinegar-baked Bupleuri Radix. Moreover, the pharmacokinetic study in pathological state could provide more useful information to guide the clinical usage of Bupleuri Radix. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Simultaneous determination of eight flavonoids in plasma using LC-MS/MS and application to a pharmacokinetic study after oral administration of Pollen Typhae extract to rats.

    Science.gov (United States)

    Yu, Xie-An; Azietaku, John Teye; Li, Jin; Cao, Jun; An, Mingrui; He, Jun; Gao, Xiu-Mei; Chang, Yan-Xu

    2017-02-15

    A sensitive, reliable and validated LC-MS/MS method was developed to determine the presence of eight flavonoids (catechin, typhaneoside, isorhamnetin-3-O-neohesperidoside, astragalin, isorhamnetin-3-O-β-d-glucoside, naringenin, kaempferol and isorhamnetin) in rat plasma. Puerarin was selected as the internal standard. Precipitation of the protein method with acetonitrile was used to extract these flavonoids from the rat plasma samples. The analysis was carried out on an Eclipse plus C18 column (4.6 mm×100mm, 1.8μm) when acetonitrile and formic acid aqueous solution (0.1%) was used as the mobile phase at a flow rate of 0.3mLmin-1. A tandem mass spectrometer having an electrospray ionization (ESI) source was used to detect eight flavonoids using multiple reaction monitoring (MRM) in the negative ionization mode. The LLOQs for catechin, typhaneoside, isorhamnetin-3-O-neohesperidoside, astragalin, isorhamnetin-3-O-β-d-glucoside, naringenin, kaempferol and isorhamnetin are 4, 4, 4, 0.8, 1, 0.4, 2 and 0.2ngmL-1, respectively. The precision, accuracy and recovery were all within acceptable limits and the analytes were stable in plasma for all conditions tested. The method was successfully applied to pharmacokinetic study of four flavonoids in rat plasma after administering Pollen Typhae extract orally to rats. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Comparison of different extraction methods for simultaneous determination of B complex vitamins in nutritional yeast using LC/MS-TOF and stable isotope dilution assay.

    Science.gov (United States)

    Hälvin, Kristel; Paalme, Toomas; Nisamedtinov, Ildar

    2013-02-01

    The application of LC/MS-TOF method combined with stable isotope dilution assay was studied for determination of thiamine, riboflavin, nicotinamide, nicotinic acid, pantothenic acid, pyridoxal, and pyridoxine in food. Nutritional yeast powder was used as a model food matrix. Acid extraction was compared with various enzymatic treatments in ammonium formate buffer to find a suitable method for the conversion of more complex vitamers into the same forms as the used isotope-labeled internal standards. The enzyme preparations α-amylase, takadiastase, β-glucosidase, and acid phosphatase were all able to liberate thiamine and riboflavin. The diastatic enzyme preparations α-amylase and takadiastase also expressed proteolytic side activities resulting in the formation of small peptides which interfered with the mass spectra of thiamine and riboflavin. Liberation of nicotinamide and pantothenic acid from NAD(+) and CoA, respectively, could not be achieved with any of the studied enzyme preparations. Hydrochloric acid extraction at 121 °C for 30 min was found to be destructive to pantothenic acid, but increased the liberation of pyridoxal.

  14. Sample Preparation of Eggs From Laying Hens Using QuEChERS Dispersive Extraction for the Simultaneous Determination of Melamine and Cyromazine Residues by HPLC-DAD

    Science.gov (United States)

    Tsartsali, Niki; Samanidou, Victoria F.

    2015-01-01

    A quick, easy, cheap, effective, rugged, and safe (QuEChERS) dispersive extraction method is proposed herein for the isolation and cleanup of melamine and cyromazine from chicken egg yolk. Analytes are determined by high-performance liquid chromatography using photodiode array detector after separation on a LiChroCART® (250 × 4 mm)—LiChrospher® RP-8e, 5 μm analytical column using a mobile phase of 0.1% trifluoracetic acid and methanol (80:20 v/v) delivered isocratically at a flow rate of 1 mL/minute. Extraction of isolated compounds was achieved by methanol and acetonitrile mixture (1:1 v/v). Recovery rates ranged between 74.5% and 115.8%. The method was validated in terms of 657/2002/EC decision. The within-laboratory reproducibility, expressed as a relative standard deviation, was <11%. Decision limits (CCalfa) were 2.56 mg/kg for melamine and 0.22 mg/kg−1 for cyromazine, and the corresponding results for detection capability (CCbeta) were 2.8 mg/kg for melamine and 0.24 mg/kg for cyromazine. Ruggedness was estimated according to the Youden approach studying egg yolk mass, sorbent mass, centrifugation time, organic solvents volume, evaporation temperature, and vortex time. PMID:26715832

  15. [Simultaneous determination of sixteen perfluorinated organic compounds in surface water by solid phase extraction and ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Ming; Tang, Fangliang; Yu, Yayun; Chen, Feng; Xu, Jianfen; Ye, Yonggen

    2014-05-01

    A high-throughput detection method has been developed for the determination of sixteen perfluorinated organic compounds (PFCs) in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI-MS/MS). The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLC BEH C18 column utilizing a gradient elution program of methanol (containing 2 mmol/L ammonium acetate) and water (containing 2 mmol/L ammonium acetate) as the mobile phases at a flow rate of 0.4 mL/min. The MS/MS detection was performed under negative electrospray ionization ( ESI ) in multiple reaction monitoring (MRM) mode. Good linearities were observed in the range of 0.5-100 gg/L or 1.0 - 100 microg/L with correlation coefficients from 0.998 7 to 0.999 9. The limits of detection (LODs) for the sixteen perfluorinated organic compounds were in the range of 0.06-0.46 ng/L. The recoveries ranged from 67.6% to 103% with the relative standard deviations between 2.94% and 12.0%. This method was characterized by high sensitivity and precision, extensive range and high speed, and can be applied for the analysis of PFC contaminants in surface water.

  16. On-line solid phase extraction using ion-pair microparticles combined with ICP-OES for the simultaneous preconcentration and determination of uranium and thorium

    Energy Technology Data Exchange (ETDEWEB)

    Yousefi, Seyed Reza; Zolfonoun, Ehsan [Nuclear Science and Technology Research Institute, Tehran (Iran, Islamic Republic of). NFCRS

    2016-07-01

    In this work, after on-line and in-situ solid phase extraction technique was used for the extraction and preconcentration of uranium and thorium from aqueous samples prior to inductively coupled plasma optical emission spectrometry (ICP-OES) determination. In this method, sodium hexafluorophosphate (as an ion-pairing agent) was added to the sample solution containing the cationic surfactant (dodecyltrimethylammonium bromide) and the complexing agent (dibenzoylmethane). A cloudy solution was formed as a result of formation of an ion pair between surfactant and hexafluorophosphate. The solid microparticles were passed through a microcolumn filter and the adsorbed microparticles were subsequently eluted with acid, which was directly introduced into the ICP-OES nebulizer. The main variables affecting the pre-concentration and determination steps of uranium and thorium were studied and optimized. Under the optimum conditions, the enhancement factors of 97 and 95 and the detection limits of 0.52 and 0.21 μg L{sup -1} were obtained for uranium and thorium, respectively.

  17. Rapid selective accelerated solvent extraction and simultaneous determination of herbicide atrazine and its metabolites in fruit by ultra high performance liquid chromatography.

    Science.gov (United States)

    Jia, Licong; Su, Ming; Wu, Xingqiang; Sun, Hanwen

    2016-12-01

    A selective accelerated solvent extraction procedure achieved one step extraction and cleanup for analysis of herbicide atrazine and its metabolites in fruit. Using a BEH C18 analytical column and the gradient mode with 2 mM ammonium acetate aqueous solution/acetonitrile as a mobile phase achieved effective chromatographic separation of the five analytes within 4 min. The calibration curves were linear over two orders of magnitude of concentration with correlation coefficients (r) of 0.9996-0.9999. The method limit of quantification was 1, 2, 1.5, 3, and 2 μg/kg for atrazine, desethylatrazine, desisopropylatrazine, desethyldesisopropylatrazine, and hydroxyatrazine, respectively, in the case of atrazine it is at least two orders of magnitude lower than the maximum residue limit (0.25 mg/kg). The intra-day and inter-day precisions of the five analytes were in the range of 2.1-3.5 and 3.1-4.8 %, respectively. The recoveries of the five analytes at three spiked levels varied from 85.9 to 107% with a relative standard deviation of 1.8-4.9% for pear and apple samples. The ultra high performance liquid chromatography with diode array detection method was proved to be fast, inexpensive, selective, sensitive, and accurate for the quantification of the analytes in pear and apple samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Pharmacokinetics of 2 Formulations of Transdermal Fentanyl in Cynomolgus Macaques (Macaca fascicularis)

    Science.gov (United States)

    Carlson, Amy M; Kelly, Richard; Fetterer, David P; Rico, Pedro J; Bailey, Emily J

    2016-01-01

    Fentanyl is a μ-opioid agonist that often is used as the analgesic component for balanced anesthesia in both human and veterinary patients. Minimal information has been published regarding appropriate dosing, and the pharmacokinetics of fentanyl are unknown in NHP. The pharmacokinetic properties of 2 transdermal fentanyl delivery methods, a solution (2.6 and 1.95 mg/kg) and a patch (25 µg/h), were determined when applied topically to the dorsal scapular area of cynomolgus macaques (Macaca fascicularis). Serum fentanyl concentrations were analyzed by using liquid chromatography–mass spectrometry. Compared with the patch, the transdermal fentanyl solution generated higher drug concentrations over longer time. Adverse reactions occurred in the macaques that received the transdermal fentanyl solution at 2.6 mg/kg. Both preparations showed significant interanimal variability in the maximal serum drug levels, time to achieve maximal fentanyl levels, elimination half-life, and AUC values. Both the maximal concentration and the time at which this concentration occurred were increased in macaques compared with most other species after application of the transdermal fentanyl patch and compared with dogs after application of the transdermal fentanyl solution. The pharmacokinetic properties of transdermal fentanyl in macaques are markedly different from those in other veterinary species and preclude its use as a long-acting analgesic drug in NHP. PMID:27423151

  19. Optimization and Characterization of Chitosan Films for Transdermal Delivery of Ondansetron

    Directory of Open Access Journals (Sweden)

    Yıldız Özsoy

    2013-05-01

    Full Text Available The aim of this study was to develop novel transdermal films of ondansetron HCl with high molecular weight chitosan as matrix polymer and 2-(2-ethoxy-ethoxy ethanol (Transcutol® as plasticizer. In this context, firstly the physicochemical properties of gels used to formulate transdermal films were characterized and, physicochemical properties and bioadhesiveness of the transdermal films prepared with chitosan gels were assessed. The impact of three different types of terpenes, namely limonene, nerolidol and eucalyptol on in vitro skin permeation of ondansetron from transdermal films were also examined. ATR-FTIR measurements were performed to investigate the effects of the chitosan film formulations on in vitro conformational order of stratum corneum intercellular lipids after 24 h permeation study. The results showed that the chitosan gels consisting of Transcutol® as plasticizer and terpenes as penetration enhancer may be used to prepare transdermal films of ondansetron due to the good mechanical properties and bioadhesiveness of the transdermal films. Eucalyptol (1% showed higher permeation enhancer effect than the other terpenes and control. ATR-FTIR data confirmed that finding in which eucalyptol induced a blue shift in the both CH2 asymmetric and symmetric absorbance peak positions indicating increased lipid fluidity of stratum corneum.

  20. Transdermal drug delivery: feasibility for treatment of superficial bone stress fractures.

    Science.gov (United States)

    Aghazadeh-Habashi, Ali; Yang, Yang; Tang, Kathy; Lőbenberg, Raimar; Doschak, Michael R

    2015-12-01

    Transdermal drug delivery offers the promise of effective drug therapy at selective sites of pathology whilst reducing systemic exposure to the pharmaceutical agents in off-target organs and tissues. However, that strategy is often limited to cells comprising superficial tissues of the body (rarely to deeper bony structures) and mostly indicated with small hydrophobic pharmacological agents, such as steroid hormones and anti-inflammatory gels to skin, muscle, and joints. Nonetheless, advances in transdermal liposomal formulation have rendered the ability to readily incorporate pharmacologically active hydrophilic drug molecules and small peptide biologics into transdermal dosage forms to impart the effective delivery of those bioactive agents across the skin barrier to underlying superficial tissue structures including bone, often enhanced by some form of electrical, chemical, and mechanical facilitation. In the following review, we evaluate transdermal drug delivery systems, with a particular focus on delivering therapeutic agents to treat superficial bone pain, notably stress fractures. We further introduce and discuss several small peptide hormones active in bone (such as calcitonins and parathyroid hormone) that have shown potential for transdermal delivery, often under the added augmentation of transdermal drug delivery systems that employ lipo/hydrophilicity, electric charge, and/or microprojection facilitation across the skin barrier.

  1. Simultaneous determination and pharmacokinetic study of three flavonoid glycosides in rat plasma by LC-MS/MS after oral administration of Rubus chingii Hu extract.

    Science.gov (United States)

    Zan, Tao; Piao, Li; Wei, Yuntao; Gu, Yue; Liu, Baohua; Jiang, Daqing

    2018-03-01

    A simple and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of isoquercitrin, kaempferol-3-O-rutinoside and tiliroside in rat plasma. Plasma samples were deproteinized with methanol and separated on a Hypersil Gold C 18 column (2.1 × 50 mm, i.d., 3.0 μm) using gradient elution with the mobile phase of water and methanol at a flow rate of 0.4 mL/min. Mass spectrometric detection was performed with negative ion electrospray ionization in selected reaction monitoring mode. All analytes showed good linearity over their investigated concentration ranges (r 2  > 0.99). The lower limit of quantification was 1.0 ng/mL for isoquercitrin and 2.0 ng/mL for kaempferol-3-O-rutinoside and tiliroside, respectively. Intra- and inter-day precisions were 80.4%. The assay was successfully applied to investigate the pharmacokinetic study of the three ingredients after oral administration of Rubus chingii Hu to rats. Copyright © 2017 John Wiley & Sons, Ltd.

  2. Antioxidant Activity of Leaf Extracts from Different Hibiscus sabdariffa Accessions and Simultaneous Determination Five Major Antioxidant Compounds by LC-Q-TOF-MS

    Directory of Open Access Journals (Sweden)

    Jin Wang

    2014-12-01

    Full Text Available Hibiscus sabdariffa has gained attention for its antioxidant activity. There are many accessions of H. sabdariffa in the world. However, information on the quantification of antioxidant compounds in different accessions is rather limited. In this paper, a liquid chromatography/quadrupole-time-of-flight mass spectrometry (LC-Q-TOF-MS method for simultaneous determination of five antioxidant compounds (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, and isoquercitrin in H. sabdariffa leaves was developed. The method was validated for linearity, sensitivity, precision, repeatability and accuracy. The validated method has been successfully applied for determination of the five analytes in eight accessions of H. sabdariffa. The eight accessions of H. sabdariffa were evaluated for their antioxidant activities by DPPH free radical scavenging assay. The investigated accessions of H. sabdariffa were rich in rutin and exhibited strong antioxidant activity. The two accessions showing the highest antioxidant activities were from Cuba (No. 2 and Taiwan (No. 5. The results indicated that H. sabdariffa leaves could be considered as a potential antioxidant source for the food industry. The developed LC-Q-TOF-MS method is helpful for quality control of H. sabdariffa.

  3. Antioxidant activity of leaf extracts from different Hibiscus sabdariffa accessions and simultaneous determination five major antioxidant compounds by LC-Q-TOF-MS.

    Science.gov (United States)

    Wang, Jin; Cao, Xianshuang; Jiang, Hao; Qi, Yadong; Chin, Kit L; Yue, Yongde

    2014-12-17

    Hibiscus sabdariffa has gained attention for its antioxidant activity. There are many accessions of H. sabdariffa in the world. However, information on the quantification of antioxidant compounds in different accessions is rather limited. In this paper, a liquid chromatography/quadrupole-time-of-flight mass spectrometry (LC-Q-TOF-MS) method for simultaneous determination of five antioxidant compounds (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, and isoquercitrin) in H. sabdariffa leaves was developed. The method was validated for linearity, sensitivity, precision, repeatability and accuracy. The validated method has been successfully applied for determination of the five analytes in eight accessions of H. sabdariffa. The eight accessions of H. sabdariffa were evaluated for their antioxidant activities by DPPH free radical scavenging assay. The investigated accessions of H. sabdariffa were rich in rutin and exhibited strong antioxidant activity. The two accessions showing the highest antioxidant activities were from Cuba (No. 2) and Taiwan (No. 5). The results indicated that H. sabdariffa leaves could be considered as a potential antioxidant source for the food industry. The developed LC-Q-TOF-MS method is helpful for quality control of H. sabdariffa.

  4. A comparison of solid-phase microextraction (SPME) with simultaneous distillation-extraction (SDE) for the analysis of volatile compounds in heated beef and sheep fats.

    Science.gov (United States)

    Watkins, P J; Rose, G; Warner, R D; Dunshea, F R; Pethick, D W

    2012-06-01

    A comparison has been made on the application of SPME and SDE for the extraction of volatile compounds from heated beef and sheep fats with separation and measurement by gas chromatography-mass spectrometry. As far as we know, this report represents the first time that such a comparison has been made for the measurement of volatile compounds in heated sheep fat. Approximately 100 compounds (in relatively high abundance) were characterised in the volatile profiles of heated beef and sheep fats using both techniques. Differences were observed in the volatile profiles obtained from each technique, independent of compound class. Rather than rate one technique as superior to another, the techniques can be regarded as complementary to each other. Crown Copyright © 2011. Published by Elsevier Ltd. All rights reserved.

  5. Simultaneous Screening and Quantification of 29 Drugs of Abuse in Oral Fluid by Solid-Phase Extraction and Ultraperformance LC-MS/MS

    DEFF Research Database (Denmark)

    Linnet, Kristian; Badawi, Nora; Simonsen, Kirsten W.

    2009-01-01

    Background: The European DRUID (Driving under the Influence of Drugs, Alcohol And Medicines) project calls for analysis of oral fluid (OF) samples, collected randomly and anonymously at the roadside from drivers in Denmark throughout 2008–2009. To analyze these samples we developed an ultra...... performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) method for detection of 29 drugs and illicit compounds in OF. The drugs detected were opioids, amphetamines, cocaine, benzodiazepines, and {Delta}-9-tetrahydrocannabinol. Method: Solid-phase extraction was performed with a Gilson ASPEC XL......4 system equipped with Bond Elut Certify sample cartridges. OF samples (200 mg) diluted with 5 mL of ammonium acetate/methanol (vol/vol 90:10) buffer were applied to the columns and eluted with 3 mL of acetonitrile with aqueous ammonium hydroxide. Target drugs were quantified by use of a Waters...

  6. Simultaneous determination of eight alkaloids and oleandrin in herbal cosmetics by dispersive solid-phase extraction coupled with ultra high performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Xun, Zhiqing; Liu, Donghong; Huang, Rongrong; He, Shuang; Hu, Du; Guo, Xindong; Xian, Yanping

    2017-05-01

    We utilized ultra-high performance liquid chromatography with tandem mass spectrometry and dispersive solid-phase extraction to develop a new method for the detection of nine analytes (scopolamine, cephaeline, strychnine, hyoscyamine, brucine, hydrastine, ajmalicine, colchicine, and oleandrin) in herbal cosmetics. Acetonitrile/water and 2-propylaminoethylamine were used to disperse and purify during the dispersive solid-phase extraction step. The analytes were separated by a Waters UPLC HSS T3 column and detected through electrospray ionization source in the positive mode with multi-reaction monitoring conditions. Under the optimal conditions, the calibration curves were linear in the range of 0.2-100.0 μg/L with the correlation coefficients higher than 0.995. The method limit of quantitation (S/N = 10) were 5.0 μg/kg for oleandrin and 1.0 μg/kg for the other eight alkaloids. The mean recoveries at three spiked concentration levels of 1.0-10.0 μg/kg were in the range of 86.9-116.5% with the intra-day relative standard deviations (n = 6) ranging from 2.4 to 8.8%, and inter-day relative standard deviations ranging from 2.7 to 5.7%. This method is accurate, simple and rapid, and has been applied to the quality supervision of herbal cosmetics in Guangzhou. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Utilization of prodrugs to enhance the transdermal absorption of morphine

    DEFF Research Database (Denmark)

    Drustrup, J.; Fullerton, A.; Christrup, Lona Louring

    1991-01-01

    The feasibility of providing transdermal delivery of morphine was examined using the prodrug approach. Various alkyl esters formed at the 3- and/or 6-hydroxy group in morphine were prepared and their physico-chemical and skin penetration properties studied as well as their hydrolysis kinetics....... The esters showed generally a higher water and lipid solubility than morphine and were also much more lipophilic than the parent drug in terms of octanol-buffer partition coefficients. Diffusion experiments in vitro using human skin samples showed that whereas morphine did not penetrate the skin to any...... measurable extent whether applied in the form of saturated solutions in water at pH 7.0 or in isopropyl myristate, the ester prodrugs showed a high penetrating capacity under the same conditions. Steady-state fluxes up to 35 μg morphine/cm per h were observed. For some esters essentially all of the amounts...

  8. Enhanced transdermal delivery of salbutamol sulfate via ethosomes.

    Science.gov (United States)

    Bendas, Ehab R; Tadros, Mina I

    2007-12-14

    The main objective of the present work was to compare the transdermal delivery of salbutamol sulfate (SS), a hydrophilic drug used as a bronchodilator, from ethosomes and classic liposomes containing different cholesterol and dicetylphosphate concentrations. All the systems were characterized for shape, particle size, and entrapment efficiency percentage, by image analysis optical microscopy or transmission electron microscopy, laser diffraction, and ultracentrifugation, respectively. In vitro drug permeation via a synthetic semipermeable membrane or skin from newborn mice was studied in Franz diffusion cells. The selected systems were incorporated into Pluronic F 127 gels and evaluated for both drug permeation and mice skin deposition. In all systems, the presence of spherical-shaped vesicles was predominant. The vesicle size was significantly decreased (P ethosomal systems were much more efficient at delivering SS into mice skin (in terms of quantity and depth) than were liposomes or aqueous or hydroalcoholic solutions.

  9. Hemicrania Continua-Like Headache Related to Transdermal Nitroglycerine Therapy.

    Science.gov (United States)

    Mainardi, Federico; Zanchin, Giorgio; Maggioni, Ferdinando

    2017-03-01

    Several cases of symptomatic hemicrania continua (HC) have been reported. A 66-year-old man, suffering from migraine without aura, presented with a four month history of a new headache fulfilling the ICHD 3beta clinical criteria for HC. HC onset was strictly related to the use of transdermal nitroglycerine patch (TNP). In agreement with the cardiologist, TNP was discontinued and the headache promptly disappeared; symptoms reappeared within 6-12 hours after nitroglycerine reintroduction. After permanent discontinuation of TNP, headache disappeared at one year follow-up. To the best of our knowledge, this is the first report of the occurrence of an HC-like headache related to TNP. © 2016 American Headache Society.

  10. Dissolving microneedles for transdermal drug delivery: Advances and challenges.

    Science.gov (United States)

    Ita, Kevin

    2017-09-01

    Over the last number of years, a significant body of evidence has shown the benefit of using dissolving microneedles (DMNs) for transdermal drug delivery. These devices are prepared from a wide range of materials such as sugars and polymers. DMNs are mainly fabricated by micromolding, photopolymerization, drawing lithography and droplet-airborne blowing. In this review, we have focused on the advances made in the field in recent years using a representative set of studies. Although the list of studies is not exhaustive, they highlight the challenges encountered such as the need to increase mechanical strength as well as medication dose while ensuring fast release of the active ingredient. DMNs can be used to delivery low molecular drugs as well as peptides, proteins and other high molecular weight compounds. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  11. Carbon nanotubes buckypapers for potential transdermal drug delivery

    Energy Technology Data Exchange (ETDEWEB)

    Schwengber, Alex [PINMATE-Departamento de Industrias, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, C1428EGA Buenos Aires (Argentina); Prado, Héctor J. [PINMATE-Departamento de Industrias, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, C1428EGA Buenos Aires (Argentina); Cátedra de Tecnología Farmacéutica II, Departamento de Tecnología Farmacéutica, Facultad de Farmacia y Bioquímica, Universidad de Buenos Aires, Junín 956, C1113AAD Buenos Aires (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Zilli, Darío A. [PINMATE-Departamento de Industrias, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, C1428EGA Buenos Aires (Argentina); Bonelli, Pablo R. [PINMATE-Departamento de Industrias, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires, Ciudad Universitaria, C1428EGA Buenos Aires (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); and others

    2015-12-01

    Drug loaded buckypapers based on different types of carbon nanotubes (CNTs) were prepared and characterized in order to evaluate their potentialities for the design of novel transdermal drug delivery systems. Lab-synthesized CNTs as well as commercial samples were employed. Clonidine hydrochloride was used as model drug, and the influence of composition of the drug loaded buckypapers and processing variables on in vitro release profiles was investigated. To examine the influence of the drug nature the evaluation was further extended to buckypapers prepared with flurbiprofen and one type of CNTs, their selection being based on the results obtained with the former drug. Scanning electronic microscopy images indicated that the model drugs were finely dispersed on the CNTs. Differential scanning calorimetry, and X-ray diffraction pointed to an amorphous state of both drugs in the buckypapers. A higher degree of CNT–drug superficial interactions resulted in a slower release of the drug. These interactions were in turn affected by the type of CNTs employed (single wall or multiwall CNTs), their functionalization with hydroxyl or carboxyl groups, the chemical structure of the drug, and the CNT:drug mass ratio. Furthermore, the application of a second layer of drug free CNTs on the loaded buckypaper, led to decelerate the drug release and to reduce the burst effect. - Highlights: • Drug loaded buckypapers from carbon nanotubes were prepared and characterized. • Their potentialities for transdermal drug delivery applications were evaluated. • Characteristics of carbon nanotubes and the structure of the drug affected release • A higher carbon nanotube:drug mass ratio decelerated release • Up to one week controlled release profiles were obtained for the drug flurbiprofen.

  12. Enhanced Controlled Transdermal Delivery of Ambroxol from the EVA Matrix

    Science.gov (United States)

    Cho, C. W.; Kim, D. B.; Cho, H. W.; Shin, S. C.

    2012-01-01

    To avoid the systemic adverse effects that might occur after oral administration, transdermal delivery of ambroxol was studied as a method for maintaining proper blood levels for an extended period. Release of ambroxol according to concentration and temperature was determined, and permeation of drug through rat skin was studied using two chamber-diffusion cells. The solubility according to PEG 400 volume fraction was highest at 40% PEG 400. The rate of drug release from the EVA matrix increased with increased temperature and drug loading doses. A linear relationship existed between the release rate and the square root of loading rate. The activation energy (Ea) was measured from the slope of the plot of log P versus 1000/T and was found to be 10.71, 10.39, 10.33 and 9.87 kcal/mol for 2, 3, 4 and 5% loading dose from the EVA matrix, respectively. To increase the permeation rate of ambroxol across rat skin from the EVA matrix, various penetration enhancers such as fatty acids (saturated, unsaturated), propylene glycols, glycerides, pyrrolidones, and non-ionic surfactants were used. The enhancing effects of the incorporated enhancers on the skin permeation of ambroxol were evaluated using Franz diffusion cells fitted with intact excised rat skin at 37° using 40% PEG 400 solution as a receptor medium. Among the enhancers used, polyoxyethylene-2-oleyl ether increased the permeation rate by 4.25-fold. In conclusion, EVA matrix containing plasticizer and permeation enhancer could be developed for enhanced transdermal delivery of ambroxol. PMID:23325993

  13. Simultaneous pressurized enzymatic hydrolysis extraction and clean up for arsenic speciation in seafood samples before high performance liquid chromatography-inductively coupled plasma-mass spectrometry determination.

    Science.gov (United States)

    Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; Moreda-Piñeiro, Antonio; Moscoso-Pérez, Carmen; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío; Bermejo-Barrera, Pilar

    2010-10-29

    The feasibility of pressurized conditions to assist enzymatic hydrolysis of seafood tissues for arsenic speciation was novelty studied. A simultaneous in situ (in cell) clean-up procedure was also optimized, which speeds up the whole sample treatment. Arsenic species (As(III), MMA, DMA, As(V), AsB and AsC) were released from dried seafood tissues using pepsin as a protease, and the arsenic species were separated/quantified by anion exchange high performance liquid chromatography (HPLC) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). Variables inherent to the enzymatic activity (pH, temperature and ionic strength), the amount of enzyme (pepsin), and factors affecting pressurization (pressure, static time, number of cycles and amount of dispersing agent, C-18) were fully evaluated. Pressurized assisted enzymatic hydrolysis (PAEH) with pepsin can be finished after few minutes (two cycles of 2 min each one plus 3 min to reach the hydrolysis temperature of 50 °C). A total sample solubilisation is not achieved after the procedure, however it is efficient enough for breaking down certain bonds of bio-molecules and for releasing arsenic species. The developed method has been found to be precise (RSDs lower than 6% for As(III), DMA and As(V); and 3% for AsB) and sensitive (LOQs of 18.1, 36.2, 35.7, 28.6, 20.6 and 22.5 ng/g for As(III), MMA, DMA, As(V), AsB and AsC, respectively). The optimized methodology was successfully applied to different certified reference materials (DORM-2 and BCR 627) which offer certified AsB and DMA contents, and also to different seafood products (mollusks, white fishes and cold water fishes). Copyright © 2010 Elsevier B.V. All rights reserved.

  14. Rapid and simple method by combining FTA™ card DNA extraction with two set multiplex PCR for simultaneous detection of non-O157 Shiga toxin-producing Escherichia coli strains and virulence genes in food samples.

    Science.gov (United States)

    Kim, S A; Park, S H; Lee, S I; Ricke, S C

    2017-12-01

    The aim of this research was to optimize two multiplex polymerase chain reaction (PCR) assays that could simultaneously detect six non-O157 Shiga toxin-producing Escherichia coli (STEC) as well as the three virulence genes. We also investigated the potential of combining the FTA™ card-based DNA extraction with the multiplex PCR assays. Two multiplex PCR assays were optimized using six primer pairs for each non-O157 STEC serogroup and three primer pairs for virulence genes respectively. Each STEC strain specific primer pair only amplified 155, 238, 321, 438, 587 and 750 bp product for O26, O45, O103, O111, O121 and O145 respectively. Three virulence genes were successfully multiplexed: 375 bp for eae, 655 bp for stx1 and 477 bp for stx2. When two multiplex PCR assays were validated with ground beef samples, distinctive bands were also successfully produced. Since the two multiplex PCR examined here can be conducted under the same PCR conditions, the six non-O157 STEC and their virulence genes could be concurrently detected with one run on the thermocycler. In addition, all bands clearly appeared to be amplified by FTA card DNA extraction in the multiplex PCR assay from the ground beef sample, suggesting that an FTA card could be a viable sampling approach for rapid and simple DNA extraction to reduce time and labour and therefore may have practical use for the food industry. Two multiplex polymerase chain reaction (PCR) assays were optimized for discrimination of six non-O157 Shiga toxin-producing Escherichia coli (STEC) and identification of their major virulence genes within a single reaction, simultaneously. This study also determined the successful ability of the FTA™ card as an alternative to commercial DNA extraction method for conducting multiplex STEC PCR assays. The FTA™ card combined with multiplex PCR holds promise for the food industry by offering a simple and rapid DNA sample method for reducing time, cost and labour for detection of STEC in

  15. Magnetic solid-phase extraction using nanoporous three dimensional graphene hybrid materials for high-capacity enrichment and simultaneous detection of nine bisphenol analogs from water sample.

    Science.gov (United States)

    Wang, Lingling; Zhang, Zhenzhen; Zhang, Jing; Zhang, Lei

    2016-09-09

    The synthesis of a magnetic nanoporous three dimensional graphene (3DG)/ZnFe2O4 composite has been achieved. Through formation of graphene hydrogel, ZnFe2O4 magnetic particles was successfully introduced into the nanoporous 3DG, resulting in a magnetic porous carbon material. The morphology, structure, and magnetic behavior of the as-prepared 3DG/ZnFe2O4 were characterized by using the techniques of SEM, XRD, BET, VSM, FTIR, Raman and TGA. The 3DG/ZnFe2O4 has a high specific surface area and super paramagnetism. Its performance was evaluated by the magnetic solid-phase extraction of nine bisphenol analogs (BPs) from water samples followed by HPLC analysis, and showed excellent adsorption capability for the nine target compounds. Under optimized condition, the lower method detection limits (0.05-0.18ngmL(-1)), the higher enrichment factors (800 fold) and good recoveries (95.1-103.8%) with relative standard deviation (RSD) values less than 6.2% were achieved. The results indicated that the developed method based on the use of 3DG/ZnFe2O4 as the magnetic adsorbent has the advantages of convenience and high efficiency, and can be successfully applied to detect the nine BPs in real water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Simultaneous determination of three active components in rat plasma by UPLC-MS/MS: Application to pharmacokinetic study after oral administration of Herba Sarcandrae extract.

    Science.gov (United States)

    Zhang, Bin; Chen, Jianguo; Jiang, Qichuan; Wang, Xuefeng; Lu, Yan; Gong, Liang; Chen, Dong

    2017-04-01

    A rapid, specific and sensitive ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for determination of isofraxidin, rosmarinic acid and kaempferol-3-O-glucuronide in rat plasma using warfarin as an internal standard (IS). Separation was conducted on a Thermo Hypersil GOLD C18 column with linear gradient elution using methanol and water. Mass spectrometric detection was conducted using selected reaction monitoring (SRM) via an electrospray ionization (ESI) source. All analytes exhibited good linearity within their concentration ranges (r > 0.9990). The lower limits of quantitations of isofraxidin, rosmarinic acid, and kaempferol-3-O-glucuronide were 1.31, 0.67 and 0.92 ng/mL, respectively. Intra- and inter-day precisions of these investigated components exhibited an RSD within 11.7%, and the accuracy ranged from -12.5 to 15.0% at all QC levels. The developed method was successfully applied to a pharmacokinetic study of isofraxidin, rosmarinic acid, and kaempferol-3-O-glucuronide in rats after oral administration of Herba Sarcandrae Extract. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Simultaneous quantification of cortisol and cortisone in urines from infants with packed-fiber solid-phase extraction coupled to HPLC-MS/MS.

    Science.gov (United States)

    Li, Chen; Zhang, Zhao; Liu, Xiongwei; Shen, Kangwei; Gu, Pan; Kang, Xuejun

    2017-09-01

    Cortisol and cortisone are two important glucocorticoids in human body, their interconversion is controlled by two isotypes of 11β-hydroxy steroid dehydrogenase (11β-HSD1 and 11β-HSD2). The ratio of urinary cortisol to cortisone can be used to assess the activity of 11β-HSDs. An analytical method to quantify urinary cortisol and cortisone using high performance liquid chromatographic tandem mass spectrometry following a packed-fiber solid-phase extraction (PFSPE) was developed. The proposed method was validated and applied to determine the urinary cortisol and cortisone concentrations in infants. Linearity was observed in the range of 0.6-150ng/mL for cortisol and 0.8-200ng/mL for cortisone. The intra-day RSD was 2.4-4.5% for cortisol and 3.3-6.2% for cortisone. Inter-day RSD was 3.7-6.6% for cortisol and 4.3-8.2% for cortisone. The recovery was 97.8±4.6% for cortisol and 98.9±4.4% for cortisone. The established method is simple and efficient for the quantification of urinary cortisol and cortisone and for indirectly assessing the activity of 11β-hydroxy steroid dehydrogenase. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Simultaneous determination of caffeine, theophylline and theobromine in human plasma by on-line solid-phase extraction coupled to reversed-phase chromatography.

    Science.gov (United States)

    Emara, Samy

    2004-10-01

    A reversed-phase liquid chromatographic column switching system was described for the determination of caffeine (CF), theophylline (TH) and theobromine (TB) in human plasma with a direct injection procedure. A short protein-coated mu Bondapak CN silica pre-column (20 x 3 mm, i.d.) was used for enrichment of the drugs and clean up from weakly retained plasma components using phosphate buffer saline pH 7.4. After washing step, the retained drugs were flushed into a reversed-phase column (5 microm TSK gel ODS-80 TM, 150 x 4.6 mm i.d.) with a mobile phase of methanol-0.01 M phosphate buffer, pH 3.5 (30:70, v/v) for the final separation. The eluent was monitored with a UV detector at 275 nm. The resulting chromatograms showed no interference from endogenous plasma components. A linear relationship between the concentration of drug and peak height was confirmed in the range of 0.5-20 microg/mL for all drugs. High extraction recoveries from plasma ranging from 96.12 to 100.32% were achieved. Validation of the method was examined performing intra- and inter-day accuracy and precision and was found to be satisfactory. The coefficients of variation of the three drugs were less than 3% for intra-day and less than 4% for inter-day run assays.

  19. Simultaneous determination of 14 sulfonamides and tetracyclines in biogas plants by liquid-liquid-extraction and liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Spielmeyer, Astrid; Ahlborn, Jenny; Hamscher, Gerd

    2014-04-01

    A new method for the analysis of sulfonamides and tetracyclines in heterogenic biogas plant input samples and fermentation residues is introduced. Veterinary antibiotics are only partially absorbed in the animal gut; therefore, animal manure can contain high loads of these substances. Animal manure is used for biogas generation, so antibiotics can enter the anaerobic fermentation process this way. However, only little is known about the fate of antibiotics within this process, also due to the lack of suitable analytical methods for this complex sample matrix. Therefore, we developed a method for the analysis of ten sulfonamides (sulfachloropyridazine, sulfadiazine, sulfadimethoxine, sulfaguanidine, sulfamerazine, sulfamethazine, sulfamethoxazol, sulfamethoxypyridazin, sulfapyridine, sulfathiazole) and four tetracyclines (chlortetracycline, doxycycline, oxytetracycline, tetracycline) in biogas plant input and output samples, including a single liquid-liquid-extraction step and analysis via liquid chromatography (LC) and triple quadrupole mass spectrometry. The detection limit of this method ranges from 0.01 to 0.08 mg kg(-1). Matrix calibration using antibiotic-free cattle feces and isotopic-labeled internal standards enables quantification of antibiotics in different matrices such as animal manure, dung, or fermenter outputs with recovery rates between 70 and 130 %. This makes the method suitable for investigating the fate of antibiotics in animal manure and fermentation processes. A screening of 15 German biogas plants revealed the presence of several antibiotics up to 9 mg kg(-1) (201 mg kg(-1) dry matter). During the fermentation process, elimination occurs; however, with the exception of chlortetracycline, the antibiotic content remains in the same order of magnitude.

  20. Developing a Commercial Air Ultrasonic Ceramic Transducer to Transdermal Insulin Delivery.

    Science.gov (United States)

    Jabbari, Nasrollah; Asghari, Mohammad Hossein; Ahmadian, Hassan; Mikaili, Peyman

    2015-01-01

    The application of low-frequency ultrasound for transdermal delivery of insulin is of particular public interest due to the increasing problem of diabetes. The purpose of this research was to develop an air ultrasonic ceramic transducer for transdermal insulin delivery and evaluate the possibility of applying a new portable and low-cost device for transdermal insulin delivery. Twenty-four rats were divided into four groups with six rats in each group: one control group and three experimental groups. Control group (C) did not receive any ultrasound exposure or insulin (untreated group). The second group (T1) was treated with subcutaneous insulin (Humulin(®) R, rDNA U-100, Eli Lilly and Co., Indianapolis, IN) injection (0.25 U/Kg). The third group (T2) topically received insulin, and the fourth group (T3) received insulin with ultrasound waves. All the rats were anesthetized by intraperitoneal injection of ketamin hydrochloride and xylazine hydrochloride. Blood samples were collected after anesthesia to obtain a baseline glucose level. Additional blood samples were taken every 15 min in the whole 90 min experiment. In order for comparison the changes in blood glucose levels" to " In order to compare the changes in blood glucose levels. The statistical multiple comparison (two-sided Tukey) test showed a significant difference between transdermal insulin delivery group (T2) and subcutaneous insulin injection group (T1) during 90 min experiment (P = 0.018). In addition, the difference between transdermal insulin delivery group (T2) and ultrasonic transdermal insulin delivery group (T3) was significant (P = 0.001). Results of this study demonstrated that the produced low-frequency ultrasound from this device enhanced the transdermal delivery of insulin across hairless rat skin.

  1. Simultaneous determination of three flavonoids and one coumarin by LC-MS/MS: application to a comparative pharmacokinetic study in normal and arthritic rats after oral administration of Daphne genkwa extract.

    Science.gov (United States)

    Zhou, Luyi; Li, Jing; Yan, Chong

    2018-03-03

    A selective and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for investigating the pharmacokinetics of umbelliferone, apigenin, genkwanin, and hydroxygenkwanin after oral administration of Daphne genkwa extract. Plasma samples were treated by protein precipitation with acetonitrile. Analytes were detected by triple-quadrupole MS/MS with an ESI source in negative selection reaction monitoring mode. The transitions of m/z 161→133 for umbelliferone, m/z 269→117 for apigenin, m/z 283→268 for genkwanin, and m/z 299→284 for hydroxygenkwanin were confirmed for quantification. Chromatographic separation was conducted using an Eclipse XDB-C 18 column, and the applied isocratic elution program allowed for simultaneous determination of the four analytes for a total run time of 2.5 min. The linearity was validated over the plasma concentration ranges of 1.421-1421 ng/mL for umbelliferone, 0.845-845 ng/mL for apigenin, 1.025-1025 ng/mL for genkwanin, and 0.845-845 ng/mL for hydroxygenkwanin. The extraction recovery rate was >82.7% for each analyte. No apparent matrix effect was observed during the bioanalysis. After full validation, the proposed method was successfully applied to compare the pharmacokinetics of these analytes between normal and arthritic rats. This article is protected by copyright. All rights reserved.

  2. Simultaneous determination of two plant growth regulators in ten food samples using ion chromatography combined with QuEChERS extraction method (IC-QuEChERS) and coupled with fluorescence detector.

    Science.gov (United States)

    Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Lou, Chaoyan; Liu, Junwei; Zhu, Yan

    2018-02-15

    A new simple, isocratic, selective and highly sensitive method has been developed for the simultaneous separation and determination of two plant growth regulators (PGRs): 2-(1-Naphthyl)acetic acid (NAA) and 2-(Naphthalen-1-yl)acetamide (NAD). Both PGRs were extracted by modified and miniaturized ion chromatography-Quick, Easy, Cheap, Effective, Rugged and Safe (IC-QuEChERS) method from ten food samples. The separation and sensitive determination were carried out by using ion chromatography coupled with fluorescence and ultraviolet (IC-FLD/UV) detector. The proposed analytical and extraction methods were validated by using blank samples, fortified with a standard solution of these two PGRs at three concentration levels 5, 15 and 25µg/kg. The method showed good linearity (r(2)≥0.980), satisfactory recoveries (76.3-112) with tolerable precision having relative standard deviations less than 15.4% (RSDs, n=3). The limit of detection and limit of quantification were also in the range of 0.08-6.6ng/kg and 2.2-20ng/kg, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Development of a liquid chromatography-tandem mass spectrometry with ultrasound-assisted extraction method for the simultaneous determination of sudan dyes and their metabolites in the edible tissues and eggs of food-producing animals.

    Science.gov (United States)

    Chen, Dongmei; Li, Xueqin; Tao, Yanfei; Pan, Yuanhu; Wu, Qinghua; Liu, Zhenli; Peng, Dapeng; Wang, Xu; Huang, Lingli; Wang, Yulian; Yuan, Zonghui

    2013-11-15

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of sudan I, sudan II, sudan III, sudan IV, and their metabolites such as 4-aminoazobenzene and ortho-aminoazotoluole in 12 animal derived foods (including the muscle and liver of swine, muscle, liver and skin of chicken and duck, muscle and skin of fish, as well as the eggs of hen and duck). Sample preparation procedure included ultrasound-assisted extraction with acetonitrile, defatting with n-hexane and final clean-up with solid phase extraction (SPE) on Aluminum B cartridges. The detection and quantification of the 6 sudan dyes and their metabolites were performed by a reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS). The CCαs and the CCβs of various samples varied from 0.03μg/kg to 0.12μg/kg, 0.09μg/kg to 0.19μg/kg, respectively. The recoveries of spiked sample from 0.2μg/kg to 0.8μg/kg ranged from 61.9% to 87.4% with the relative standard deviations of less than 19.1%. Performances of the whole analytical procedure meet the criteria established by the European Commission for mass spectrometric detection. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Synthesis and characterization of a novel molecularly imprinted polymer for simultaneous extraction and determination of water-soluble and fat-soluble synthetic colorants in chilli products by solid phase extraction and high performance liquid chromatography.

    Science.gov (United States)

    Long, Chaoyang; Mai, Zhibin; Yang, Yingfen; Zhu, Binghui; Xu, Xiumin; Lu, Lin; Zou, Xiaoyong

    2009-11-20

    A sorbent was synthesized and investigated for molecularly imprinted solid phase extraction (MISPE). Molecularly imprinted polymers (MIP) were synthesized via precipitation polymerization procedure, where 4-vinyl pyridine (4-VP) was used as functional monomer and ethylene glycol dimethacrylate (EDMA) as cross-linking agent. The imprinting effect of the MISPE was evaluated by elution experiments. The resulting MISPE showed high extraction selectivity to water-soluble and fat-soluble synthetic colorants. The determination of multi-residue for three kinds of water-soluble and six kinds of fat-soluble synthetic colorants in chilli products was also investigated by HPLC coupled with MISPE. The mean recoveries calculated by solvent calibration curve for water-soluble and fat-soluble synthetic colorants were from 72.1% to 95.6% for chilli spice and 72.1% to 92.3% for chilli powder. The decision limit (CCalpha) and the detection capability (CCbeta) obtained for water-soluble and fat-soluble synthetic colorants were in the range of 1.2-1.6 and 1.9-2.4 microg kg(-1) in chilli spice and chilli powder. The resulting MISPE was successfully used off-line for the determination of nine kinds of synthetic colorants in chilli products.

  5. Simultaneous determination of vitexin-2"-O-glucoside, vitexin-2"-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn (Crataegus pinnatifida Bge.) leaves by RP-HPLC with ultraviolet photodiode array detection.

    Science.gov (United States)

    Cheng, Shan; Qiu, Feng; Huang, Jia; He, Junqi

    2007-03-01

    RP-HPLC with UV photodiode array detection (UV-DAD) was developed and validated for the simultaneous determination of vitexin-2"-O-glucoside, vitexin-2"-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn (Crataegus pinnatifida Bge.) leaves. The analytes of interest were separated on a Diamonsil C18 column (250 x 4.6 mm id, 5 microm) with the mobile phase consisting of THF/ACN/methanol/ 0.05% phosphoric acid solution (pH 5.0) (18:1:1:80 v/vl/v). The flow rate was set at 1.0 mL/min and the eluent was detected at 340 nm for the four flavonoids. The method was linear over the studied range of 1.00-100 microg/mL for the four analytes of interest with the correlation coefficient for each analyte greater than 0.999. The LOD and LOQwere 0.03 and 0.10 microg/mL, 0.03 and 0.10 microg/mL, 0.05 and 0.15 pg/mL, 0.10 and 0.30 microg/mL for vitexin-2"-O-glucoside, vitexin-2"-0-rhamnoside, rutin, and hyperoside, respectively. The optimized method was successfully applied to the analysis of four important flavonoids in the extract of hawthorn leaves. The total amounts of the four flavonoids were 22.2, 62.3, 4.27, and 8.24 mg/g dry weight for vitexin-2"-O-glucoside, vitexin-2"-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn leaves, respectively.

  6. Simultaneous extraction and determination of lead, cadmium and copper in rice samples by a new pre-concentration technique: Hollow fiber solid phase microextraction combined with differential pulse anodic stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Es' haghi, Zarrin, E-mail: z_eshaghi@pnu.ac.i [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Khalili, Maryam; Khazaeifar, Ali [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Rounaghi, Gholam Hossein [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

    2011-03-30

    In the present work, a novel solid phase microextraction (SPME) technique using a hollow fiber-supported sol-gel combined with multi-walled carbon nanotubes, coupled with differential pulse anodic stripping voltammetry (DPASV) was employed in the simultaneous extraction and determination of lead, cadmium and copper in rice. In this technique, an innovative solid sorbent containing mixture of carbon nanotube and a composite microporous compound was developed by the sol-gel method via the reaction of tetraethylorthosilicate (TEOS) with 2-amino-2-hydroxymethyl-propane-1,3-diol (TRIS). The growth process was initiated in basic condition (pH 10-11). Afterward this sol was injected into a polypropylene hollow fiber segment for in situ gelation process. The main factors influencing the pre-concentration and extraction of the metal ions; pH of the aqueous feed solution, extraction time, aqueous feed volume, agitation speed, the role of carbon nanotube reinforcement (as-grown and functionalized MWCNT) and salting effect have been examined in detail. Under the optimized conditions, linear calibration curves were established for the concentration of Cd(II), Pb(II) and Cu(II) in the range of 0.05-500, 0.05-500 and 0.01-100 ng mL{sup -1}, respectively. Detection limits obtained in this way are, 0.01, 0.025 and 0.0073 ng mL{sup -1} for Cd(II), Pb(II) and Cu(II), respectively. The relative standard deviations (RSDs) were found to be less than 5% (n = 5, conc.: 1.0 ng mL{sup -1}).

  7. Simultaneous detection and quantification of amphetamines, diazepam and its metabolites, cocaine and its metabolites, and opiates in hair by LC-ESI-MS-MS using a single extraction method.

    Science.gov (United States)

    Miller, Eleanor I; Wylie, Fiona M; Oliver, John S

    2008-09-01

    A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous identification and quantification of amphetamines, diazepam and its metabolites, cocaine and its metabolites, and opiates from hair using a single extraction method. As part of the method development, Gemini C18, Synergi Hydro RP, and Zorbax Stablebond-Phenyl LC columns were tested with three different mobile phases. Analyte recovery and limit of detection were evaluated for two different solid-phase extraction methods that used Bond Elut Certify and Clean Screen cartridges. Phosphate buffer (pH 5.0) was chosen as the optimum hair incubation medium because of the high stability of cocaine and 6-monoacetylmorphine using this method and faster sample preparation. The optimized method was fully validated. Linearity was established over the concentration range 0.2-10 ng/mg hair, and the correlation coefficients were all greater than 0.99. Total extraction recoveries were greater than 76%, detection limits were between 0.02 and 0.09 ng/mg, and the intra- and interday imprecisions were generally less than 20% in spiked hair. The intra- and interbatch imprecision of the method for a pooled authentic hair sample ranged from 1.4 to 23.4% relative standard deviation (RSD) and 8.3 to 25.4% RSD, respectively, for representative analytes from the different drug groups. The percent matrix effect ranged from 63.5 to 135.6%, with most analytes demonstrating ion suppression. Sixteen postmortem samples collected from suspected drug-related deaths were analyzed for the 17 drugs of abuse and metabolites included in the method. The method was sufficiently sensitive and specific for the analysis of drugs and metabolites in postmortem hair samples. There is scope for the inclusion of other target drugs and metabolites in the method.

  8. Simultaneous determination of acrylamide, asparagine and glucose in food using short chain methyl imidazolium ionic liquid based ultrasonic assisted extraction coupled with analyte focusing by ionic liquid micelle collapse capillary electrophoresis.

    Science.gov (United States)

    Abd El-Hady, Deia; Albishri, Hassan M

    2015-12-01

    Acrylamide (AA) is a known lethal neurotoxin and carcinogen. AA is formed in foods during the browning process by the Maillard reaction of glucose (GL) with asparagine (AS). For the first time, the simultaneous online preconcentration and separation of AA, AS and GL using analyte focusing by ionic liquid micelle collapse capillary electrophoresis (AFILMC) was presented. Samples were prepared in a 1-butyl-3-methylimidazolium bromide (BMIMBr) micellar matrix with a conductivity 4 times greater than that of the running buffer (12.5 mmol L(-1) phosphate buffer at pH 8.5). Samples were hydrodynamically injected into a fused silica capillary at 25.0 mbar for 25.0 s. Separations were performed by applying a voltage of 25.0 kV and a detection at 200.0 nm. To sufficiently reduce BMIMBr adsorption on the interior surface of capillary, an appropriate rinsing procedure by hydrochloric acid and water was optimized. AFILMC measurements of analytes within the concentration range of 0.05-10.0 μmol L(-1) achieved adequate reproducibility and accuracy with RSD 1.14-3.42% (n=15) and recovery 98.0-110.0%, respectively. Limits of detections were 0.71 ng g(-1) AA, 1.06 ng g(-1) AS and 27.02 ng g(-1) GL with linearity ranged between 2.2 and 1800 ng g(-1). The coupling of AFILMC with IL based ultrasonic assisted extraction (ILUAE) was successfully applied to the efficient extraction and determination of AA, AS and GL in bread samples. The structure of ILs has significant effects on the extraction efficiency of analytes. The optimal extraction efficiency (97.8%) was achieved by an aqueous extraction with 4:14 ratio of sample: 3.0 mol L(-1) BMIMBr followed by sonication at 35 °C. The proposed combination of ILUAE and AFILMC was simple, ecofriendly, reliable and inexpensive to analyze a toxic compound and its precursors in bread which is applicable to food safety. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Acute immunological responses to a combined viral-bacterial respiratory disease challenge in heifers administered transdermal flunixin meglumine

    Science.gov (United States)

    Time of flunixin meglumine transdermal (FTD; Finadyne Transdermal, Merck Animal Health, Summit, NJ) administration relative to a viral-bacterial challenge was evaluated in beef heifers. Thirty-two beef heifers (170 ± 21.1 kg BW) were randomly assigned to one of four treatments: 1) Control (CON), rec...

  10. Nanoemulsions as vehicles for transdermal delivery of glycyrrhizin

    Directory of Open Access Journals (Sweden)

    Ranjit Kumar Harwansh

    2011-12-01

    Full Text Available The present investigation aims to evaluate an isotropic and thermodynamically stable nanoemulsion formulation for transdermal delivery of glycyrrhizin (GZ, with minimum surfactant and cosurfactant (Smix concentrations that could improve its solubility, permeation enhancement, and stability. Pseudo-ternary phase diagrams were developed and various nanoemulsion formulations were prepared using soyabean oil as oil, Span 80, Brij 35 as a surfactant and isopropyl alcohol as a cosurfactant. Nanoemulsion formulations that passed the thermodynamic stability tests were characterized for pH, viscosity and droplet size using a transmission electron microscopy. The transdermal ability of glycyrrhizin through human cadaver skin was determined using Franz diffusion cells. The in vitro skin permeation profile of the optimized nanoemulsion formulation (NE2 was compared to that of conventional gel. A significant increase in permeability parameters such as steady-state flux (Jss and permeability coefficient (Kp was observed in the optimized nanoemulsion formulation (NE2, which consisted of 1% wt/wt of mono ammonium glycyrrhizinate (MAG, 32.4% Span 80, 3.7% Brij 35, 10% isopropyl alcohol, 46.5% soyabean oil and 6.4% distilled water. No obvious skin irritation was observed for the studied nanoemulsion formulation (NE2 or the gel. The results indicated that nanoemulsions are promising vehicles for transdermal delivery of glycyrrhizin through human cadaver skin, without the use of additional permeation enhancers, because excipients of nanoemulsions act as permeation enhancers themselves.O objetivo da investigação é avaliar uma nanoemulsão isotrópica termodinamicamente estável para a administração transdérmica da glicirrizina (GZ, com concentrações mínimas de tensoativo e co-tensoativo (Smix, que poderiam melhorar a sua solubilidade, a permeação e a estabilidade. Os diagramas pseudo-ternários de fase foram desenvolvidos e diversas nanoemulsões foram

  11. Influence of peptide dendrimers and sonophoresis on the transdermal delivery of ketoprofen.

    Science.gov (United States)

    Manikkath, Jyothsna; Hegde, Aswathi R; Kalthur, Guruprasad; Parekh, Harendra S; Mutalik, Srinivas

    2017-04-15

    The aim of this study was to determine the individual and combined effects of peptide dendrimers and low frequency ultrasound on the transdermal permeation of ketoprofen. Arginine terminated peptide dendrimers of varying charges (4(+), 8(+) and 16(+), named as A4. A8 and A16 respectively) were synthesized and characterized. Ketoprofen was subjected to passive, peptide dendrimer-assisted and sonophoretic permeation studies (with and without dendrimer application) across Swiss albino mouse skin, both in vitro and in vivo. The studies revealed that the synthesized peptide dendrimers considerably increased the transdermal permeation of ketoprofen and displayed enhancement ratios of up to 3.25 (with A16 dendrimer), compared to passive diffusion of drug alone in vitro. Moreover, the combination of peptide dendrimer treatment and ultrasound application worked in synergy and gave enhancement ratios of up to 1369.15 (with ketoprofen-A16 dendrimer complex). In vivo studies demonstrated that dendrimer and ultrasound-assisted permeation of drug achieved much higher plasma concentration of drug, compared to passive diffusion. Comparison of transdermal and oral absorption studies revealed that transdermal administration of ketoprofen with A8 dendrimer showed comparable absorption and plasma drug levels with oral route. The excised mouse skin after in vivo permeation study with dendrimers and ultrasound did not show major toxic reactions. This study demonstrates that arginine terminated peptide dendrimers combined with sonophoresis can effectively improve the transdermal permeation of ketoprofen. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Effect of transdermal hormone therapy on platelet haemostasis in menopausal women.

    Science.gov (United States)

    Stachowiak, Grzegorz; Pertyński, Tomasz; Pertyńska-Marczewska, Magdalena

    2015-01-01

    Despite the undeniably positive effect on the quality of life of menopausal women, menopausal hormone therapy (HT) also has negative side-effects, which include, among others, thromboembolic complications. To assess the effect of a popular type of this therapy - transdermal HT on platelet hemostasis, which plays a significant role in intravascular coagulation. The study group consisted of 92 postmenopausal women: 1) group G1 (n=30), treated with transdermal HT (17β-estradiol 50 μg/day plus NETA 170 μg/day); 2) group G2 (n=31), treated with the above transdermal HT and low dosage of acetylsalicylic acid (ASA); 3) control group P (n=31). All the women qualified for the study had two or more risk factors for arterial thrombosis, such as: smoking, hypertension, visceral obesity, hypercholesterolaemia, hypertriglyceridaemia, elevated levels of PAI-1, and increased fibrinogen, increased activity of coagulation factor VII. After three months of therapy, in the G1 group there was a decrease in platelet count (p = 0.004) and a decrease in GP IIb/IIIa - a platelet receptor for fibrinogen (p = 0.022). In the G2 group, no changes in the tested parameters were observed. 1) Transdermal HT in the form of combined, estrogen-progestogen patches favourably modifies platelets haemostasis, reversing the adverse effects that occur after menopause. 2) The use of low ASA doses as a thromboprophylaxis in short-term transdermal HT is not necessary.

  13. Transport efficiency in transdermal drug delivery: What is the role of fluid microstructure?

    Science.gov (United States)

    Liuzzi, Roberta; Carciati, Antonio; Guido, Stefano; Caserta, Sergio

    2016-03-01

    Interaction of microstructured fluids with skin is ubiquitous in everyday life, from the use of cosmetics, lotions, and drugs, to personal care with detergents or soaps. The formulation of microstructured fluids is crucial for the control of the transdermal transport. In biomedical applications transdermal delivery is an efficient approach, alternative to traditional routes like oral and parenteral administration, for local release of drugs. Poor skin permeability, mainly due to its outer layer, which acts as the first barrier against the entry of external compounds, greatly limits the applicability of transdermal delivery. In this review, we focus on recent studies on the improvement of skin transport efficiency by using microemulsions (ME). Quantitative techniques, which are able to investigate both skin morphology and penetration processes, are also reviewed. ME are increasingly used as transdermal systems due to their low preparation cost, stability and high bioavailability. ME may act as penetration enhancers for many active principles, but ME microstructure should be chosen appropriately considering several factors such as ratio and type of ingredients and physic-chemical properties of the active components. ME microstructure is strongly affected by the flow conditions applied during processing, or during spreading and rubbing onto skin. Although the role played by ME microstructure has been generally recognized, the skin transport mechanisms associated with different ME microstructures are still to be elucidated and further investigations are required to fully exploit the potential of ME in transdermal delivery. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Formulation, in vitro and in vivo evaluation of transdermal patches containing risperidone.

    Science.gov (United States)

    Aggarwal, Geeta; Dhawan, Sanju; Hari Kumar, S L

    2013-01-01

    The efficacy of oral risperidone treatment in prevention of schizophrenia is well known. However, oral side effects and patient compliance is always a problem for schizophrenics. In this study, risperidone was formulated into matrix transdermal patches to overcome these problems. The formulation factors for such patches, including eudragit RL 100 and eudragit RS 100 as matrix forming polymers, olive oil, groundnut oil and jojoba oil in different concentrations as enhancers and amount of drug loaded were investigated. The transdermal patches containing risperidone were prepared by solvent casting method and characterized for physicochemical and in vitro permeation studies through excised rat skin. Among the tested preparations, formulations with 20% risperidone, 3:2 ERL 100 and ERS 100 as polymers, mixture of olive oil and jojoba oil as enhancer, exhibited greatest cumulative amount of drug permeated (1.87 ± 0.09 mg/cm(2)) in 72 h, so batch ROJ was concluded as optimized formulation and assessed for pharmacokinetic, pharmacodynamic and skin irritation potential. The pharmacokinetic characteristics of the optimized risperidone patch were determined using rabbits, while orally administered risperidone in solution was used for comparison. The calculated relative bioavailability of risperidone transdermal patch was 115.20% with prolonged release of drug. Neuroleptic efficacy of transdermal formulation was assessed by rota-rod and grip test in comparison with control and marketed oral formulations with no skin irritation. This suggests the transdermal application of risperidone holds promise for improved bioavailability and better management of schizophrenia in long-term basis.

  15. Terpene microemulsions for transdermal curcumin delivery: effects of terpenes and cosurfactants.

    Science.gov (United States)

    Liu, Chi-Hsien; Chang, Fu-Yen; Hung, De-Kai

    2011-01-01

    Microemulsion systems composed of terpenes, polysorbate 80, cosurfactants, and water were investigated as transdermal delivery vehicles for curcumin. Pseudoternary phase diagrams of three terpenes (limonene, 1,8-cineole, and α-terpineol) at a constant surfactant/cosurfactant ratio (1:1) were constructed to illustrate their phase behaviors. Limonene combined with cosurfactants like ethanol, isopropanol, and propylene glycol were employed as microemulsion ingredients to study their potential for transdermal curcumin delivery. The transdermal delivery efficacy and skin retention of curcumin were evaluated using neonate pig skin mounted on a Franz diffusion cell. The curcumin permeation rates in the limonene microemulsion studied were 30- and 44-fold higher than those of 1,8-cineole and α-terpineol microemulsions, respectively. Significant effects on the skin permeation rates were observed from microemulsions containing different limonene/water contents. Histological examination of treated skin was performed to investigate the change of skin morphologies. Characteristics such as droplet size, conductivity, interfacial tension, and viscosity were analyzed to understand the physicochemical properties of the transdermal microemulsions. In conclusion, microemulsions loaded with curcumin were successfully optimized for transdermal delivery after screening various terpenes, cosurfactants, and limonene/water ratios. These results indicate that the limonene microemulsion system is a promising tool for the percutaneous delivery of curcumin. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Investigation of antihypertensive activity of carbopol valsartan transdermal gel containing 1,8-cineole.

    Science.gov (United States)

    Ahad, Abdul; Aqil, Mohd; Ali, Asgar

    2014-03-01

    The purpose of this work was to develop a transdermal gel formulation for enhanced delivery of valsartan for the management of hypertension. Transdermal gels bearing valsartan, carbopol and 1,8-cineole (penetration enhancer) were prepared and characterized for various parameters including in vitro skin permeation studies, pH, spreadability, viscosity, skin irritation potential and in vivo antihypertensive activity. Optimized valsartan gel formulation (VTGF9) showed highest transdermal flux (143.51 μg/cm(2)/h), with an enhancement ratio of 4.53 when compared to control gel formulation (VTGF8). Incorporation of 1,8-cineole and ethanol in gel formulation enhance the permeation of valsartan significantly. Skin irritation and histopathological study revealed that the VTGF9 was safe, less irritant and well tolerable formulation for transdermal delivery. In vivo antihypertensive activity revealed that optimized VTGF9 was successful in reverting the rat BP to normal values in experimental hypertensive rats. Finally, it could be concluded that VTGF9 accentuates the flux of valsartan and is an efficient transdermal therapeutic system for delivery of valsartan. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. [Effect of wintergreen oil on in vitro transdermal permeation of osthole and geniposide].

    Science.gov (United States)

    Gao, Xue-Cheng; Tong, Yan

    2017-04-01

    The aim of this study was to investigate the transdermal penetration enhancement effect of wintergreen oil and its action mechanisms. The in vitro transdermal tests were carried out to study the transdermal penetration enhancement effect of wintergreen oil by using osthole and geniposide as the lipophilic and hydriphilic model drugs. Fourier-transform infrared spectroscopy was used to investigate the effect of wintergreen oil on the molecular structure of rat stratum corneum, and the scanning electron microscope was employed to observe the change of rat skin surface after treatment by the oil. The wintergreen oil at proper concentrations could effectively promote the transdermal permeation of osthole and geniposide, and exhibited better penetration-enhancing activity for the lipophilic osthole, close to the commonly used classical penetration enhancer azone. The infrared spectroscopy study and scanning electron microscope showed that wintergreen oil mainly acted on the stratum corneum lipids, reduced dense stratum corneum, and reduced the skin barrier function. Thus, the wintergreen oil could effectively facilitate the transdermal absorption of the lipophilic and hydrophilic drugs, resulting from the lowed skin barrier function. Copyright© by the Chinese Pharmaceutical Association.

  18. Formulation and evaluation of lidocaine base ethosomes for transdermal delivery.

    Science.gov (United States)

    Zhu, Xiaoliang; Li, Fuli; Peng, Xuebiao; Zeng, Kang

    2013-08-01

    Although transdermal preparations of local anesthetics have been used to reduce pain caused by skin surgery, these preparations cannot effectively penetrate through the epidermis because of the barrier formed by the stratum corneum and the thick epidermis. Ethosomes can effectively transport drugs across the skin because of their thermodynamic stability, small size, high encapsulation efficiency, and percutaneous penetration. We evaluated lidocaine base ethosomes by measuring their loading efficiency, encapsulation efficiency, thermodynamic stability, and percutaneous penetration capability in vitro, and their effectiveness and cutaneous irritation in vivo. Lidocaine base ethosomes were prepared using the injection-sonication-filter method. Size, loading efficiency, encapsulation efficiency, and stability were evaluated using a Zetasizer and high performance liquid chromatography. Formulation was determined by measuring the maximum encapsulation efficiency in the orthogonal test. Percutaneous penetration efficiency in vitro was analyzed using a Franz-type diffusion cell experiment. In vivo effectiveness was analyzed using the pinprick test. Cutaneous irritancy tests were performed on white guinea pigs, followed by histopathologic analysis. The results were compared with lidocaine liposomes as well as lidocaine delivered in a hydroethanolic solution. Lidocaine base ethosomes composed of 5% (w/w) egg phosphatidyl choline, 35% (w/w) ethanol, 0.2% (w/w) cholesterol, 5% (w/w) lidocaine base, and ultrapure water had a mean maximum encapsulation of 51% ± 4%, a mean particle size of 31 ± 3 nm, and a mean loading efficiency of 95.0% ± 0.1%. The encapsulation efficiency of lidocaine base ethosomes remained stable for 60 days at 25°C ± 1°C (95% confidence interval [CI], -1.12% to 1.34%; P = 0.833). The transdermal flux of lidocaine base differed significantly for the 3 preparations (F = 120, P ethosomes than from liposomes (95% corrected CI, 1129-1818 µg/(cm(2)·h); P

  19. Iontophoretic and Microneedle Mediated Transdermal Delivery of Glycopyrrolate

    Directory of Open Access Journals (Sweden)

    Meera Gujjar

    2014-12-01

    Full Text Available Purpose: The objective of this study was to investigate the use of iontophoresis, soluble microneedles and their combination for the transdermal delivery of glycopyrrolate. Methods: In vitro permeation was tested using full thickness porcine ear skin mounted onto Franz diffusion cells. Iontophoresis (0.5 mA/cm2 was done for 4 h using Ag/AgCl electrodes. For microneedles, three line array (27 needles/line of maltose microneedles were used to microporate the skin prior to mounting. Pore uniformity was determined by taking fluorescent images of distribution of calcein into pores and processing the images using an image analysis tool, which measured the fluorescent intensity in and around each pore to provide a pore permeability index (PPI. The donor chamber contained 500 µL of a 1 mg/mL solution of glycopyrrolate, and the receptor chamber contained 5 mL of 50 mM NaCl in deionized water. Samples were collected at predetermined time points over a period of 24 h and analyzed by HPLC. Skin irritation testing was performed with a 3D cell culture kit of human skin. MTT assay determined cell viability; viability less than 50% was considered irritant. Results: A control experiment which investigated passive permeation of glycopyrrolate delivered an average cumulative amount of 24.92 ± 1.77 µg/cm2 at 24 h, while microneedle pretreatment increased permeability to 46.54 ± 6.9 µg/cm2. Both iontophoresis (158.53 ± 17.50 µg/cm2 and a combination of iontophoresis and microneedles (182.43 ± 20.06 µg/ cm2 significantly increased delivery compared to passive and microneedles alone. Glycopyrrolate solution was found to be nonirritant with cell viability of 70.4% ± 5.03%. Conclusion: Iontophoresis and a combination of iontophoresis with microneedle pretreatment can be effectively used to enhance the transdermal delivery of glycopyrrolate. Glycopyrrolate was found to be non-irritant to skin.

  20. Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with pressurized liquid extraction for simultaneous quantification and confirmation of cyromazine, melamine and its metabolites in foods of animal origin.

    Science.gov (United States)

    Yu, Huan; Tao, Yanfei; Chen, Dongmei; Wang, Yulian; Liu, Zhaoying; Pan, Yuanhu; Huang, Lingli; Peng, Dapeng; Dai, Menghong; Liu, Zhenli; Yuan, Zonghui

    2010-12-03

    Simple and sensitive methods have been developed for simultaneous detection of cyromazine, melamine and their metabolites (ammeline, ammelide and cyanuric acid) in samples of animal origins. These include a high performance liquid chromatography (HPLC) method and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and are useful in regular monitoring and in toxicity studies of these molecules. Representative samples used in this study include muscles and livers of swine, bovine, sheep and chicken, kidneys of swine, bovine and sheep, and milk powder. A new sample preparation procedure with pressurized liquid extraction (PLE) at 1400psi and 70°C was investigated. Quantification of these five compounds by HPLC was achieved using an APS-2 column with UV detection at 230 nm. Limit of detection (LOD) was at 10 μgkg(-1), and limit of quantification (LOQ) was at 40 μgkg(-1). Recoveries of the five analytes in spiked samples ranged from 72.2% to 115.4% with RSD less than 12%. Confirmatory analysis of the analytes was performed using LC-MS/MS in selected reaction monitoring (SRM) mode. The LOD and LOQ were 5 μgkg(-1) and 15 μgkg(-1), respectively. This is the first simultaneous analysis of cyromazine, melamine, ammeline, ammelide and cyanuric acid residues in complex tissue samples using PLE and HPLC. It is expected that these methods will find many practical applications in evaluating the safety of cyromazine, melamine and their metabolites. Copyright © 2010 Elsevier B.V. All rights reserved.

  1. A simple and rapid analytical method based on solid-phase extraction and liquid chromatography-tandem mass spectrometry for the simultaneous determination of free catecholamines and metanephrines in urine and its application to routine clinical analysis.

    Science.gov (United States)

    Woo, Hye In; Yang, Jeong Soo; Oh, Hyeon Ju; Cho, Yoon Young; Kim, Jae Hyeon; Park, Hyung-Doo; Lee, Soo-Youn

    2016-05-01

    Urinary catecholamines and metanephrines are biochemical indicators of pheochromocytoma. We developed and validated a rapid and precise analytical method based on solid-phase extraction (SPE) and liquid chromatography separation coupled to tandem mass spectrometry (LC-MS/MS) for measuring urinary free catecholamines and metanephrines in a clinical setting. Following SPE purification of catecholamines and metanephrines from urine specimens, chromatographic separation and quantitative detection were performed using LC-MS/MS. The developed method for simultaneous measurement of urinary free catecholamines and metanephrines was validated with clinical urine specimens and was compared with other clinical and biochemical results, including urinary total metanephrines, vanillylmandelic acid (VMA), and plasma free metanephrines. The performance of our newly developed method for measuring urinary free epinephrine (EPI), norepinephrine (NE), dopamine (DA), metanephrine (MN), and normetanephrine (NMN), was acceptable. The recoveries and matrix effects of analytes were 61-107% and 84.5-130.7%. The linear ranges of each analyte were 3.8-2163μg/L, 7.4-2,359μg/L, 5.4-2,825μg/L, 3.5-2,466μg/L, and 3.7-2,569μg/L, and the coefficients of variation (CV) were less than 10% with respect to imprecision. Carryover and sample stability were also validated. Validation using clinical urine specimens by comparison with various biochemical results showed that urinary free metanephrines had comparable sensitivity (100%) and superior specificity (97.1%) to urinary total and plasma free metanephrines. The facile and reliable simultaneous measurement method for urinary free catecholamines and metanephrines using LC-MS/MS developed in this study is helpful in obtaining information about multiple metabolites and is applicable to routine clinical settings for the screening of pheochromocytoma. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights

  2. Simultaneous Determination of Purpurin, Munjistin and Mollugin in Rat Plasma by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study after Oral Administration of Rubia cordifolia L. Extract

    Directory of Open Access Journals (Sweden)

    Mingjie Gao

    2016-06-01

    Full Text Available A specific, simple, sensitive Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry (UHPLC-MS/MS method has been developed and validated for the simultaneous determination and pharmacokinetic study of purpurin, munjistin, and mollugin in rat plasma. Chromatographic separation was carried out using a C18 column (ACQUITY UPLC® HSS T3, 1.8 μm, 2.1 × 100 mm with gradient elution. The compounds were detected on a 6430 triple-quadrupole tandem MS with an electrospray ionization (ESI interface using multiple reaction monitoring (MRM in positive ionization mode. The samples were prepared by a liquid-liquid extraction (LLE method with ethyl acetate after being spiked with an internal standard (bifendate. The current UHPLC-MS/MS assay was validated for its linearity, intra-day and inter-day precisions, accuracy, extraction recovery, matrix effect and stability in different conditions. The method was linear for all analytes over the investigated range with all determined correlation coefficients exceeding 0.9900. The intra-day and inter-day precisions were in the range of 4.21% to 14.84%, and the relative errors of accuracies were in the range of −14.05% to 14.75%. The mean recoveries and matrix effects of purpurin, munjistin, and mollugin were higher than 78.87% and 92.56%, repectively. After oral administration of 0.82 g/kg of Rubia cordifolia extract, the maximum plasma concentrations (Cmax were 70.10 ± 11.78 ng/mL for purpurin, 26.09 ± 6.6 ng/mL for munjistin, and 52.10 ± 6.71 ng/mL for mollugin. The time for maximal concentration (Tmax was 1.61 ± 0.24 h for purpurin, 2.58 ± 0.19 h for munjistin, and 1.99 ± 0.21 h for mollugin. The established method was further applied to a pharmacokinetic study of purpurin, munjistin, and mollugin in rat plasma. It was concluded from the pharmacokinetic parameters that the three analytes showed a process of slow absorption and metabolism after oral administration of R. cordifolia extract to

  3. Carbon Nanotube Membranes for use in the Transdermal Treatment of Nicotine Addiction and Opioid Withdrawal Symptoms

    Directory of Open Access Journals (Sweden)

    Caroline L. Strasinger

    2009-01-01

    Full Text Available Transdermal systems are attractive methods of drug administration specifically when treating patients for drug addiction. Current systems however are deficient in therapies that allow variable flux values of drug, such as nicotine for smoking cessation or complex dosing regimens using clonidine when treating opioid withdrawal symptoms. Through the use of functionalized carbon nanotube (CNT membranes, drug delivery to the skin can be controlled by applying a small electrical bias to create a programmable drug delivery system. Clearly, a transdermal patch system that can be tailored to an individual's needs will increase patient compliance as well as provide much more efficient therapy. The purpose of this paper is to discuss the applicability of using carbon nanotube membranes in transdermal systems for treatment of drug abuse.

  4. Carbon Nanotube Membranes for use in the Transdermal Treatment of Nicotine Addiction and Opioid Withdrawal Symptoms

    Directory of Open Access Journals (Sweden)

    Audra L. Stinchcomb

    2009-01-01

    Full Text Available Transdermal systems are attractive methods of drug administration specifically when treating patients for drug addiction. Current systems however are deficient in therapies that allow variable flux values of drug, such as nicotine for smoking cessation or complex dosing regimens using clonidine when treating opioid withdrawal symptoms. Through the use of functionalized carbon nanotube (CNT membranes, drug delivery to the skin can be controlled by applying a small electrical bias to create a programmable drug delivery system. Clearly, a transdermal patch system that can be tailored to an individual’s needs will increase patient compliance as well as provide much more efficient therapy. The purpose of this paper is to discuss the applicability of using carbon nanotube membranes in transdermal systems for treatment of drug abuse.

  5. Synthesis and characterization of modified starch/polybutadiene as novel transdermal drug delivery system.

    Science.gov (United States)

    Saboktakin, Mohammad Reza; Akhyari, Shahab; Nasirov, Fizuli A

    2014-08-01

    Transdermal drug delivery systems are topically administered medicaments in the form of patches that deliver drugs for systemic effects at a predetermined and controlled rate. It works very simply in which drug is applied inside the patch and it is worn on skin for long period of time. Polymer matrix, drug, permeation enhancers are the main components of transdermal drug delivery systems. The objective of the present study was to develop the modified starch and 1,4-cis polybutadiene nanoparticles as novel polymer matrix system. We have been studied the properties of a novel transdermal drug delivery system with clonidine as drug model. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Correlation between the transdermal characteristics of pseudoephedrine and amygdalin in majiepingchuan in vitro.

    Science.gov (United States)

    Kong, Hui; Qu, Huihua; Qu, Baoping; Zeng, Wenhao; Zhao, Yan; Wang, Xueqian; Wang, Qingguo

    2016-04-01

    To analyze the transdermal profile of pseudoephedrine and amygdalin in the Traditional Chinese Medicine majiepingchuan in rat skin and to reveal their interaction. A Franz diffusion cell was used in vitro to evaluate the transdermal parameters of cumulative transdermal flux (Q(tot)), cumulative transmission (T(tot)), and mean penetration rate (Kp) of pseudoephedrine and amygdalin in majiepingchuan. Linear regression analyses of Q(tot) over time of pseudoephedrine vs amygdalin and their ratios was adopted for correlation evaluation. At 1, 2, 4, 6, and 8 h, the Q(tot), T(tot) and Kp of pseudoephedrine showed a good correlation with that of amygdalin. There was a small difference in the ratios of Q(tot), T(tot) and Kp between pseudoephedrine and amygdalin, and a correlation between them.

  7. Optimization of Biopolymer Based Transdermal Films of Metoclopramide as an Alternative Delivery Approach

    Directory of Open Access Journals (Sweden)

    Betül Aktar

    2014-05-01

    Full Text Available The objectives of this study were to develop and to characterize sodium alginate based matrix-type transdermal films of metoclopramide hydrochloride (MTC in order to improve patient compliance to treatment. The suitability of sodium alginate was shown to be a natural film former in terms of the physicochemical, mechanical, and bioadhesive features of the MTC loaded transdermal films. Terpinolene provided the highest drug release among the different terpenes (nerolidol, eucalyptol, dl-limonene, or terpinolene assessed as enhancer. Attenuated Total Reflectance Infrared (ATR-FTIR spectroscopy analysis performed to evaluate the effect of the transdermal films on skin barrier confirmed enhancer induced lipid bilayer disruption in stratum corneum, indicating its permeation enhancement effect.

  8. Nanoparticle-Enabled Transdermal Drug Delivery Systems for Enhanced Dose Control and Tissue Targeting

    Directory of Open Access Journals (Sweden)

    Brian C. Palmer

    2016-12-01

    Full Text Available Transdermal drug delivery systems have been around for decades, and current technologies (e.g., patches, ointments, and creams enhance the skin permeation of low molecular weight, lipophilic drugs that are efficacious at low doses. The objective of current transdermal drug delivery research is to discover ways to enhance skin penetration of larger, hydrophilic drugs and macromolecules for disease treatment and vaccination. Nanocarriers made of lipids, metals, or polymers have been successfully used to increase penetration of drugs or vaccines, control drug release, and target drugs to specific areas of skin in vivo. While more research is needed to identify the safety of nanocarriers, this technology has the potential to expand the use of transdermal routes of administration to a wide array of therapeutics. Here, we review the current state of nanoparticle skin delivery systems with special emphasis on targeting skin diseases.

  9. Minimally invasive transdermal delivery of iron-dextran.

    Science.gov (United States)

    Juluri, Abhishek; Modepalli, Naresh; Jo, Seongbong; Repka, Michael A; Shivakumar, H Nanjappa; Murthy, S Narasimha

    2013-03-01

    Iron deficiency is one of the most prevalent and serious health issues among people all over the world. Iron-dextran (ID) colloidal solution is one among the very few US Food and Drug Administration (FDA)-approved iron sources for parenteral administration of iron. Parenteral route does not allow frequent administration because of its invasiveness and other associated complications. The main aim of this project was to investigate the plausibility of transdermal delivery of ID facilitated by microneedles, as an alternative to parenteral iron therapy. In vitro permeation studies were carried out using freshly excised hairless rat abdominal skin in a Franz diffusion apparatus. Iron repletion studies were carried out in hairless anemic rat model. The anemic rats were divided into intact skin (control), microneedle pretreated, and intraperitoneal (i.p.) groups depending on the mode of delivery of iron. The hematological parameters were measured intermittently during treatment. There was no improvement in the hematological parameters in case of control group, whereas, in case of microneedle pretreated and i.p. group, there was significant improvement within 2-3 weeks. The results suggest that microneedle-mediated delivery of ID could be developed as a potential treatment method for iron-deficiency anemia. Copyright © 2012 Wiley Periodicals, Inc.

  10. Enhanced transdermal deposition and characterization of quercetin-loaded ethosomes

    Energy Technology Data Exchange (ETDEWEB)

    Park, Soo Nam; Lee, Hye Jin; Kim, Hae Soo; Park, Min A; Gu, Hyun A [Seoul National University of Science and Technology, Seoul (Korea, Republic of)

    2013-03-15

    We sought to evaluate the transdermal permeation potential of quercetin-loaded ethosomes. Quercetinloaded ethosomes were prepared and characterized with regard to particle size, loading efficiency, stability, and in vitro skin permeation. The optimized formulation of ethosomes was confirmed using 2% egg phosphatidylcholine and hydrated 20% ethanol. After quercetin was applied using this formulation, the stability of the ethosomes was determined when loaded with up to 0.04% quercetin. We observed that loading efficiency was improved with increasing concentrations of quercetin. Ethosomes loaded with 0.04% quercetin showed both the greatest loading efficiency (63.9%±6.0%) and an optimal size range (132±32 nm). Ethosomes loaded with quercetin were superior in skin permeation ability (29.5±7.0 µg/cm{sup 2}) compared to either ethanolic solution or liposomes. Therefore, we concluded that quercetin-loaded ethosomes increased the skin delivery of quercetin. Our results suggest that quercetin-loaded ethosomes may enhance the effect of cosmetic materials.

  11. Transdermal delivery devices: fabrication, mechanics and drug release from silk.

    Science.gov (United States)

    Raja, Waseem K; Maccorkle, Scott; Diwan, Izzuddin M; Abdurrob, Abdurrahman; Lu, Jessica; Omenetto, Fiorenzo G; Kaplan, David L

    2013-11-11

    Microneedles are a relatively simple, minimally invasive and painless approach to deliver drugs across the skin. However, there remain limitations with this approach because of the materials most commonly utilized for such systems. Silk protein, with tunable and biocompatibility properties, is a useful biomaterial to overcome the current limitations with microneedles. Silk devices preserve drug activity, offer superior mechanical properties and biocompatibility, can be tuned for biodegradability, and can be processed under aqueous, benign conditions. In the present work, the fabrication of dense microneedle arrays from silk with different drug release kinetics is reported. The mechanical properties of the microneedle patches are tuned by post-fabrication treatments or by loading the needles with silk microparticles, to increase capacity and mechanical strength. Drug release is further enhanced by the encapsulation of the drugs in the silk matrix and coating with a thin dissolvable drug layer. The microneedles are used on human cadaver skin and drugs are delivered successfully. The various attributes demonstrated suggest that silk-based microneedle devices can provide significant benefit as a platform material for transdermal drug delivery. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Photoinduced disaggregation of TiO₂ nanoparticles enables transdermal penetration.

    Directory of Open Access Journals (Sweden)

    Samuel W Bennett

    Full Text Available Under many aqueous conditions, metal oxide nanoparticles attract other nanoparticles and grow into fractal aggregates as the result of a balance between electrostatic and Van Der Waals interactions. Although particle coagulation has been studied for over a century, the effect of light on the state of aggregation is not well understood. Since nanoparticle mobility and toxicity have been shown to be a function of aggregate size, and generally increase as size decreases, photo-induced disaggregation may have significant effects. We show that ambient light and other light sources can partially disaggregate nanoparticles from the aggregates and increase the dermal transport of nanoparticles, such that small nanoparticle clusters can readily diffuse into and through the dermal profile, likely via the interstitial spaces. The discovery of photoinduced disaggregation presents a new phenomenon that has not been previously reported or considered in coagulation theory or transdermal toxicological paradigms. Our results show that after just a few minutes of light, the hydrodynamic diameter of TiO(2 aggregates is reduced from ∼280 nm to ∼230 nm. We exposed pigskin to the nanoparticle suspension and found 200 mg kg(-1 of TiO(2 for skin that was exposed to nanoparticles in the presence of natural sunlight and only 75 mg kg(-1 for skin exposed to dark conditions, indicating the influence of light on NP penetration. These results suggest that photoinduced disaggregation may have important health implications.

  13. Exacerbation of asthma secondary to fentanyl transdermal patch.

    Science.gov (United States)

    Parmar, Malvinder S

    2009-01-01

    Asthma is a common chronic inflammatory disorder of the airways associated with hyperresponsiveness, reversible airflow limitation and respiratory symptoms.1 All patients with asthma are at risk for exacerbations that may range from mild to life threatening. Different triggers cause asthma exacerbation by inducing airway inflammation and/or provoking bronchospasm. Allergen-induced bronchospasm results from IgE-dependent release of mediators including histamine, prostaglandins and leukotrienes.2 Opiates are commonly used to treat chronic pain.3 Although hypersensitivity to opiates or accumulation of opiates can cause respiratory depression, opiates are also used in the management of cough and dyspnoea associated with advanced COPD and heart failure.4(,)5 Here, a report is presented on a patient who developed persistent exacerbation of underlying stable asthma after initiating fentanyl transdermal therapy for chronic low back pain. He underwent extensive investigations and a detailed reassessment of history, especially medication history, led to the possible causative factor; once recognised, removal of the offending agent (fenatnyl) resulted in complete improvement in his symptoms within 72 h.

  14. Formulation and evaluation of ethosomes for transdermal delivery of lamivudine.

    Science.gov (United States)

    Jain, Subheet; Tiwary, Ashok K; Sapra, Bharti; Jain, Narendra K

    2007-12-21

    The purpose of the present research was to investigate the mechanism for improved intercellular and intracellular drug delivery from ethosomes using visualization techniques and cell line study. Ethosomal formulations were prepared using lamivudine as model drug and characterized in vitro, ex vivo and in vivo. Transmission electron microscopy, scanning electron microscopy, and fluorescence microscopy were employed to determine the effect of ethosome on ultrastructure of skin. Cytotoxicity and cellular uptake of ethosome were determined using T-lymphoid cell line (MT-2). The optimized ethosomal formulation showed 25 times higher transdermal flux (68.4 +/- 3.5 microg/cm(2)/h) across the rat skin as compared with that of lamivudine solution (2.8 +/- 0.2 microg/cm(2)/h). Microscopic studies revealed that ethosomes influenced the ultrastructure of stratum corneum. Distinct regions with lamellar stacks derived from vesicles were observed in intercellular region of deeper skin layers. Results of cellular uptake study showed significantly higher intracellular uptake of ethosomes (85.7% +/- 4.5%) as compared with drug solution (24.9% +/- 1.9%). The results of the characterization studies indicate that lipid perturbation along with elasticity of ethosomes vesicles seems to be the main contributor for improved skin permeation.

  15. Opioids Switching with Transdermal Systems in Chronic Cancer Pain

    Directory of Open Access Journals (Sweden)

    Barbarisi M

    2009-05-01

    Full Text Available Abstract Background Due to tolerance development and adverse side effects, chronic pain patients frequently need to be switched to alternative opioid therapy Objective To assess the efficacy and tolerability of an alternative transdermally applied (TDS opioid in patients with chronic cancer pain receiving insufficient analgesia using their present treatment. Methods A total of 32 patients received alternative opioid therapy, 16 were switched from buprenorphine to fentanyl and 16 were switched from fentanyl to buprenorphine. The dosage used was 50% of that indicated in equipotency conversion tables. Pain relief was assessed at weekly intervals for the next 3 weeks Results Pain relief as assessed by VAS, PPI, and PRI significantly improved (p Conclusion Opioid switching at 50% of the calculated equianalgesic dose produced a significant reduction in pain levels and rescue medication. The incidence of side effects decreased and no new side effects were noted. Further studies are required to provide individualized treatment for patients according to their different types of cancer.

  16. Curcumin nanoemulsion for transdermal application: formulation and evaluation.

    Science.gov (United States)

    Rachmawati, Heni; Budiputra, Dewa Ken; Mauludin, Rachmat

    2015-04-01

    The aim of this work is to develop a curcumin nanoemulsion for transdermal delivery. The incorporation of curcumin inside a nanoglobul should improve curcumin stability and permeability. A nanoemulsion was prepared by the self-nanoemulsification method, using an oil phase of glyceryl monooleate, Cremophor RH40 and polyethylene glycol 400. Evaluation of the nanoemulsion included analysis of particle size, polydispersity index, zeta potential, physical stability, Raman spectrum and morphology. In addition, the physical performance of the nanoemulsion in Viscolam AT 100P gel was studied. A modified vertical diffusion cell and shed snake skin of Python reticulatus were used to study the in vitro permeation of curcumin. A spontaneously formed stable nanoemulsion has a loading capacity of 350 mg curcumin/10 g of oil phase. The mean droplet diameter, polydispersity index and zeta potential of optimized nanoemulsion were 85.0 ± 1.5 nm, 0.18 ± 0.0 and -5.9 ± 0.3 mV, respectively. Curcumin in a nanoemulsion was more stable than unencapsulated curcumin. Furthermore, nanoemulsification significantly improved the permeation flux of curcumin from the hydrophilic matrix gel; the release kinetic of curcumin changed from zero order to a Higuchi release profile. Overall, the developed nanoemulsion system not only improved curcumin permeability but also protected the curcumin from chemical degradation.

  17. Development of the ambroxol gels for enhanced transdermal delivery.

    Science.gov (United States)

    Cho, Cheong-Weon; Choi, Jun-Shik; Shin, Sang-Chul

    2008-03-01

    Ambroxol is an expectoration improver and mucolytic agent that has been used to treat acute and chronic disorders. However, ambroxol needs to be administered percutaneously in order to avoid systemic adverse effects, such as headache, drowsiness, dizziness, and insomnia, which can occur after oral administration. The aim of this study was to develop a gel preparation containing a permeation enhancer to enhance the delivery of ambroxol. The ambroxol gels were prepared using hydroxypropyl methylcellulose (HPMC) and poloxamer 407. The release characteristics of the drug from the gels were examined according to the receptor medium, drug concentration, and temperature. The rate of drug permeation into the skin was enhanced by incorporating various enhancers such as the ethylene glycols, the propylene glycols, the glycerides, the non-ionic surfactants, and the fatty acids into the gels. The permeation study through mouse skin was examined at 37 C. The rate of drug release increased with increasing drug concentration and temperature. Among the enhancers used, propylene glycol mono caprylate showed the best enhancing effects. The estimated activation energy of release (Ea), which was calculated from the slope of a log P versus 1000/T plot, was 14.80, 14.22, 13.91, and 12.46 kcal/mol for ambroxol loading doses of 2, 3, 4, and 5%, respectively. The results of this study show that the gel preparation of ambroxol containing a permeation enhancer could be developed for the enhanced transdermal delivery of ambroxol.

  18. Novel in situ forming hydrogel microneedles for transdermal drug delivery.

    Science.gov (United States)

    Sivaraman, Arunprasad; Banga, Ajay K

    2017-02-01

    Novel in situ forming hydrogel microneedles were evaluated for transdermal drug delivery using a biocompatible non-ionic triblock amphiphilic thermosensitive copolymer. The transition property of poloxamer from solution at room temperature to gel at skin temperature (32 °C) was utilized in preparation of in situ forming hydrogel microneedles. Methotrexate has been used to treat solid tumors, but because of its narrow safety margin, it requires sustained delivery within the therapeutic window. Formulations with and without poloxamer at different methotrexate concentrations were prepared and evaluated for drug permeation across skin using vertical Franz diffusion cell for 72 h. Sol-gel transition, skin resistance and thickness, microneedles geometry, microchannel depth, shape, formation and uniformity, viscoelasticity of skin, and in vitro drug permeation were characterized and tested. An average cumulative drug amount of 32.2 ± 15.76 and 114.54 ± 40.89 μg/cm(2) for porcine ear skin and 3.89 ± 0.60 and 10.27 ± 6.98 μg/cm(2) for dermatomed human skin from 0.2 % w/w and 0.4 % w/w methotrexate formulations was delivered by the in situ forming hydrogel microneedles. These in situ hydrogel microneedles embedded within the porated site of the skin provided a steady and sustained drug delivery.

  19. Two Photon Polymerization of Microneedles for Transdermal Drug Delivery

    Science.gov (United States)

    Gittard, Shaun D.; Ovsianikov, Aleksandr; Chichkov, Boris N.; Doraiswamy, Anand; Narayan, Roger J.

    2010-01-01

    Importance of the field Microneedles are small-scale devices that are finding use for transdermal delivery of protein-based pharmacologic agents and nucleic acid-based pharmacologic agents; however, microneedles prepared using conventional microelectronics-based technologies have several shortcomings, which have limited translation of these devices into widespread clinical use. Areas covered in this review Two photon polymerization is a laser-based rapid prototyping technique that has been recently used for direct fabrication of hollow microneedles with a wide variety of geometries. In addition, an indirect rapid prototyping method that involves two photon polymerization and polydimethyl siloxane micromolding has been used for fabrication of solid microneedles with exceptional mechanical properties. What the reader will gain In this review, the use of two photon polymerization for fabricating in-plane and out-of-plane hollow microneedle arrays is described. The use of two photon polymerization-micromolding for fabrication of solid microneedles is also reviewed. In addition, fabrication of microneedles with antimicrobial properties is discussed; antimicrobial microneedles may reduce the risk of infection associated with formation of channels through the stratum corneum. Take home message It is anticipated that the use of two photon polymerization as well as two photon polymerization-micromolding for fabrication of microneedles and other microstructured drug delivery devices will increase over the coming years. PMID:20205601

  20. Two-photon polymerization of microneedles for transdermal drug delivery.

    Science.gov (United States)

    Gittard, Shaun D; Ovsianikov, Aleksandr; Chichkov, Boris N; Doraiswamy, Anand; Narayan, Roger J

    2010-04-01

    Microneedles are small-scale devices that are finding use for transdermal delivery of protein-based pharmacologic agents and nucleic acid-based pharmacologic agents; however, microneedles prepared using conventional microelectronics-based technologies have several shortcomings, which have limited translation of these devices into widespread clinical use. Two-photon polymerization is a laser-based rapid prototyping technique that has been used recently for direct fabrication of hollow microneedles with a wide variety of geometries. In addition, an indirect rapid prototyping method that involves two-photon polymerization and polydimethyl siloxane micromolding has been used for fabrication of solid microneedles with exceptional mechanical properties. In this review, the use of two-photon polymerization for fabricating in-plane and out-of-plane hollow microneedle arrays is described. The use of two-photon polymerization-micromolding for fabrication of solid microneedles is also reviewed. In addition, fabrication of microneedles with antimicrobial properties is discussed; antimicrobial microneedles may reduce the risk of infection associated with the formation of channels through the stratum corneum. It is anticipated that the use of two-photon polymerization as well as two-photon polymerization-micromolding for fabrication of microneedles and other microstructured drug delivery devices will increase over the coming years.

  1. Critical appraisal of selegiline transdermal system for major depressive disorder.

    Science.gov (United States)

    Cristancho, Mario A; Thase, Michael E

    2016-01-01

    Although safer and easier to use antidepressants (ie.,SSRIs/SNRIs) have largely displaced MAOIs, these medications still have a role in difficult to treat conditions. Efforts to improve MAOIs benefit-risk profile resulted on the reversible MAOI and in the first antidepressant patch (selegiline transdermal delivery system-STS). The later had been available in the US since 2006. Thus a review on its safety profile and comparative efficacy is timely. This review provides an overview of STS's clinical pharmacology and summarizes what has been learned across nearly a decade of experience. Product labels and the search engine PubMed were used to obtain relevant information. STS remains a unique treatment option. It is the only FDA-approved antidepressant for patients with significant problems ingesting, tolerating, or absorbing oral medications. It remains the only MAOI that can be initiated without dietary restrictions at a therapeutic dose and has a low incidence of side effects when compared to other MAOIs. STS also provides an interesting option for depressed patients suffering from Parkinson's disease. However these advantages are counterweighted by drawbacks including the need for wash-out periods and the lack of convincing data illustrating its utility for treatment of more severe, treatment refractory depression.

  2. Transdermal nitroglycerine enhances postoperative analgesia of intrathecal neostigmine following abdominal hysterectomies

    Directory of Open Access Journals (Sweden)

    Fareed Ahmed

    2010-01-01

    Full Text Available This study was carried out to assess the effect of nitroglycerine (transdermal on intrathecal neostigmine with bupivacaine on postoperative analgesia and note the incidence of adverse effects, if any. After taking informed consent, 120 patients of ASA Grade I and II were systematically randomised into four groups of 30 each. Patients were premedicated with midazolam 0.05 mg/kg intravenously and hydration with Ringer′s lactate solution 10ml/kg preoperatively in the holding room. Group I patients received Intrathecal injection of 15 mg bupivacaine with 1ml of normal saline and transdermal placebo patch. Group II patients received Intrathecal injection of 15 mg bupivacaine with 5 mcg of neostigmine and transdermal placebo patch. Group III patients received Intrathecal injection of 15 mg bupivacaine with 1ml of normal saline with transdermal nitroglycerine patch (5 mg/24 hours. Group IV patients received Intrathecal injection of 15 mg bupivacaine with 5mcg of neostigmine and transdermal nitroglycerine patch (5 mg/24 hours, applied on a non anaesthetised area after 20 minutes. Groups were demographically similar and did not differ in intraoperative characteristics like sensory block, motor block, haemodynamic parameters and SpO 2 . The mean duration of analgesia was 202.17 minutes, 407.20 minutes, 207.53 minutes and 581.63 minutes in control group (I, neostigmine group (II, nitroglycerine group (III and nitroglycerine neostigmine group (IV respectively (P< 0.01. To conclude, our results show that transdermal nitroglycerine itself does not show any analgesic potential but it enhances the analgesic potential of intrathecal neostigmine.

  3. Transdermal permeation of drugs with differing lipophilicity: Effect of penetration enhancer camphor.

    Science.gov (United States)

    Xie, Feng; Chai, Jia-Ke; Hu, Quan; Yu, Yong-Hui; Ma, Li; Liu, Ling-Ying; Zhang, Xu-Long; Li, Bai-Ling; Zhang, Dong-Hai

    2016-06-30

    The aim of the present study was to investigate the potential application of (+)-camphor as a penetration enhancer for the transdermal delivery of drugs with differing lipophilicity. The skin irritation of camphor was evaluated by in vitro cytotoxicity assays and in vivo transdermal water loss (TEWL) measurements. A series of model drugs with a wide span of lipophilicity (logP value ranging from 3.80 to -0.95), namely indometacin, lidocaine, aspirin, antipyrine, tegafur and 5-fluorouracil, were tested using in vitro transdermal permeation experiments to assess the penetration-enhancing profile of camphor. Meanwhile, the in vivo skin microdialysis was carried out to further investigate the enhancing effect of camphor on the lipophilic and hydrophilic model drugs (i.e. lidocaine and tegafur). SC (stratum corneum)/vehicle partition coefficient and Fourier transform infrared spectroscopy (FTIR) were performed to probe the regulation action of camphor in the skin permeability barrier. It was found that camphor produced a relatively low skin irritation, compared with the frequently-used and standard penetration enhancer laurocapram. In vitro skin permeation studies showed that camphor could significantly facilitate the transdermal absorption of model drugs with differing lipophilicity, and the penetration-enhancing activities were in a parabola curve going downwards with the drug logP values, which displayed the optimal penetration-enhancing efficiency for the weak lipophilic or hydrophilic drugs (an estimated logP value of 0). In vivo skin microdialysis showed that camphor had a similar penetration behavior on transdermal absorption of model drugs. Meanwhile, the partition of lipophilic drugs into SC was increased after treatment with camphor, and camphor also produced a shift of CH2 vibration of SC lipid to higher wavenumbers and decreased the peak area of the CH2 vibration, probably resulting in the alteration of the skin permeability barrier. This suggests that

  4. Development and validation of high liquid performance chromatography-tandem mass spectrometry method for simultaneous determination of geniposidic acid and aucubin in rat plasma for pharmacokinetic study after oral administration of Du-zhong tea extract.

    Science.gov (United States)

    Zhang, Lin; Ma, Yu-Liang; Liu, Yang; Zu, Yuan-Gang

    2014-07-15

    A specific and sensitive high performance liquid chromatography coupled with tandem mass spectrometric (HPLC-MS/MS) method was developed and validated for the simultaneous determination of geniposidic acid and aucubin in rat plasma after oral administration of Du-zhong tea extract. The plasma samples were pretreated by protein precipitation with methanol and the chromatographic separation was performed on a Hypersil C18 column (4.6 mm×250 mm, 5 μm), using a gradient mobile phase system of water-methanol (0.05% formic acid). The detection was accomplished by multiple-reaction monitoring (MRM) scanning via electrospray ionization source operating in the negative ionization mode. The linear range was 1-1,000 ng/mL for geniposidic acid and 0.2-200 ng/mL for aucubin, respectively. The accuracy (relative error, R.E.%) were between -5.40 and 5.00%, while the intra-day and inter-day precisions were less than 7.95 and 7.87% for the two analytes, respectively. The method was fully validated for the sensitivity, selectivity, recovery, matrix effect and stability. Then this method was successfully applied to the pharmacokinetic study of geniposidic acid and aucubin after oral administration of Du-zhong tea extract to rats and the results indicated that this HPLC-MS/MS assay is a valuable method for the pharmacokinetic study of geniposidic acid and aucubin in rat plasma. Copyright © 2014. Published by Elsevier B.V.

  5. A Rare Cause of Metabolic Acidosis: Fatal Transdermal Methanol Intoxication in an Infant.

    Science.gov (United States)

    Sahbudak Bal, Zumrut; Can, Fulya Kamit; Anil, Ayse Berna; Bal, Alkan; Anil, Murat; Gokalp, Gamze; Yavascan, Onder; Aksu, Nejat

    2016-08-01

    Oral methanol intoxication is common, but dermal intoxication is rare. We report a previously healthy 19-month-old female infant admitted to the emergency department (ED) with vomiting and tonic-clonic seizure. On physical examination, she was comatose and presented signs of decompensated shock with Kussmaul breathing. Her left thigh was edematous, with purple coloration. Methanol intoxication was suspected due to high anion gap metabolic acidosis (pH, 6.89; HCO3, metabolic acidosis. This case report demonstrates that fatal transdermal methanol intoxication can occur in children, and it is the second report in the English literature of transdermal methanol intoxication in an infant.

  6. Development of vertical SU-8 microneedles for transdermal drug delivery by double drawing lithography technology.

    Science.gov (United States)

    Xiang, Zhuolin; Wang, Hao; Pant, Aakanksha; Pastorin, Giorgia; Lee, Chengkuo

    2013-01-01

    Polymer-based microneedles have drawn much attention in transdermal drug delivery resulting from their flexibility and biocompatibility. Traditional fabrication approaches are usually time-consuming and expensive. In this study, we developed a new double drawing lithography technology to make biocompatible SU-8 microneedles for transdermal drug delivery applications. These microneedles are strong enough to stand force from both vertical direction and planar direction during penetration. They can be used to penetrate into the skin easily and deliver drugs to the tissues under it. By controlling the delivery speed lower than 2 μl/min per single microneedle, the delivery rate can be as high as 71%.

  7. Transdermal delivery of insulin with bioceramic composite microneedles fabricated by gelatin and hydroxyapatite.

    Science.gov (United States)

    Yu, Weijiang; Jiang, Guohua; Liu, Depeng; Li, Lei; Tong, Zaizai; Yao, Juming; Kong, Xiangdong

    2017-04-01

    The organic-inorganic bioceramic composite microneedles (MNs) were prepared from hydroxyapatite (Hap) and gelatin (Gel) via a template method. The resultant hydroxyapatite and gelatin composite MNs exhibited low cytotoxicity and excellent mechanical properties. After transdermal administration to the diabetic rats, the insulin could be released from bioceramic composite MNs. An obvious and effective hypoglycemic effect could be obtained compared with that of subcutaneous injection route. This work suggests that bioceramic composite MNs containing of insulin have a potential application in diabetes treatment via transdermal ingestion. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Genetic variation in nicotine metabolism predicts the efficacy of extended-duration transdermal nicotine therapy.

    Science.gov (United States)

    Lerman, C; Jepson, C; Wileyto, E P; Patterson, F; Schnoll, R; Mroziewicz, M; Benowitz, N; Tyndale, R F

    2010-05-01

    In a placebo-controlled trial, we examined the efficacy of a 6-month ("extended") transdermal nicotine therapy vs. the 8-week ("standard") therapy in 471 Caucasian smokers with either normal or reduced rates of nicotine metabolism as determined at pretreatment. Extended therapy was superior to standard therapy in genotypic or phenotypic reduced metabolizers (RMs) of nicotine but not in normal metabolizers (NMs). RMs of nicotine are candidates for extended transdermal nicotine therapy, whereas an alternative therapeutic approach may be needed for those with normal rates of nicotine metabolism.

  9. Enrichment of total steroidal saponins from the extracts of Trillium tschonoskii Maxim by macroporous resin and the simultaneous determination of eight steroidal saponins in the final product by HPLC.

    Science.gov (United States)

    Zhou, Yulan; Gao, Xin; Fu, Qiang; Guo, Pengqi; Xu, Xinya; Zhang, Ting; Ge, Yanhui; Zhang, Bilin; Wang, Mingchan; Zeng, Aiguo; Luo, Zhimin; Chang, Chun

    2017-03-01

    An effective and simple method was established for the separation and enrichment of steroidal saponins from Trillium tschonoskii Maxim. The adsorption and desorption properties of seven macroporous resins were investigated. Among the tested resins, AB-8 resin showed the best adsorption and desorption capacities. The adsorption of steroidal saponins on AB-8 at 25°C was quite consistent with both the Freundlich isotherm model and the pseudo-second-order kinetics model. By optimizing the dynamic adsorption and desorption parameters, the content of steroidal saponins increased from 5.20% in the crude extracts to 51.93% in the final product, with a recovery yield of 86.67%. Furthermore, by scale-up separation, the concentration and recovery of total steroidal saponins were 43.8 and 85.5%, respectively, which suggested that AB-8 resin had great industrial and pharmaceutical potential because of its high efficiency and cost-effectiveness. In addition, a high-performance liquid chromatography method for the simultaneous determination of eight steroidal saponins was established for the first time, which was employed to qualitatively and quantitatively analyze the final product. Based on the methodological validation results, the high-performance liquid chromatography method can be widely applied to the quality control of steroidal saponins from Trillium tschonoskii Maxim due to its excellent accuracy, stability, and repeatability. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Simultaneous determination of corosolic acid and euscaphic acid in the plasma of normal and diabetic rat after oral administration of extract of Potentilla discolor Bunge by high-performance liquid chromatography/electrospray ionization mass spectrometry.

    Science.gov (United States)

    Li, Jing-jing; Li, Yi; Bai, Min; Tan, Jing-fu; Wang, Qiang; Yang, Jie

    2014-05-01

    Potentilla discolor Bunge has been used for diabetes in China for a long time. Corosolic acid (CA) and euscaphic acid (EA), with significant anti-diabetic activity, are two major triterpenoids in P. discolor. In this study, a specific, sensitive and convenient LC-MS method has been developed for simultaneous determination of CA and EA in the plasma of normal and diabetic rats after oral administration of the extract of P. discolor. The chromatographic separation was achieved using an Alltima C18 column (53 × 7.0 mm, i.d., 3 µm) with a mobile phase composed of 0.1% formic acid water and 0.1% formic acid acetonitrile at a flow rate of 1.0 mL/min. The detection was performed by MS with electrospray ionization interface in negative selected ion monitoring mode. All the validation data, such as specificity, linearity (r(2)  > 0.9991 within 0.025-10.0 µg/mL), lower limit of quantitation (2.5 ng/mL), precision (intra- and inter-day <14.7%), accuracy (<15.0%), recovery (85.7-110.8%) and stability were determined and all of them were within the required limits. This method was successfully applied for the evaluation of the pharmacokinetic behaviors of these two compounds in the plasma of normal and diabetic rats. Copyright © 2013 John Wiley & Sons, Ltd.

  11. Simultaneous determination of scopoletin, psoralen, bergapten, xanthotoxin, columbianetin acetate, imperatorin, osthole and isoimperatorin in rat plasma by LC-MS/MS for pharmacokinetic studies following oral administration of Radix Angelicae Pubescentis extract.

    Science.gov (United States)

    Chang, Yan-xu; Zhang, Qiu-Hong; Li, Jin; Zhang, Ling; Guo, Xin-rong; He, Jun; Zhang, Peng; Ma, Lin; Deng, Yan-ru; Zhang, Bo-li; Gao, Xiu-mei

    2013-04-15

    A rapid and sensitive bioassay based on liquid chromatography tandem mass spectrometry (LC-MS/MS) has been developed and validated for the simultaneous determination of eight coumarins in rat plasma. The liquid-liquid extraction method with ethyl acetate was used to prepare the plasma samples after addition of warfarin as an internal standard (IS). Chromatographic separation was performed on an Eclipse plus C18 column (100mm×4.6mm, 1.8μm) using gradient elution when 1mM ammonium acetate aqueous solution - acetonitrile was used as the mobile phase. The lower limit of quantitation (LLOQ) of each coumarin was lower than 2.16ngmL(-1). Intra-day and inter-day precisions were less than 15%. The accuracies were in the range of 88.9-117%. The mean recoveries of coumarins and IS were higher than 84%. The method was successfully applied to a pharmacokinetic study of eight coumarins in rats after oral administration of radix angelicae pubescentis. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  12. Extração e fracionamento simultâneo do óleo da castanha-do-Brasil com etanol Extraction and simultaneous separation of the Brazil nuts oil with ethanol

    Directory of Open Access Journals (Sweden)

    Suely Pereira Freitas

    2007-08-01

    Full Text Available O objetivo deste trabalho foi utilizar o etanol comercial para extração e fracionamento simultâneos das frações lipídicas presentes na castanha-do-Brasil (Bertholletia excelsea H.B.K.. O óleo foi obtido a partir da castanha desidratada e moída. O processo foi conduzido na proporção 4:1 solvente/substrato (v.p-1 em banho termostatizado a 65 °C, sob agitação de 30 rpm. A mistura foi filtrada, resfriada a 10 °C e, a seguir, centrifugada para separação das fases: uma fase com consistência de gel (micela rica, contendo 75% de óleo e 25% de etanol, e a outra líquida, contendo 2,4% de óleo e 97,6% de etanol (micela pobre. Pelas características apresentadas, a micela rica tem potencial para ser utilizada no preparo de cremes vegetais como substituto parcial de gorduras hidrogenadas, cujos efeitos biológicos na saúde dos consumidores vêm provocando muitas polêmicas. Além de ser uma alternativa na obtenção de gorduras para a formulação de alimentos mais seguros, a tecnologia proposta poderá ser estendida a diferentes oleaginosas de interesse comercial, eliminando o uso de n-hexano no processamento de óleos e gorduras vegetais.In this work, the extraction and simultaneous separation of lipids from Brazil nuts (Bertholletia excelsa H.B.K. with ethanol were investigated. Brazil nuts were dried and triturated prior to oil extraction. The process was carried out at a rate of 4:1 solvent to substrate (v.w-1. The raw material and ethanol were placed in an erlenmeyer flask and maintained in a temperature-controlled bath at 65 °C and 30 rpm. After 1 hour, the mixture was filtered under a vacuum and the resultant miscella was maintained at 10 °C and centrifuged for phase separation. A rich miscella containing 75% oil and 25% ethanol was obtained presenting a gel consistency while a poor miscella, containing 2.4% oil and 97.6% ethanol, was liquid. The rich miscella presented an important potential to partially replace hydrogenate

  13. Interpretation of urine drug testing results in patients using transdermal buprenorphine preparations for the treatment of chronic noncancer pain.

    Science.gov (United States)

    Markman, John D; Barbosa, William A; Gewandter, Jennifer S; Frazer, Maria; Rast, Shirley; Dugan, Michelle; Nandigam, Kiran; Villareal, Armando; Kwong, Tai C

    2015-06-01

    To determine whether the prevailing liquid chromatography and tandem mass spectroscopy assay (LC-MS/MS) assay designed to monitor buprenorphine compliance of the sublingual formulation used in the substance abuse treatment setting can be extrapolated to the transdermal formulation used in the chronic pain treatment setting, which is 1000-fold less concentrated. Retrospective chart review. Self-reported compliant patients using the transdermal or sublingual formulations of buprenorhphine. Transdermal patch application was also visually confirmed during clinic visits. Urine drug test results from a LC-MS/MS were compared between samples from transdermal and sublingual patients. While all sublingual patients tested positive for at least one metabolite of buprenorphine, only 69% of the transdermal patients did so. In addition, the most abundant metabolite in the transdermal patients was buprenorphine-glucuronide, as compared with norbuprenorphine-glucuronide in sublingual patients. These data suggest that currently available urine drug tests for buprenorphine, including the more expensive LC-MS/MS based assays, may not be sufficiently sensitive to detect the metabolites from transdermal buprenorphine patients. This study highlights the need to evaluate the value and sensitivity of urine drug tests given the wide range of buprenorphine dosing in clinical practice. These results underscore the need for additional cost benefit analyses comparing different confirmatory drug testing techniques including many commercially available drug testing options. © 2014 Wiley Periodicals, Inc. Wiley Periodicals, Inc.

  14. Design of a Dissolving Microneedle Platform for Transdermal Delivery of a Fixed-Dose Combination of Cardiovascular Drugs.

    Science.gov (United States)

    Quinn, Helen L; Bonham, Louise; Hughes, Carmel M; Donnelly, Ryan F

    2015-10-01

    Microneedles (MNs) are a minimally invasive drug delivery platform, designed to enhance transdermal drug delivery by breaching the stratum corneum. For the first time, this study describes the simultaneous delivery of a combination of three drugs using a dissolving polymeric MN system. In the present study, aspirin, lisinopril dihydrate, and atorvastatin calcium trihydrate were used as exemplar cardiovascular drugs and formulated into MN arrays using two biocompatible polymers, poly(vinylpyrrollidone) and poly(methylvinylether/maleic acid). Following fabrication, dissolution, mechanical testing, and determination of drug recovery from the MN arrays, in vitro drug delivery studies were undertaken, followed by HPLC analysis. All three drugs were successfully delivered in vitro across neonatal porcine skin, with similar permeation profiles achieved from both polymer formulations. An average of 126.3 ± 18.1 μg of atorvastatin calcium trihydrate was delivered, notably lower than the 687.9 ± 101.3 μg of lisinopril and 3924 ± 1011 μg of aspirin, because of the hydrophobic nature of the atorvastatin molecule and hence poor dissolution from the array. Polymer deposition into the skin may be an issue with repeat application of such a MN array, hence future work will consider more appropriate MN systems for continuous use, alongside tailoring delivery to less hydrophilic compounds. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  15. Enhanced both in vitro and in vivo kinetics by SLNs induced transdermal system of furosemide: A novel approach.

    Science.gov (United States)

    Mannam, Revathi; Yallamalli, Indira Muzib

    2017-11-28

    Furosemide is a potent diuretic agent used to treat pulmonary arterial hypertension. Variable dosage regimen and poor pharmacokinetic parameters has led to the development of transdermal drug delivery system. A patent on suitability of multi-lamellar structures for excellent transdermal delivery (US 0367475A1) has encouraged us to formulate the solid lipid nanoparticles (SLNs) induced transdermal systems of furosemide to enhance the kinetic properties without incorporating any penetration enhancer and rate limiting polymers. SLNs were prepared by hot homogenization and ultra-sonication method; optimization was done basing on entrapment efficiency and particle size. Optimized SLNs were incorporated in to transdermal patches by solvent casting method. In-vitro and in-vivo studies were carried out for characterization of transdermal patches. SLNs of F9 (GMS: Span 60: Pluronic F 68 in 6:2.5:0.2) were optimized for incorporating in to transdermal system (entrapment efficiency 94.5±0.045%, particle size 69.6±1.48 nm and in-vitro release 94.38±1.02%). Transdermal patches were formulated using combinations of hydrophilic and hydrophobic polymers to study the diffusion kinetics. Formulation FS1 (HPMC 4 parts) was optimized for further studies (in-vitro release 98.11±1.21% with flux of 58.726±0.023 µg/cm2/h) and no significant difference from ex-vivo permeation studies was observed. Drug release followed mixed order diffusion kinetics and super case -II transport mechanism. In-vivo pharmacokinetic data of SLNs induced transdermal system suggested a 3.6 times increase in AUC and 5.4 times increase in MRT when compared with oral route. The SLNs induced transdermal patch was found to beneficial in enhancing kinetic properties both in-vitro and in-vivo. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  16. Fabrication of coated polymer microneedles for transdermal drug delivery.

    Science.gov (United States)

    Chen, Yang; Chen, Bo Zhi; Wang, Qi Lei; Jin, Xuan; Guo, Xin Dong

    2017-03-24

    As an alternative to hypodermic needles, coated polymer microneedles (MNs) are able to deliver drugs to subcutaneous tissues after being inserted into the skin. The dip-coating process is a versatile, rapid fabricating method that can form coated MNs in a short time. However, it is still a challenge to fabricate coated MNs with homogeneous and precise drug doses in the dip-coating process. In this study, to fabricate coated polymer microneedles with controlled drug loading, an adjustable apparatus that can be lifted and lowered was designed to immerse a polylactic acid (PLA) MN patch in the coating solutions. Using the coating solution containing 0.5% (w/w) sulforhodamine B, the drug loadings were up to 12ng, 14ng, and 18ng per needle for the MNs with heights of 550μm, 650μm, and 750μm, respectively. Moreover, for the MNs with a 650-μm height, when increasing the viscosity of the coating solutions from 150mPa·s to 1360mPa·s, 2850mPa·s, and 8200mPa·s, the drug loading increased from 2.5ng to 5ng, 14ng, and 22ng per needle, respectively. Meanwhile, the drug delivery efficiencies of these MNs were approximately 90%. In the insertion experiments, the MNs could successfully penetrate the skin and deliver the coated drug with approximately 90% efficiency when the MN tips were exposed to the outer environment. In vivo studies in mice indicated that the coated polymer MNs continuously delivered drugs, and the skin recovered without any injuries. These results demonstrated that the coated polymer MN was a safe and effective method for transdermal drug delivery. Copyright © 2017. Published by Elsevier B.V.

  17. A minimally invasive microchip for transdermal injection/sampling applications.

    Science.gov (United States)

    Strambini, Lucanos M; Longo, Angela; Diligenti, Alessandro; Barillaro, Giuseppe

    2012-09-21

    The design, fabrication, and characterization of a minimally invasive silicon microchip for transdermal injection/sampling applications are reported and discussed. The microchip exploits an array of silicon-dioxide hollow microneedles with density of one million needles cm(-2) and lateral size of a few micrometers, protruding from the front-side chip surface for one hundred micrometers, to inject/draw fluids into/from the skin. The microneedles are in connection with independent reservoirs grooved on the back-side of the chip. Insertion experiments of the microchip in skin-like polymers (agarose hydrogels with concentrations of 2% and 4% wt) demonstrate that the microneedles successfully withstand penetration without breaking, despite their high density and small size, according to theoretical predictions. Operation of the microchip with different liquids of biomedical interest (deionized water, NaCl solution, and d-glucose solution) at different differential pressures, in the range 10-100 kPa, highlights that the flow-rate through the microneedles is linearly dependent on the pressure-drop, despite the small section area (about 13 μm(2)) of the microneedle bore, and can be finely controlled from a few ml min(-1) up to tens of ml min(-1). Evaporation (at room temperature) and acceleration (up to 80 g) losses through the microneedles are also investigated to quantify the ability of the chip in storing liquids (drug to be delivered or collected fluid) in the reservoir, and result to be of the order of 70 nl min(-1) and 1300 nl min(-1), respectively, at atmospheric pressure and room temperature.

  18. Mechanism of transdermal permeation promotion of lipophilic drugs by ethosomes.

    Science.gov (United States)

    Yang, Li; Wu, Lifang; Wu, Dongze; Shi, Deshun; Wang, Tai; Zhu, Xiaoliang

    2017-01-01

    Ethosomes can promote the penetration of lipophilic drugs into the skin, but the underlying mechanism is still unknown. The purpose of this study was to investigate the mechanism of transdermal permeation promotion of lipophilic drugs by ethosomes. The formulation of ethosomes was optimized using the Box-Behnken experimental design, in which Rhodamine B and 1-palmitoyl-2-{12-[(7-nitro-2-1,3-benzoxadiazol-4-yl)amino]dodecanoyl}-sn-glycero-3-phosphocholine were used to simulate a model lipophilic drug and act as a fluorescent tracer of ethosomal phospholipids, respectively. Liposomes with the same phospholipid concentration and a hydroethanolic solution with the same ethanol concentration were also prepared as controls. The percutaneous progression of the above fluorescent preparations was observed by confocal laser scanning microscopy, and the fluorescence intensity of the images was analyzed. The optimized ethosome formulation consisted of 2.45% yolk phospholipids, 30% ethanol, and 67.55% distilled water. The percutaneous permeation of Rhodamine B in the optimized ethosomes was superior to that in hydroethanolic solution (Pethosomes could penetrate the skin via the percutaneous pathway of the hair follicle and stratum corneum, while during the process of penetration, the vesicles were broken and the phospholipids were retained in the upper epidermis, with the test compounds penetrating gradually. The superior percutaneous penetration of ethosomes was linked to the synergistic effects of their ingredients. The percutaneous pathways of ethosomes included open hair follicles and stratum corneum pathways. In addition, the vesicles might break up during percutaneous penetration in the superficial layer of the skin, allowing the test compounds to keep permeating into the deeper layer alone, while the phospholipid was retained in the upper epidermis.

  19. Transdermal nicotine absorption handling e-cigarette refill liquids.

    Science.gov (United States)

    Maina, Giovanni; Castagnoli, Carlotta; Passini, Valter; Crosera, Matteo; Adami, Gianpiero; Mauro, Marcella; Filon, Francesca Larese

    2016-02-01

    The concentrated nicotine in e-cigarette refill liquids can be toxic if inadvertently ingested or absorbed through the skin. Reports of poisonings due to accidental ingestion of nicotine on refill liquids are rapidly increasing, while the evaluation of nicotine dermally absorbed still lacks. For that reason we studied transdermal nicotine absorption after the skin contamination with e-liquid. Donor chambers of eight Franz diffusion cells were filled with 1 mL of 0.8 mg/mL nicotine e-liquid for 24 h. The concentration of nicotine in the receiving phase was determined by high-performance liquid chromatography (LOD:0.1 μg/mL). Nicotine was detectable in receiving solution 2 h after the start of exposure and increased progressively. The medium flux calculated was 4.82 ± 1.05 μg/cm(2)/h with a lag time of 3.9 ± 0.1 h. After 24 h, the nicotine concentration in the receiving compartment was 101.02 ± 22.35 μg/cm(2) corresponding to 3.04 mg of absorbed nicotine after contamination of a skin surface of 100 cm(2). Skin contamination with e-liquid can cause nicotine skin absorption: caution must be paid when handling refill e-liquids. Copyright © 2015 Elsevier Inc. All rights reserved.

  20. The pharmacokinetics of transdermal flunixin meglumine in Holstein calves.

    Science.gov (United States)

    Kleinhenz, M D; Van Engen, N K; Gorden, P J; KuKanich, B; Rajewski, S M; Walsh, P; Coetzee, J F

    2016-12-01

    This study describes the pharmacokinetics of topical and intravenous (IV) flunixin meglumine in Holstein calves. Eight male Holsteins calves, aged 6 to 8 weeks, were administered flunixin at a dose of 2.2 mg/kg intravenously. Following a 10-day washout period, calves were dosed with flunixin at 3.33 mg/kg topically (transdermal). Blood samples were collected at predetermined times from 0 to 48 h for the intravenous portions and 0 to 72 h following topical dosing. Plasma drug concentrations were determined using liquid chromatography with mass spectroscopy. Pharmacokinetic analysis was completed using noncompartmental methods. The mean bioavailability of topical flunixin was calculated to be 48%. The mean AUC for flunixin was determined to be 13.9 h × ug/mL for IV administration and 10.1 h × ug/mL for topical administration. The mean half-life for topical flunixin was 6.42 h and 4.99 h for the intravenous route. The C max following topical application of flunixin was 1.17 μg/mL. The time to maximum concentration was 2.14 h. Mean residence time (MRT) following IV injection was 4.38 h and 8.36 h after topical administration. In conclusion, flunixin when administered as a topical preparation is rapidly absorbed and has longer half-life compared to IV administration. © 2016 John Wiley & Sons Ltd.

  1. Transdermal influenza immunization with vaccine-coated microneedle arrays.

    Directory of Open Access Journals (Sweden)

    Dimitrios G Koutsonanos

    Full Text Available Influenza is a contagious disease caused by a pathogenic virus, with outbreaks all over the world and thousands of hospitalizations and deaths every year. Due to virus antigenic drift and short-lived immune responses, annual vaccination is required. However, vaccine coverage is incomplete, and improvement in immunization is needed. The objective of this study is to investigate a novel method for transdermal delivery using metal microneedle arrays (MN coated with inactivated influenza virus to determine whether this route is a simpler and safer approach than the conventional immunization, capable to induce robust immune responses and confer protection against lethal virus challenge.Inactivated A/Aichi/2/68 (H3N2 influenza virus was coated on metal microneedle arrays and applied to mice as a vaccine in the caudal dorsal skin area. Substantial antibody titers with hemagglutination inhibition activity were detected in sera collected two and four weeks after a single vaccine dose. Challenge studies in mice with 5 x LD(50 of mouse adapted Aichi virus demonstrated complete protection. Microneedle vaccination induced a broad spectrum of immune responses including CD4+ and CD8+ responses in the spleen and draining lymph node, a high frequency of antigen-secreting cells in the lung and induction of virus-specific memory B-cells. In addition, the use of MN showed a dose-sparing effect and a strong Th2 bias when compared to an intramuscular (IM reference immunization.The present results show that delivery of inactivated influenza virus through the skin using metal microneedle arrays induced strong humoral and cellular immune responses capable of conferring protection against virus challenge as efficiently as intramuscular immunization, which is the standard vaccination route. In view of the convenience of delivery and the potential for self-administration, vaccine-coated metal microneedles may provide a novel and highly effective immunization method.

  2. Treatment with subcutaneous and transdermal fentanyl: Results from a population pharmacokinetic study in cancer patients

    NARCIS (Netherlands)

    A.W. Oosten (Astrid); J.A. Abrantes (João A.); S. Jönsson (Siv); P. de Bruijn (Peter); E.J.M. Kuip (Evelien); A. Falcão (Amílcar); C.C.D. van der Rijt (Carin); A.H.J. Mathijssen (Ron)

    2016-01-01

    textabstractPurpose: Transdermal fentanyl is effective for the treatment of moderate to severe cancer-related pain but is unsuitable for fast titration. In this setting, continuous subcutaneous fentanyl may be used. As data on the pharmacokinetics of continuous subcutaneous fentanyl are lacking, we

  3. Treatment with subcutaneous and transdermal fentanyl: results from a population pharmacokinetic study in cancer patients

    NARCIS (Netherlands)

    Oosten, A.W.; Abrantes, J.A.; Jonsson, S.; Bruijn, P. de; Kuip, E.J.M.; Falcao, A.; Rijt, C.C. van der; Mathijssen, R.H.

    2016-01-01

    PURPOSE: Transdermal fentanyl is effective for the treatment of moderate to severe cancer-related pain but is unsuitable for fast titration. In this setting, continuous subcutaneous fentanyl may be used. As data on the pharmacokinetics of continuous subcutaneous fentanyl are lacking, we studied the

  4. Methylphenidate Transdermal System in Adult ADHD and Impact on Emotional and Oppositional Symptoms

    Science.gov (United States)

    Marchant, Barrie K.; Reimherr, Frederick W.; Robison, Reid J.; Olsen, John L.; Kondo, Douglas G.

    2011-01-01

    Objective: This trial evaluated the effect of methylphenidate transdermal system (MTS) on the full spectrum of adult symptoms (attention-disorganization, hyperactivity-impulsivity, emotional dysregulation [ED], and oppositional-defiant disorder [ODD]) found in this disorder. Method: This placebo-controlled, double-blind, flexible-dose, crossover…

  5. Alfuzosin hydrochloride transdermal films: evaluation of physicochemical, in vitro human cadaver skin permeation and thermodynamic parameters

    Directory of Open Access Journals (Sweden)

    Satyanarayan Pattnaik

    2009-12-01

    Full Text Available Purpose: The main objective of the investigation was to develop a transdermal therapeutic system for alfuzosin hydrochloride and to study the effects of polymeric system and loading dose on the in vitro skin permeation pattern. Materials and methods: Principles of experimental design have been exploited to develop the dosage form. Ratio of ethyl cellulose (EC and polyvinyl pyrrolidone (PVP and loading dose were selected as independent variables and their influence on the cumulative amount of alfuzosin hydrochloride permeated per cm2 of human cadaver skin at 24 h (Q24, permeation flux (J and steady state permeability coefficient (P SS were studied using experimental design. Various physicochemical parameters of the transdermal films were also evaluated. Activation energy for in vitro transdermal permeation has been estimated. Results: Ratio of EC and PVP was found to be the main influential factor for all the dependent variables studied. Drug loading dose was also found to influence the dependent variables but to a lesser extent. Physicochemical parameters of the prepared films were evaluated and found satisfactory. Activation energy for alfuzosin permeation has also been estimated and reported. Conclusion: The therapeutic system was found to be dermatologically non-irritant and hence, a therapeutically effective amount of alfuzosin hydrochloride can be delivered via a transdermal route.

  6. Double-layer weekly sustained release transdermal patch containing gestodene and ethinylestradiol.

    Science.gov (United States)

    Gao, Yanli; Liang, Jinying; Liu, Jianping; Xiao, Yan

    2009-07-30

    The combination therapy of gestodene (GEST) and ethinylestradiol (EE) has shown advanced contraception effect and lower side effect. The present study was designed to develop a weekly sustained release matrix type transdermal patch containing GEST and EE using blends of different polymeric combinations. The multiple-layer technique was adopted in order to maintain a steady permeation flux for 7 days. The effects of polymer types, polymer ratios, permeation enhancers, drug loadings and drug ratios in different layers on the skin permeations of the drugs were evaluated using excised mice skin. Polariscope examination was carried out to observe the drug distribution behavior. The formulation with the mixture of polyvinyl alcohol (PVA) and polyvinyl pyrrolidone (PVP) (7:1) was found to provide the regular release and propylene glycol (PG) could enhance the permeation fluxes of drugs. Double-layer transdermal drug delivery system (TDDS) could sustain the steady permeation flux of drugs for 7 days when the ratio of drug in drug release layer and drug reservoir layer was 1:4 with the identical total drug amount. The in vitro transdermal permeation fluxes were 0.377 microg/cm(2)/h and 0.092 microg/cm(2)/h, for GEST and EE respectively. The uniformity of dosage units test showed that the distribution of drugs in the matrix was homogeneous, which was further demonstrated by the polariscope result. The developed transdermal delivery system containing GEST and EE could be a promising non-oral contraceptive method.

  7. Transdermal iontophoresis of the dopamine agonist 5-OH-DPAT in human skin in vitro

    NARCIS (Netherlands)

    Nugroho, AK; Li, L; Dijkstra, D; Wikstrom, H; Danhof, M; Bouwstra, JA

    2005-01-01

    The feasibility of transdermal iontophoretic delivery of a potent dopamine agonist 5-OH-DPAT was studied in vitro in side by side diffusion cells across human stratum corneum (HSC) and dermatomed human skin (DHS) according to the following protocol: 6 h of passive diffusion, 9 h of iontophoresis and

  8. Buprenorphine Transdermal System for Opioid Therapy in Patients with Chronic Low Back Pain

    Directory of Open Access Journals (Sweden)

    Allan Gordon

    2010-01-01

    Full Text Available OBJECTIVE: The present randomized, double-blinded, crossover study compared the efficacy and safety of a seven-day buprenorphine transdermal system (BTDS and placebo in patients with low back pain of moderate or greater severity for at least six weeks.

  9. Functionalization of Cotton Fabrics with Polycaprolactone Nanoparticles for Transdermal Release of Melatonin

    Directory of Open Access Journals (Sweden)

    Daniele Massella

    2017-12-01

    Full Text Available Drug delivery by means of transdermal patches raised great interest as a non-invasive and sustained therapy. The present research aimed to design a patch for transdermal delivery of melatonin, which was encapsulated in polycaprolactone (PCL nanoparticles (NPs by employing flash nanoprecipitation (FNP technique. Melatonin-loaded PCL nanoparticles were successfully prepared with precise control of the particle size by effectively tuning process parameters. The effect of process parameters on the particle size was assessed by dynamic light scattering for producing particles with suitable size for transdermal applications. Quantification of encapsulated melatonin was performed by mean of UV spectrophotometry, obtaining the estimation of encapsulation efficiency (EE% and loading capacity (LC%. An EE% higher than 80% was obtained. Differential scanning calorimetry (DSC analysis of NPs was performed to confirm effective encapsulation in the solid phase. Cotton fabrics, functionalized by imbibition with the nano-suspension, were analyzed by scanning electron microscopy to check morphology, adhesion and distribution of the NPs on the surface; melatonin transdermal release from the functionalized fabric was performed via Franz’s cells by using a synthetic membrane. NPs were uniformly distributed on cotton fibres, as confirmed by SEM observations; the release test showed a continuous and controlled release whose kinetics were satisfactorily described by Baker–Lonsdale model.

  10. FORMULASI MATRIKS TRANSDERMAL PENTAGAMAVUNON-0 DENGAN KOMBINASI POLIMER PVP K30 DAN HIDROKSIPROPIL METILSELULOSA

    Directory of Open Access Journals (Sweden)

    Beti Pudyastuti

    2016-04-01

    Full Text Available Abstract: Transdermal delivery system is one of the delivery system for Pentagamavunon-0 (PGV-0 to avoid the high intensity of first pass metabolism of PGV-0 in peroral route. The purpose of this research was to optimize the formula of PGV-0 transdermal matrix with a combination of PVP K30 and HPMC polymers.The simplex lattice optimization approach of the transdermal matrix formulas was performed by using Design Expert 7.1.5 software. The visual appearance, weight, thickness, moisture content, moisture uptake, folding endurance, drug content, and dissolution efficiency of the release profil of PGV-0 from the matrix for 6 hours were evaluated as responses to determine optimum formula of matrix. The result showed that a combination of PVP K30 and HPMC polymers had a significant influence on the visual appearance, moisture content, and dissolution efficiency of PGV-0. Combination of 1.98% of PVP K30 and 4.52% of HPMC as the optimum formula could produce homogeneous and flexible matrix with moisture content of 3.21%. The dissolution efficiency was 9.11%, indicating that 101.93 µg of PGV-0 was released from the optimum formula during 6 hours. Keywords : Pentagamavunon-0, Transdermal matrix, PVP K30, HPMC

  11. P-Glycoprotein in skin contributes to transdermal absorption of topical corticosteroids.

    Science.gov (United States)

    Hashimoto, Naoto; Nakamichi, Noritaka; Yamazaki, Erina; Oikawa, Masashi; Masuo, Yusuke; Schinkel, Alfred H; Kato, Yukio

    2017-04-15

    ATP binding cassette transporters, P-glycoprotein (P-gp) and breast cancer resistance protein (BCRP), are expressed in skin, but their involvement in transdermal absorption of clinically used drugs remains unknown. Here, we examined their role in transdermal absorption of corticosteroids. Skin and plasma concentrations of dexamethasone after dermal application were reduced in P-gp and BCRP triple-knockout (Mdr1a/1b/Bcrp(-/-)) mice. The skin concentration in Mdr1a/1b/Bcrp(-/-) mice was reduced in the dermis, but not in the epidermis, indicating that functional expression of these transporters in skin is compartmentalized. Involvement of these transporters in dermal transport of dexamethasone was also supported by the observation of a higher epidermal concentration in Mdr1a/1b/Bcrp(-/-) than wild-type mice during intravenous infusion. Transdermal absorption after dermal application of prednisolone, but not methylprednisolone or ethinyl estradiol, was also lower in Mdr1a/1b/Bcrp(-/-) than in wild-type mice. Transport studies in epithelial cell lines transfected with P-gp or BCRP showed that dexamethasone and prednisolone are substrates of P-gp, but are minimally transported by BCRP. Thus, our findings suggest that P-gp is involved in transdermal absorption of at least some corticosteroids in vivo. P-gp might be available as a target for inhibition in order to deliver topically applied drugs and cosmetics in a manner that minimizes systemic exposure. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Ethosomes as Vesicles for Effective Transdermal Delivery: From Bench to Clinical Implementation.

    Science.gov (United States)

    Akhtar, Nida; Varma, Anurag; Pathak, Kamla

    2016-01-01

    Drug delivery across the deeper layers of skin to make it systemically available is a considerable challenge in the development of a carrier. Numerous efforts have been put forward to find ways to overcome the formidable barrier of stratum corneum. Various lipid based vesicles viz liposomes, transfersomes, and invasomes have gained prominent deliberations across the globe. More recently, ethosomes have been investigated for their potential for transdermal delivery of several drugs. In the present review an attempt has been made to illustrate preclinical and clinical studies depicting enhanced safety and efficacy of drugs delivered via ethosomes. Further, patents on transdermal delivery have been highlighted specifying the effectiveness of ethosomes in the transport of therapeutic actives. Through the search engine "Scopus" literature on therapeutic categories such as antimicrobials, anti-inflammatory, and drugs acting on CNS has been collected. Preclinical and clinical studies that have been carried out by various researchers affirm the potentiality of ethosomes for delivering wide variety of drugs belonging to different therapeutic categories. In vitro and in vivo permeability analyses delineated the enhancement of permeability. Consequently, enhanced transdermal flux was reported and in vivo confocal laser scanning microscopy depicted the quantity as well as depth of penetrability via ethosomes. From various research reports, it can be concluded that ethosomes are the competent and efficient vesicles to provide better drug transport via transdermal route.

  13. A study on ethosomes as mode for transdermal delivery of an antidiabetic drug.

    Science.gov (United States)

    Bodade, Siddhodhan S; Shaikh, Karimunnisa Sameer; Kamble, Meghana S; Chaudhari, Praveen D

    2013-01-01

    A transdermal delivery system is warranted for repaglinide (RPG) which possesses half-life of 1 h and oral bioavailability of 56%. Ethosomes are useful tools for transdermal drug delivery. To prepare and evaluate ethosomes as mode for transdermal delivery of RPG. Ethosomes loaded with RPG were prepared from dipalmitoyl phosphatidylcholine and ethanol by the cold method. They were characterized using Fourier transform infrared spectroscopy and differential scanning calorimetry. They were evaluated for vesicle size, entrapment efficiency and ex-vivo skin permeation. Ethosomal composition was optimized using the 3(2) factorial design. Gel containing optimzsed ethosomes was studied for antidiabetic activity in rats. RPG ethosomes possessing the size of 0.171-1.727 µm and entrapment efficiency of 75-92% were obtained. They demonstrated a significantly higher permeation (64-97% of the administered dose) across excised rat skin when compared to free drug and its hydro alcoholic solution. In-vivo, RPG ethosomal system caused sustained antidiabetic effect. The lipid and ethanol concentration affected the physicochemical attributes and performance of ethosomes. The flexible ethosomes permeated the stratum corneum and improvized the availability of RPG for antidiabetic action. They prolonged the antidiabetic effect of RPG over a significantly longer period of time in comparison with the equivalent oral dose. Ethosomal system can successfully deliver RPG transdermally; sustain its effect and thus reduce its dosing frequency. Ethosomes are useful for enhancing the efficacy of RPG in the treatment of diabetes.

  14. Arbutin encapsulated micelles improved transdermal delivery and suppression of cellular melanin production.

    Science.gov (United States)

    Liang, Ke; Xu, Keming; Bessarab, Dmitri; Obaje, Jonathan; Xu, Chenjie

    2016-04-30

    Hyperpigmentation is a skin disorder characterized by elevated production of melanin. Current treatment approaches mainly rely on the application of skin lightening chemicals, most of which have safety issues. Efficacy of delivery of the active ingredients to the target organ has also been a challenge. Transdermal based drug delivery platform has been shown to improve drug bioavailability, avoiding the hepatic first pass metabolism, decrease gastrointestinal side effects, and eventually enhance patient compliance. This article explores the utilization of micellar transdermal delivery technology to improve skin penetration and efficacy of arbutin, a hyperpigmentation agent. The suppression efficacy of cellular melanin production versus cell viability of four active ingredients commonly used in skin lightening products, namely allantoin, arbutin, glycolic acid, and hyaluronic acid were first compared. Arbutin was selected for the micellar delivery studies base on its comparatively low cytotoxicity and better performance in reducing melanin production. Micellar Arbutin cream was formulated using Urah® proprietary micellar technology and was assessed for its cellular melanin suppression efficacy and skin penetration capacity. The results show that micellar arbutin cream improved both the delivery and cellular melanin suppression, suggesting that micellar transdermal delivery may have potential application in addressing hyperpigmentation skin disorders. Graphical abstract Transdermal delivery of arbutin with micelles for melanin production suppression.

  15. Pharmacokinetics of multiple doses of transdermal flunixin meglumine in adult Holstein dairy cows.

    Science.gov (United States)

    Kleinhenz, M D; Gorden, P J; Smith, J S; Schleining, J A; Kleinhenz, K E; Wulf, L L; Sidhu, P K; Rea, D; Coetzee, J F

    2018-02-20

    A transdermal formulation of the nonsteroidal anti-inflammatory drug, flunixin meglumine, has been approved in the United States and Canada for single-dose administration. Transdermal flunixin meglumine was administered to 10 adult Holstein cows in their second or third lactation at the label dose of 3.33 mg/kg every 24 hr for three total treatments. Plasma flunixin concentrations were determined using high-pressure liquid chromatography with mass spectroscopy (HPLC-MS). Pharmacokinetic analysis was completed on each individual animal with noncompartmental methods using computer software. The time to maximum drug concentration (Tmax) was 2.81 hr, and the maximum drug concentration was 1.08 μg/ml. The mean terminal half-life (T½) was determined to be 5.20 hr. Clearance per fraction absorbed (Cl/F) was calculated to be 0.294 L/hr kg -1 , and volume of distribution of fraction (Vz/F) absorbed was 2.20 L/kg. The mean accumulation factor was 1.10 after three doses. This indicates changes in dosing may not be required when giving multiple doses of flunixin transdermal. Further work is required to investigate the clinical efficacy of transdermal flunixin after multiple daily doses. © 2018 John Wiley & Sons Ltd.

  16. An improved model for studies on transdermal drug absorption in-vivo in rats

    NARCIS (Netherlands)

    Vollmer, U.; Muller, B.W.; Wilffert, B.; Peters, Thies

    1993-01-01

    In rats, transdermal drug absorption can be studied under physiological conditions cannulating the peripheral skin vein, draining the area of the skin which is used for drug application, and collecting the blood. This method leads to decreased blood volume, which causes a reduction in skin blood

  17. Transdermal Delivery and Cutaneous Targeting of Antivirals using a Penetration Enhancer and Lysolipid Prodrugs

    Czech Academy of Sciences Publication Activity Database

    Diblíková, D.; Kopečná, M.; Školová, B.; Krečmerová, Marcela; Roh, J.; Hrabálek, A.; Vávrová, K.

    2014-01-01

    Roč. 31, č. 4 (2014), s. 1071-1081 ISSN 0724-8741 Grant - others:GA ČR(CZ) GAP207/11/0365 Institutional support: RVO:61388963 Keywords : acyclic nucleoside phosphonate antivirals * lysolipid prodrug * penetration enhancer * skin absorption * transdermal drug delivery Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 3.420, year: 2014

  18. Low dose transdermal estradiol induces breast density and heterogeneity changes comparable to those of raloxifene

    DEFF Research Database (Denmark)

    Nielsen, Mads; Raundahl, Jakob; Pettersen, Paola

    2009-01-01

    Objective: To investigate whether transdermal low dose estradiol treatment induces changes in mammographic density or heterogeneity compared to raloxifene. Secondarily, if these changes relate to changes in bone formation/resorption markers, and if these findings indicate elevation of breast cancer...

  19. Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

    Science.gov (United States)

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

    2013-01-01

    A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

  20. Pharmacokinetic studies of meloxicam following oral and transdermal administration in Beagle dogs

    Science.gov (United States)

    Yuan, Yue; Chen, Xiao-yan; Li, San-ming; Wei, Xiu-yan; Yao, Hui-min; Zhong, Da-fang

    2009-01-01

    Aim: The potential for topical delivery of meloxicam was investigated by examining its pharmacokinetic profiles in plasma and synovial fluid following oral and transdermal administration in Beagle dogs. Methods: The experiment was a two-period, crossover design using 6 Beagle dogs. Meloxicam tablets were administered orally at a dose of 0.31 mg/kg, and meloxicam gel was administered transdermally at a dose of 1.25 mg/kg. Drug concentrations in plasma and synovial fluid were determined by liquid chromatography-tandem mass spectrometry (LC/MS/MS). The pharmacokinetic parameters were calculated using the Topfit 2.0 program. Results: The pharmacokinetic results showed that AUC0–t (23.9±8.26 μg.h.mL−1) in plasma after oral administration was significantly higher than after transdermal delivery (1.00±0.43 μg.h.mL−1). In contrast, the ratio of the average concentration in synovial fluid to that in plasma following transdermal administration was higher than that for an oral delivery. The synovial fluid concentration in the treated leg was much higher than that in the untreated leg, whereas the synovial fluid concentration in the untreated leg was similar to the plasma concentration. Conclusion: The high concentration ratio of synovial fluid to plasma indicates direct penetration of meloxicam following topical administration to the target tissue. This finding is further supported by the differences observed in meloxicam concentrations in synovial fluid in the treated and untreated joints at the same time point. Our results suggest that transdermal delivery of meloxicam is a promising method for decreasing its adverse systemic effects. PMID:19543299

  1. Transdermal delivery of isoniazid and rifampin in guinea pigs by electro-phonophoresis.

    Science.gov (United States)

    Chen, Suting; Han, Yi; Yu, Daping; Huo, Fengmin; Wang, Fen; Li, Yunxu; Dong, Lingling; Liu, Zhidong; Huang, Hairong

    2017-11-01

    Electro-phonophoresis (EP) has been used as a drug delivery approach in clinical fields. The objective of the present study is to evaluate the skin permeability of isoniazid and rifampin in guinea pigs by EP to provide reference basis for clinical applications of such transdermal delivery system in the treatment of patients with superficial tuberculosis. Isoniazid and rifampin solutions were delivered transdermally with or without EP in health guinea pigs for 0.5 h. Local skin and blood samples were collected serially at 0, 1/2, 1, 2, 4, 6 and 24 h after dosing. Drug concentrations in local skin and blood were evaluated by high-performance liquid chromatography. Isoniazid concentrations in local skin of guinea pigs receiving isoniazid through EP transdermal delivery were significantly higher than in animals receiving only isoniazid with transdermal patch. However, for rifampin, patches alone group presented almost uniform concentration versus time curve with that of EP group, and both groups had concentrations much higher than the therapeutic concentration of the drug over sustainable time. After EP transdermal delivery, the mean peak concentrations of isoniazid and rifampin in skin were 771.0 ± 163.4 μg/mL and 81.2 ± 17.3 μg/mL respectively. Neither isoniazid nor rifampin concentration in blood could be detected (below the lower detection limit of 1 μg/mL) at any time point. The present study showed that application of EP significantly enhanced INH penetration through skin in guinea pigs, while RIF patch alone obtained therapeutic concentration in local skin. Our work suggests several possible medication approaches for efficient treatment of superficial tuberculosis.

  2. Melatonin pharmacokinetics after transdermal administration changes according to the time of the day.

    Science.gov (United States)

    Flo, Ana; Cambras, Trinitat; Díez-Noguera, Antoni; Calpena, Ana

    2017-01-01

    Melatonin is a neurohormone with multiple and different actions, such as chronobiotic or antioxidant. Melatonin is usually orally administered, but dermal administration is also useful in dermatological diseases or as adjuvant to certain skin treatments. Here, we studied the variability of the pharmacokinetics of melatonin and its metabolite AFMK, when melatonin is transdermally administered to Hairless rat at two different times of day (Zeitgeber Time 4 (ZT4) and ZT16). Moreover, in order to obtain the bioavailability, kinetics after intravenous administration was also studied. In addition, a permeation study was carried out, at both ZTs, to test the amount of melatonin retained in the skin after transdermal administration. Results showed that pharmacokinetic parameters of melatonin administered exogenously depended on the time of the day. When intravenous data were fitted to a compartmental model, the extrapolated plasma concentration at time 0 and the area under the curve were higher at ZT4, while clearance, volumes of central and peripheral compartments and volume of distribution at the steady state were higher at ZT16. Transdermal administration was best fitted to a one-compartment model and tmax, half-life of absorption and area under the curve showed higher values at ZT4, while the absorption rate and constant of absorption were higher at ZT16. AFMK was detected in all cases, but no differences between the two ZTs were observed. Transdermal administration showed better bioavailability also at ZT4. Results indicate that time of day is a variable that should be taken into account when melatonin is transdermally administered. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Transdermal film-loaded finasteride microplates to enhance drug skin permeation: Two-step optimization study.

    Science.gov (United States)

    Ahmed, Tarek A; El-Say, Khalid M

    2016-06-10

    The goal was to develop an optimized transdermal finasteride (FNS) film loaded with drug microplates (MIC), utilizing two-step optimization, to decrease the dosing schedule and inconsistency in gastrointestinal absorption. First; 3-level factorial design was implemented to prepare optimized FNS-MIC of minimum particle size. Second; Box-Behnken design matrix was used to develop optimized transdermal FNS-MIC film. Interaction among MIC components was studied using physicochemical characterization tools. Film components namely; hydroxypropyl methyl cellulose (X1), dimethyl sulfoxide (X2) and propylene glycol (X3) were optimized for their effects on the film thickness (Y1) and elongation percent (Y2), and for FNS steady state flux (Y3), permeability coefficient (Y4), and diffusion coefficient (Y5) following ex-vivo permeation through the rat skin. Morphological study of the optimized MIC and transdermal film was also investigated. Results revealed that stabilizer concentration and anti-solvent percent were significantly affecting MIC formulation. Optimized FNS-MIC of particle size 0.93μm was successfully prepared in which there was no interaction observed among their components. An enhancement in the aqueous solubility of FNS-MIC by more than 23% was achieved. All the studied variables, most of their interaction and quadratic effects were significantly affecting the studied variables (Y1-Y5). Morphological observation illustrated non-spherical, short rods, flakes like small plates that were homogeneously distributed in the optimized transdermal film. Ex-vivo study showed enhanced FNS permeation from film loaded MIC when compared to that contains pure drug. So, MIC is a successful technique to enhance aqueous solubility and skin permeation of poor water soluble drug especially when loaded into transdermal films. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Effect of transdermal hormone therapy on platelet haemostasis in menopausal women

    Directory of Open Access Journals (Sweden)

    Grzegorz Stachowiak

    2015-02-01

    Full Text Available [b]Introduction[/b]. Despite the undeniably positive effect on the quality of life of menopausal women, menopausal hormone therapy (HT also has negative side-effects, which include, among others, thromboembolic complications. [b]objective[/b]. To assess the effect of a popular type of this therapy – transdermal HT on platelet hemostasis, which plays a significant role in intravascular coagulation. [b]Materials and method[/b]. The study group consisted of 92 postmenopausal women: 1 group G1 (n=30, treated with transdermal HT (17β-estradiol 50 μg/day plus NETA 170 μg/day; 2 group G2 (n=31, treated with the above transdermal HT and low dosage of acetylsalicylic acid (ASA; 3 control group P (n=31. All the women qualified for the study had two or more risk factors for arterial thrombosis, such as: smoking, hypertension, visceral obesity, hypercholesterolaemia, hypertriglyceridaemia, elevated levels of PAI-1, and increased fibrinogen, increased activity of coagulation factor VII. Results. After three months of therapy, in the G1 group there was a decrease in platelet count (p = 0.004 and a decrease in GP IIb/IIIa – a platelet receptor for fibrinogen (p = 0.022. In the G2 group, no changes in the tested parameters were observed. conclusions. 1 Transdermal HT in the form of combined, estrogen-progestogen patches favourably modifies platelets haemostasis, reversing the adverse effects that occur after menopause. 2 The use of low ASA doses as a thromboprophylaxis in short-term transdermal HT is not necessary.

  5. Transdermal Drug Delivery: Opportunities and Challenges for Controlled Delivery of Therapeutic Agents Using Nanocarriers.

    Science.gov (United States)

    Kurmi, Balak Das; Tekchandani, Pawan; Paliwal, Rishi; Paliwal, Shivani Rai

    2017-01-01

    Transdermal drug delivery represents an extremely attractive and innovative route across the skin owing to the possibility for achieving systemic effect of drugs. The present scenario demands a special focus on developing safe medicine with minimized toxic adverse effects related to most of the pharmacologically active agents. Transdermal drug delivery would be a focal paradigm which provides patient convenience, first-pass hepatic metabolism avoidance, local targeting and reduction in toxic effect related to various categories of drugs like, analgesics, antiinflammatory, antibiotics, antiviral, anaesthetic, anticancer etc. Even this route has challenges due to highly organized structure of skin which acts as a main barrier to penetration of drug via the skin. Several alternative possible strategies are available which overcome these barriers, including use of penetration enhancer, eletroporation, iontophoresis and various nanotechnologically developed nanocarrier systems. The latest one includes employing liposome, dendrimers, nanoparticles, ethosome, carbon nanotube and many more to avoid associated limitations of conventional formulations. Numerous transdermal products such as Estrasorb, Diractin, VivaGel®, Daytrana®, Aczone, Sileryst® are available in the market having a novel strategy to achieve higher penetration of drugs. This encourages formulation fraternity to develop structurally deformable and stable nanocarriers as an alternative approach for controlled and reliable drug delivery across the skin barrier. In this review, we will discuss nanocarriers mediated approaches that come-up with the solutions to the different challenges towards transdermal drug delivery, its clinical importance and latest insight to research in it. The reports presented in this review confirm the wide application of nanocarriers for transdermal delivery of drug/gene. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  6. A preliminary study of painless and effective transdermal botulinum toxin A delivery by jet nebulization for treatment of primary hyperhidrosis

    National Research Council Canada - National Science Library

    Iannitti, Tommaso; Palmieri, Beniamino; Aspiro, Anna; Di Cerbo, Alessandro

    2014-01-01

    ...™-3, a medical device used for transdermal delivery of drugs by jet nebulization, could be used to deliver lidocaine prior to the standard multiple BTX-A injections or deliver lidocaine together...

  7. An experimental trial exploring the impact of continuous transdermal alcohol monitoring upon alcohol consumption in a cohort of male students

    National Research Council Canada - National Science Library

    Neville, Fergus G; Williams, Damien J; Goodall, Christine A; Murer, Jeffrey S; Donnelly, Peter D

    2013-01-01

    .... Participants in Conditions A and B were asked not to consume alcohol for a 14-day period, with those in Condition A additionally being required to wear a continuous transdermal alcohol monitoring anklet...

  8. Genetic, pathological and physiological determinants of transdermal fentanyl pharmacokinetics in 620 cancer patients of the EPOS study

    DEFF Research Database (Denmark)

    Barratt, Daniel T; Bandak, Benedikte; Klepstad, Pål

    2014-01-01

    This study aimed to investigate whether CYP3A4/5 genetic variants, together with clinical and patient factors, influence serum fentanyl and norfentanyl concentrations and their ratio in cancer pain patients receiving transdermal fentanyl.......This study aimed to investigate whether CYP3A4/5 genetic variants, together with clinical and patient factors, influence serum fentanyl and norfentanyl concentrations and their ratio in cancer pain patients receiving transdermal fentanyl....

  9. Formulation, in vitro release and transdermal diffusion of pravastatin by the implementation of the delivery gap principle / Cornel Burger

    OpenAIRE

    Burger, Cornel

    2014-01-01

    Active pharmaceutical ingredients (APIs), which are incorporated in different formulations, i.e. creams, gels, foams, etc., are applied to the skin for a therapeutic effect. This therapeutic effect could either be required in the top layer of the skin (topical drug delivery) or deeper layers to reach the blood capillaries (transdermal drug delivery). Transdermal delivery avoids oral administration route limitations, such as first pass metabolism which is the rapid clearance of the drug in the...

  10. Simultaneous determination of rhamnose, xylitol, arabitol, fructose, glucose, inositol, sucrose, maltose in jujube (Zizyphus jujube Mill.) extract: comparison of HPLC–ELSD, LC–ESI–MS/MS and GC–MS

    National Research Council Canada - National Science Library

    Sun, Shihao; Wang, Hui; Xie, Jianping; Su, Yue

    2016-01-01

    Jujube extract is commonly used as a food additive and flavoring. The sensory properties of the extract, especially sweetness, are a critical factor determining the product quality and therefore affecting consumer acceptability...

  11. Transdermal delivery of plasmid encoding truncated nucleocapsid protein enhanced PRRSV-specific immune responses.

    Science.gov (United States)

    Suradhat, Sanipa; Wongyanin, Piya; Sirisereewan, Chaitawat; Nedumpun, Teerawut; Lumyai, Mongkol; Triyarach, Sittikorn; Chaturavittawong, Damnoen; Paphavasit, Termsit; Panyatong, Raphee; Thanawongnuwech, Roongroje

    2016-01-27

    Porcine Reproductive and Respiratory Syndrome virus (PRRSV) induces several immunomodulatory mechanisms that resulted in delayed and ineffective anti-viral immune responses. Recently, it has been shown that intradermal immunization of plasmid encoding truncated nucleocapsid protein (pORF7t) could reduce PRRSV-induced immunomodulatory activities and enhances anti-PRRSV immunity in vaccinated pigs. However, intradermal immunization may not be practical for farm setting. Currently, there are several transdermal delivery systems available in the market, although they were not originally designed for plasmid delivery. To investigate the potential use of a transdermal delivery system for delivering of pORF7t and its immunological outcomes. The immunomodulatory effects induced by transdermal delivery of pORF7t were compared with intradermal immunization in an experimental pig model. In addition, immunomodulatory effects of the DNA vaccine were determined in the fattening pigs kept in a PRRSV-positive farm environment, and in the experimental pigs receiving heterologous prime-boost, pORF7t-modified live vaccine (MLV) immunization. The patterns of PRRSV-specific cellular responses induced by transdermal and intradermal immunizations of pORF7t were similar. Interestingly, the pigs transdermally immunized with pORF7t exhibited higher number of PRRSV-specific CD8(+)IFN-γ(+) cells. Pigs immunized with pORF7t and kept at PRRSV-positive environment exhibited enhanced PRRSV-specific IFN-γ(+) production, reduced numbers of regulatory T lymphocytes (Tregs) and lower lung scores at the end of the finishing period. In the heterologous prime-boost experiment, priming with pORF7t prior to MLV vaccination resulted in significantly higher numbers of CD3(+)IFN-γ(+) subpopulations, lower numbers of PRRSV-specific CD3(+)IL-10(+) cells and Tregs, and rapid antibody responses in immunized pigs. Transdermal immunization with pORF7t reduced PRRRSV-induced immunomodulatory effects and enhanced

  12. Lipid Nanocapsule-Based Gels for Enhancement of Transdermal Delivery of Ketorolac Tromethamine

    Directory of Open Access Journals (Sweden)

    Jaleh Varshosaz

    2011-01-01

    Full Text Available Previous reports show ineffective transdermal delivery of ketorolac by nanostructured lipid carriers (NLCs. The aim of the present work was enhancement of transdermal delivery of ketorolac by another colloidal carriers, lipid nanocapsules (LNCs. LNCs were prepared by emulsification with phase transition method and mixed in a Carbomer 934P gel base with oleic acid or propylene glycol as penetration enhancers. Permeation studies were performed by Franz diffusion cell using excised rat abdominal skin. Aerosil-induced rat paw edema model was used to investigate the in vivo performance. LNCs containing polyethylene glycol hydroxyl stearate, lecithin in Labrafac as the oily phase, and dilution of the primary emulsion with 3.5-fold volume of cold water produced the optimized nanoparticles. The 1% Carbomer gel base containing 10% oleic acid loaded with nanoparticles enhanced and prolonged the anti-inflammatory effects of this drug to more than 12 h in Aerosil-induced rat paw edema model.

  13. Feasibility of xanthan gum-sodium alginate as a transdermal drug delivery system for domperidone.

    Science.gov (United States)

    Rajesh, N; Siddaramaiah

    2009-10-01

    The present investigation comprises the formulation and in vitro evaluation of domperidone loaded transdermal drug delivery system (TDDS) for controlled release. The polymer membranes were prepared using xanthan gum (XG) and sodium alginate (SA) by varying the blends compositions viz., 10:0, 8:2, 6:4, 5:5, 4:6, 2:8, and 0:10 (XG/SA, wt/wt, %). The drug loaded membranes were evaluated for thickness, content uniformity, tensile behaviours, and in vitro drug release studies. Domperidone was found to be compatible with the prepared formulation as revealed by Fourier transform infrared (FTIR) spectroscopy studies. In vitro release studies were carried out in open glass diffusion cell for a period of 8 h and it showed controlled release of drug from the XG/SA matrix. The present study concludes that, the prepared transdermal films can be used to achieve controlled release of drug and improved bioavailability.

  14. Design and evaluation of a bioadhesive film for transdermal delivery of propranolol hydrochloride.

    Science.gov (United States)

    Rasool, Bazigha K Abdul; Aziz, Uday S; Sarheed, Omar; Rasool, Alaa A Abdul

    2011-09-01

    The objective of the study was to develop a suitable trans-dermal delivery system for propranolol hydrochloride (PPL) via employing chitosan as a film former. Drug concentration uniformity, thickness, moisture uptake capacity and skin bioadhesion of the films were characterized. The effects of chitosan and PPL concentration and different penetration enhancers on the release and permeation profiles from the films were investigated. Skin irritation of the candidate film was evaluated. Chitosan film (PPL 2 mg cm(-2), chitosan 2%, m/m, cineol 10%, m/m) was found nonirritant and achieved 88.2% release after 8 hours in phosphate buffer. Significant high (p < 0.001) permeation of PPL through rat skin was obtained using this film compared to the film without enhancer (about 8 times enhancement factor), making it a promising trans-dermal delivery system for PPL.

  15. Fabrication of microneedles using two photon polymerization for transdermal delivery of nanomaterials.

    Science.gov (United States)

    Doraiswamy, Anand; Ovsianikov, Aleksandr; Gittard, Shaun D; Monteiro-Riviere, Nancy A; Crombez, Rene; Montalvo, Eva; Shen, Weidian; Chichkov, Boris N; Narayan, Roger J

    2010-10-01

    Microneedle devices for transdermal delivery of nanoscale pharmacologic agents were fabricated out of organically-modified ceramic (Ormocer) materials using two photon polymerization. Out-of-plane hollow microneedle arrays with various aspect ratios were fabricated using this rapid prototyping process. Human epidermal keratinocyte (HEK) viability on Ormocer surfaces fabricated using two photon polymerization was similar to that on control surfaces. Nanoindentation studies were performed to determine hardness and Young's modulus values for Ormocer materials. Microneedies were shown to enable more rapid distribution of the PEG-amine quantum dot solution to the deep epidermis and dermis layers of porcine skin than topical administration. Our results suggest that two photon polymerization may be used to create microneedle arrays for transdermal delivery of nanoscale pharmacologic agents.

  16. Permeasi Transdermal Losartan In Vitro dari Larutan dengan Variasi Kadar Losartan dan Propilen Glikol

    Directory of Open Access Journals (Sweden)

    Annas Binarjo

    2017-03-01

    Full Text Available Abstrak Losartan, senyawa antagonis reseptor angiotensin II, mempunyai bioavailabilitas oral 0.25-0.35.  Bioavailabilitas yang rendah ini dapat diatasi dengan penghantaran obat secara transdermal. Enhancer sering ditambahkan ke dalam formula sediaan transdermal, misalnya propilen glikol (PG.  Penelitian ini bertujuan mempelajari pengaruh kadar propilen glikol terhadap permeasi transdermal losartan pada kadar obat yang berbeda. Penelitian dilakukan secara in vitro dengan sel difusi tipe vertikal dilakukan terhadap empat formula yaitu 2% potasium losartan (k-los :15% PG (F1, 10% k-los :15% PG (F2, 2% k-los :20% PG (F3, dan 10% k-los: 20% PG (F4 dengan dapar sitrat pH 5 sebagai mediumnya.  Kulit punggung tikus jantan galur wistar digunakan sebagai membran, PBS pH 7,4 sebagai medium kompartemen reseptor, dan HPLC untuk pengukuran kadar k-los dalam kompartemen reseptor dengan detektor UV. Hasil penelitian menunjukkan bahwa peningkatan kadar k-los dari 2% ke 10% pada kadar PG 15% meningkatkan fluks, sedangkan pada kadar 20% tidak berpengaruh terhadap fluks.  Peningkatan kadar PG dari 15% ke 20% justru menurunkan fluks pada kadar k-los 2%, dan tidak berpengaruh pada kadar k-los 10%.  Nilai lag time tidak berbeda diantara semua fomula. Hal ini berarti penggunaan enhancer PG lebih dari 15% justru merugikan permeasi transdermal. Kata Kunci : transdermal, losartan, propilen glikol, enhancer   Abstract Losartan is an angiotensin receptor antagonis which has low oral bioavailability (0.25-0.35.  Transdermal drug delivery system is needed as one solution for this low oral bioavailability drug.  Propilen glikol (PG, as enhancer, is frequently added in transdermal dosage form.  This research was purposed to explore the effect of PG as losartan permeation enhancer in various concentration of potasium losartan (k-los. The research was carried out in vitro using vertical tipe difusion cel for 4 formulas, i.e. 2% potasium losartan (k-los :15% PG (F1, 10% k

  17. Flexible and Stretchable Microneedle Patches with Integrated Rigid Stainless Steel Microneedles for Transdermal Biointerfacing.

    Science.gov (United States)

    Rajabi, Mina; Roxhed, Niclas; Shafagh, Reza Zandi; Haraldson, Tommy; Fischer, Andreas Christin; Wijngaart, Wouter van der; Stemme, Göran; Niklaus, Frank

    2016-01-01

    This paper demonstrates flexible and stretchable microneedle patches that combine soft and flexible base substrates with hard and sharp stainless steel microneedles. An elastomeric polymer base enables conformal contact between the microneedle patch and the complex topography and texture of the underlying skin, while robust and sharp stainless steel microneedles reliably pierce the outer layers of the skin. The flexible microneedle patches have been realized by magnetically assembling short stainless steel microneedles into a flexible polymer supporting base. In our experimental investigation, the microneedle patches were applied to human skin and an excellent adaptation of the patch to the wrinkles and deformations of the skin was verified, while at the same time the microneedles reliably penetrate the surface of the skin. The unobtrusive flexible and stretchable microneedle patches have great potential for transdermal biointerfacing in a variety of emerging applications such as transdermal drug delivery, bioelectric treatments and wearable bio-electronics for health and fitness monitoring.

  18. A comparative study on the transdermal penetration effect of gaseous and aqueous plasma reactive species

    Science.gov (United States)

    Liu, Xin; Gan, Lu; Ma, Mingyu; Zhang, Song; Liu, Jingjing; Chen, Hongxiang; Liu, Dawei; Lu, Xinpei

    2018-02-01

    To improve the depth of plasma active species in the skin, it is very important to develop skin disease treatment using plasma. In this article, an air plasma source was used to work directly with the skin of a mouse. A tortuous pathway, hair follicles, electroporation and a microneedle do not aid the transdermal delivery of gaseous plasma active species, therefore these gaseous plasma active species cannot penetrate mouse skin with a thickness of ~0.75 mm. The plasma activated water (PAW) produced by the air plasma source was used to study the transdermal penetration of the aqueous plasma activated species. This aqueous plasma activated species can penetrate the skin through hair follicles, intercellular and transcellular routes. The pH of the PAW did not affect the penetration efficiency of the aqueous plasma active species.

  19. Transdermal flux predictions for selected selective oestrogen receptor modulators (SERMs):Comparison with experimental results

    OpenAIRE

    Güngör, Sevgi; Delgado-Charro, M. Begoña; Masini-Etévé, Valérie; Potts, Russell O.; Guy, Richard H.

    2013-01-01

    The aim of this work was to evaluate the feasibility of delivering transdermally a series of highly lipophilic compounds (log P ~ 4-7), comprising several selective oestrogen receptor modulators and a modified testosterone (danazol). The maximum fluxes of the drugs were predicted theoretically using the modified Potts & Guy algorithm (to determine the permeability coefficient (kp) from water) and the calculated aqueous solubilities. The correction provided by Cleek & Bunge took into a...

  20. Development of domperidone bilayered matrix type transdermal patches: physicochemical, in vitro and ex vivo characterization

    Directory of Open Access Journals (Sweden)

    S.K Madishetti

    2010-09-01

    Full Text Available "nBackground and the purpose of the study: Domperidone (DOM is a dopamine- receptor (D2 antagonist, which is widely used in the treatment of motion-sickness. The pharmacokinetic parameters make DOM a suitable candidate for transdermal delivery. The purpose of the present investigation was to develop transdermal delivery systems for DOM and to evaluate their physicochemical characteristics, in vitro release an ex vivo permeation through rat abdominal skin and their mechanical properties. "nMethods: Bilayered matrix type transdermal drug delivery systems (TDDS of DOM were prepared by film casting technique using hydroxypropyl methyl cellulose as primary and Eudragit RL 100 as secondary layers. Brij-35 was incorporated as a solubilizer, d-limonene and propylene glycol were employed as permeation enhancer and plasticizer respectively. The prepared TDDS were extensively evaluated for in vitro release, moisture absorption, moisture content, water vapor transmission, ex vivo permeation through rat abdominal skin, mechanical properties and stability studies. The physicochemical interaction between DOM and polymers were investigated by Differential Scanning Calorimetry (DSC and Fourier Transform Infrared Spectroscopy (FTIR. "nResults: All the formulations exhibited satisfactory physicochemical and mechanical characteristics. The optimized formulation F6 showed maximum cumulative percentage of drug release (90.7%, permeation (6806.64 μg in 24 hrs, flux (86.02 μg /hr/cm2 and permeation coefficient of 0.86x10-2 cm/hr. Values of tensile strength (4.34 kg/mm2 and elastic modulus (5.89 kg/cm2 revealed that formulation F6 was strong but not brittle. DSC and FTIR studies showed no evidence of interaction between the drug and polymers. A shelf life of 2 years is predicted for the TDDS. Conclusions: Domperidone bilayered matrix type transdermal therapeutic systems could be prepared with the required flux and suitable mechanical properties.

  1. Physical, chemical and biological studies of gelatin/chitosan based transdermal fims with embedded silver nanoparticles

    Directory of Open Access Journals (Sweden)

    Sneha Paul

    2015-12-01

    Full Text Available Objective: To study the physical, chemical and biological properties of composite chitosangelatin transdermal film along with silver nanoparticles as binding agent and determine the compatibility of the prepared amalgamation towards wound management. Methods: Transdermal film preparations were done by solvent casting method containing different concentrations of biological synthesized silver nanoparticles. The films were characterized by using scanning electron microscope for their morphology and the determination of silver metal was done by using inductively coupled plasma atomic emission spectroscopy. Then a quantity of silver nanoparticles was further proceeded by physiochemical parameters (weight, thickness, temperature, solubility, absorption, tensile strength, in vitro drug release and skin permeation and biological parameters studies (anti-microbial, cytotoxicity and reactive oxygen species. Results: The film prepared by utilizing 2 g of gelatin and 0.5 g of chitosan exhibited better results. The physiochemical parameters studies revealed higher concentration of silver nanoparticles would give better results. In vitro drug release studies through dialysis and skin permeation showed the release of drug versus time (h. These films had shown excellent inhibition against Streptococcus and Escherichia coli species. Cytotoxicity study by MTT indicated the mild toxicity existed as the concentration of silver nanoparticles increased. Reactive oxygen species generation studies of transdermal film by using 2'7'-dichlorofluorescein diacetate assay demonstrated that the fluorescent cells were found in the higher concentration, which indicated cell damage (reactive oxygen species generated. Conclusions: Based on these observations, in vitro performances against various characteristics of transdermal film, would be utilized as a distinct dressing material and patches accessible in market.

  2. Fabrication and characterization of film-forming voriconazole transdermal spray for the treatment of fungal infection

    Directory of Open Access Journals (Sweden)

    Nitin Merubhai Mori

    2017-06-01

    Full Text Available Voriconazole is second-generation triazole used for the treatment of fungal infections but has serious unwanted adverse effects, which could be reduced by topical semisolid dosage form. Major drawbacks of topical semisolid products are poor patient compliance, cross contamination; gels are easily rubbed off by clothing and during day-to-day activities, physical instability. The purpose of the present work was to fabricate 0.5% w/w voriconazole transdermal spray for fungal infection. The transdermal spray was generated by using a film forming polymers like Eudragit RLPO and ethyl cellulose (1:2 ratios along with eutectic camphor: menthol (1:1 mixture used as a penetration enhancer. The formulation optimized by constrained 32 factorial design. Regression analysis and response surface methodology were used to optimize the effect of polymers and formulate checkpoint batch based on overlay plots. The transdermal spray was subjected to evaluate parameters related to formulation and containers. The concentration of Eudragit RLPO and ethyl cellulose was showed influence on viscosity as well as t50. Diffusion study was showed 75% of voriconazole transport with 65.8 μgcm−2 h−1 fluxes. Penetration enhancers’ had shown an increase in 1.68 fold of the penetration of voriconazole through the formulation. The study was concluded that fabricated film forming voriconazole transdermal spray formulations penetrate to the deep layer of the skin and was feasible to treat the dermatological fungal infection. This delivery platform is opened a wide range of treatment of fungal infection as compared to conventional formulations.

  3. Transdermal Nicotine During Cue Reactivity in Adult Smokers With and Without Anxiety Disorders

    OpenAIRE

    Morissette, Sandra B.; Gulliver, Suzy Bird; Kamholz, Barbara W.; Spiegel, David A.; Tiffany, Stephen T.; Barlow, David H.

    2012-01-01

    Transdermal nicotine almost doubles tobacco cessation rates; however little is known about what happens to smokers during the quit process when they are wearing the nicotine patch and confronted with high-risk smoking triggers. This is particularly important for smokers with psychological disorders who disproportionately represent today’s smokers and have more trouble quitting. Using a mixed between- and within-subjects design, smokers with anxiety disorders (n = 61) and smokers without any c...

  4. Effect of transdermal hormone therapy on platelet haemostasis in menopausal women

    OpenAIRE

    Grzegorz Stachowiak; Tomasz Pertyński; Magdalena Pertyńska-Marczewska

    2015-01-01

    [b]Introduction[/b]. Despite the undeniably positive effect on the quality of life of menopausal women, menopausal hormone therapy (HT) also has negative side-effects, which include, among others, thromboembolic complications. [b]objective[/b]. To assess the effect of a popular type of this therapy – transdermal HT on platelet hemostasis, which plays a significant role in intravascular coagulation. [b]Materials and method[/b]. The study group consisted of 92 postmenopausal women: ...

  5. Transdermal delivery of scopolamine by natural submicron injectors: in-vivo study in pig.

    Directory of Open Access Journals (Sweden)

    Esther Shaoul

    Full Text Available Transdermal drug delivery has made a notable contribution to medical practice, but has yet to fully achieve its potential as an alternative to oral delivery and hypodermic injections. While transdermal delivery systems would appear to provide an attractive solution for local and systemic drug delivery, only a limited number of drugs can be delivered through the outer layer of the skin. The most difficult to deliver in this way are hydrophilic drugs. The aquatic phylum Cnidaria, which includes sea anemones, corals, jellyfish and hydra, is one of the most ancient multicellular phyla that possess stinging cells containing organelles (cnidocysts, comprising a sophisticated injection system. The apparatus is folded within collagenous microcapsules and upon activation injects a thin tubule that immediately penetrates the prey and delivers its contents. Here we show that this natural microscopic injection system can be adapted for systemic transdermal drug delivery once it is isolated from the cells and uploaded with the drug. Using a topically applied gel containing isolated natural sea anemone injectors and the muscarinic receptor antagonist scopolamine, we found that the formulated injectors could penetrate porcine skin and immediately deliver this hydrophilic drug. An in-vivo study in pigs demonstrated, for the first time, rapid systemic delivery of scopolamine, with T(max of 30 minutes and C(max 5 times higher than in controls treated topically with a scopolamine-containing gel without cnidocysts. The ability of the formulated natural injection system to penetrate a barrier as thick as the skin and systemically deliver an exogenous compound presents an intriguing and attractive alternative for hydrophilic transdermal drug delivery.

  6. A Transdermal Drug Delivery System Based on LIGA Technology and Soft Lithography

    Science.gov (United States)

    Matteucci, Marco; Perennes, Frederic; Marmiroli, Benedetta; Di Fabrizio, Enzo

    2007-01-01

    This report presents a transdermal drug delivery system based on LIGA fabricated microparts. It is a portable device combining a magnetically actuated micro gear pump with a microneedle array. The fluidic behaviour of the system is analyzed in order to predict its performance according to the dimension of the microparts and then compared to experimental data. The manufacturing process of both micropump and microneedle array are described.

  7. [Demand for emergency department care for vertebral fractures treated with transdermal buprenorphine vs. other analgesics].

    Science.gov (United States)

    Guillén Astete, Carlos A; Boteanu, Alina; Luque Alarcón, Mónica; Carballo Cardona, César; Roldán Moll, Fernando; Fernández Pérez, Cristina

    2016-01-01

    To compare the results of emergency department management of spinal pain from vertebral fractures (in terms of revisits, adverse effects at 90 days, or need for hospitalization because of poor pain control at 6 months) in patients treated with transdermal buprenorphine or another analgesic. Retrospective observational study of cohorts in an emergency department database compiled prospectively over a period of 18 months. We included all patients over the age of 60 with a radiologic diagnosis of vertebral fracture or compression causing pain for more than 3 months. Records were stratified according to the World Health Organization (WHO) analgesic scale, which was used when the patients were treated. Variables related to effectiveness were revisits at 1 month, time between visits in days, and the need for hospitalization. A total of 180 patients were included; 39 were treated with drugs on the first step of the WHO's analgesic ladder, 74 with second-step drugs (mainly tramadol), and 67 with transdermal buprenorphine, a third-step drug. Half the patients treated with buprenorphine had revisited at 50 days or later (interquartile range [IQR, 41-60 days); half those treated with first-step analgesics had revisited by 19 days IQR, 10-37 days), and half those on second-step drugs had revisited by 28 days (IQR, 21-53 days) (P<.001). After adjustment for other variables, patients treated with first-step drugs revisited 4.19-fold more (95% CI, 2.57-6.80; P<.001) and those treated with second-step drugs revisited 1.91-fold more (95% CI, 1.22-2.99; P=.005) more than patients treated with transdermal buprenorphine. Transdermal buprenorphine used to manage spinal pain seems to significantly reduce the need for revisits in comparison with treatments with first- or second-step analgesics.

  8. Arbutin encapsulated micelles improved transdermal delivery and suppression of cellular melanin production

    OpenAIRE

    Liang, Ke; Xu, Keming; Bessarab, Dmitri; Obaje, Jonathan; Xu, Chenjie

    2016-01-01

    Background Hyperpigmentation is a skin disorder characterized by elevated production of melanin. Current treatment approaches mainly rely on the application of skin lightening chemicals, most of which have safety issues. Efficacy of delivery of the active ingredients to the target organ has also been a challenge. Transdermal based drug delivery platform has been shown to improve drug bioavailability, avoiding the hepatic first pass metabolism, decrease gastrointestinal side effects, and event...

  9. Fatal overdose after ingestion of a transdermal fentanyl patch in two non-human primates

    OpenAIRE

    Deschamps, Jack-Yves; Gaulier, Jean-Michel; Podevin, Guillaume; Cherel, Yan; Ferry, Nicolas; Roux, Françoise

    2012-01-01

     ; Case history and presentation: Two non-human primates (Macaca fascicularis) enrolled in an experimental protocol received a 25 μg hour−1 transdermal fentanyl patch for postoperative analgesia. The following day both animals were clinically normal, but after a new induction of anaesthesia with ketamine, they developed severe and prolonged respiratory distress, profound coma and myosis. Management and follow-up: Attempted reversal with naloxone was ineffective. After several hours of ventila...

  10. Fatal overdose after ingestion of a transdermal fentanyl patch in two non-human primates

    OpenAIRE

    Deschamps, Jack-Yves; Podevin, Guillaume; Cherel, Yan; Ferry, Nicolas

    2012-01-01

    Case history and presentation: Two non-human primates (Macaca fascicularis) enrolled in an experimental protocol received a 25 μg hour−1 transdermal fentanyl patch for postoperative analgesia. The following day both animals were clinically normal, but after a new induction of anaesthesia with ketamine, they developed severe and prolonged respiratory distress, profound coma and myosis. Management and follow-up: Attempted reversal with naloxone was ineffective. After several hours of ventilatio...

  11. Fatal Overdose due to Confusion of an Transdermal Fentanyl Delivery System

    OpenAIRE

    Ingo Voigt

    2013-01-01

    Background. The use of transdermal fentanyl systems has increased over recent years, especially in patients with chronic pain. Large misuse potential and fatal outcomes have been described. Case Presentation. A 58-year-old patient presenting with clinical signs of opioid poisoning (hypoventilation, bradycardia, hypotension, and miosis) was admitted to our ICU. The first body check revealed a 75 mcg per hour fentanyl patch at the patient's right scapula. Some months ago, patient's aunt died af...

  12. The Influence of Solid Microneedles on the Transdermal Delivery of Selected Antiepileptic Drugs

    Directory of Open Access Journals (Sweden)

    Julia Nguyen

    2016-11-01

    Full Text Available The aim of this project was to examine the effect of microneedle rollers on the percutaneous penetration of tiagabine hydrochloride and carbamazepine across porcine skin in vitro. Liquid chromatography-mass spectrometric analysis was carried out using an Agilent 1200 Series HPLC system coupled to an Agilent G1969A TOF-MS system. Transdermal flux values of the drugs were determined from the steady-state portion of the cumulative amount versus time curves. Following twelve hours of microneedle roller application, there was a 6.74-fold increase in the percutaneous penetration of tiagabine hydrochloride (86.42 ± 25.66 µg/cm2/h compared to passive delivery (12.83 ± 6.30 µg/cm2/h. For carbamazepine in 20% ethanol, passive transdermal flux of 7.85 ± 0.60 µg/cm2/h was observed compared to 10.85 ± 0.11 µg/cm2/h after microneedle treatment. Carbamazepine reconstituted in 30% ethanol resulted in only a 1.19-fold increase in drug permeation across porcine skin (36.73 ± 1.83 µg/cm2/h versus 30.74 ± 1.32 µg/cm2/h. Differences in flux values of untreated and microneedle-treated porcine skin using solid microneedles for the transdermal delivery of tiagabine were statistically significant. Although there were 1.38- and 1.19-fold increases in transdermal flux values of carbamazepine when applied as 20% and 30% ethanol solutions across microneedle-treated porcine skin, respectively, the increases were not statistically significant.

  13. The Influence of Solid Microneedles on the Transdermal Delivery of Selected Antiepileptic Drugs.

    Science.gov (United States)

    Nguyen, Julia; Ita, Kevin B; Morra, Matthew J; Popova, Inna E

    2016-11-15

    The aim of this project was to examine the effect of microneedle rollers on the percutaneous penetration of tiagabine hydrochloride and carbamazepine across porcine skin in vitro. Liquid chromatography-mass spectrometric analysis was carried out using an Agilent 1200 Series HPLC system coupled to an Agilent G1969A TOF-MS system. Transdermal flux values of the drugs were determined from the steady-state portion of the cumulative amount versus time curves. Following twelve hours of microneedle roller application, there was a 6.74-fold increase in the percutaneous penetration of tiagabine hydrochloride (86.42 ± 25.66 µg/cm²/h) compared to passive delivery (12.83 ± 6.30 µg/cm²/h). For carbamazepine in 20% ethanol, passive transdermal flux of 7.85 ± 0.60 µg/cm²/h was observed compared to 10.85 ± 0.11 µg/cm²/h after microneedle treatment. Carbamazepine reconstituted in 30% ethanol resulted in only a 1.19-fold increase in drug permeation across porcine skin (36.73 ± 1.83 µg/cm²/h versus 30.74 ± 1.32 µg/cm²/h). Differences in flux values of untreated and microneedle-treated porcine skin using solid microneedles for the transdermal delivery of tiagabine were statistically significant. Although there were 1.38- and 1.19-fold increases in transdermal flux values of carbamazepine when applied as 20% and 30% ethanol solutions across microneedle-treated porcine skin, respectively, the increases were not statistically significant.

  14. Feasibility Study of Carbon Nanotube Microneedles for Rapid Transdermal Drug Delivery

    OpenAIRE

    Lyon, Bradley J.; Aria, Adrianus I.; Gharib, Morteza

    2013-01-01

    We introduce a new approach for fabricating hollow microneedles using vertically-aligned carbon nanotubes (VA-CNTs) for rapid transdermal drug delivery. Here, we discuss the fabrication of the microneedles emphasizing the overall simplicity and flexibility of the method to allow for potential industrial application. By capitalizing on the nanoporosity of the CNT bundles, uncured polymer can be wicked into the needles ultimately creating a high strength composite of aligned nanotubes and polym...

  15. Transdermal therapy for attention-deficit hyperactivity disorder with the methylphenidate patch (MTS).

    Science.gov (United States)

    Findling, Robert L; Dinh, Steven

    2014-03-01

    Transdermal technology is currently approved in the US for the administration of more than 20 medications. This current review describes the clinical research pertaining to the use of a methylphenidate patch in the treatment of attention-deficit hyperactivity disorder (ADHD) in children and adolescents. PubMed searches were conducted using the search term 'methylphenidate transdermal system', and were limited to clinical trials. No limits were set for dates of publication. A total of 21 citations were identified. Studies evaluating the safety and efficacy of the methylphenidate transdermal system (MTS) in children and adolescents were included in this review. Additional studies were identified from bibliographies and the 'Related Citations' section of PubMed searches. The MTS delivers a range of methylphenidate doses using a drug-in-adhesive matrix patch. According to current labeling, the patch should be applied to the hip once daily for a maximum of 9 h. Serum methylphenidate levels increase over wear time, with mean time to maximum concentration (t max) reached between 8 and 10 h for a 9-h wear time, and the elimination half-life for methylphenidate is 3-4 h after patch removal. In clinical trials, ADHD symptoms were measured using the ADHD Rating Scale, Version IV, and several parent-, teacher-, and patient-rated scales. Treatment effects show statistically significant differences from baseline symptom scores starting at the first evaluation, 2 h after the patch is applied, with significant benefit lasting up to 12 h with a 9-h wear time. Adverse events with the MTS are similar to those seen with other formulations of methylphenidate, with the exception of skin-related reactions at the site of application, which were generally mild to moderate in severity. The incidence of contact allergic dermatitis with MTS is MTS compared with placebo, and after switching from oral extended-release (ER) methylphenidate. Transdermal drug delivery is an effective and safe

  16. Experimental design and optimization of raloxifene hydrochloride loaded nanotransfersomes for transdermal application.

    Science.gov (United States)

    Mahmood, Syed; Taher, Muhammad; Mandal, Uttam Kumar

    2014-01-01

    Raloxifene hydrochloride, a highly effective drug for the treatment of invasive breast cancer and osteoporosis in post-menopausal women, shows poor oral bioavailability of 2%. The aim of this study was to develop, statistically optimize, and characterize raloxifene hydrochloride-loaded transfersomes for transdermal delivery, in order to overcome the poor bioavailability issue with the drug. A response surface methodology experimental design was applied for the optimization of transfersomes, using Box-Behnken experimental design. Phospholipon(®) 90G, sodium deoxycholate, and sonication time, each at three levels, were selected as independent variables, while entrapment efficiency, vesicle size, and transdermal flux were identified as dependent variables. The formulation was characterized by surface morphology and shape, particle size, and zeta potential. Ex vivo transdermal flux was determined using a Hanson diffusion cell assembly, with rat skin as a barrier medium. Transfersomes from the optimized formulation were found to have spherical, unilamellar structures, with a homogeneous distribution and low polydispersity index (0.08). They had a particle size of 134±9 nM, with an entrapment efficiency of 91.00%±4.90%, and transdermal flux of 6.5±1.1 μg/cm(2)/hour. Raloxifene hydrochloride-loaded transfersomes proved significantly superior in terms of amount of drug permeated and deposited in the skin, with enhancement ratios of 6.25±1.50 and 9.25±2.40, respectively, when compared with drug-loaded conventional liposomes, and an ethanolic phosphate buffer saline. Differential scanning calorimetry study revealed a greater change in skin structure, compared with a control sample, during the ex vivo drug diffusion study. Further, confocal laser scanning microscopy proved an enhanced permeation of coumarin-6-loaded transfersomes, to a depth of approximately160 μM, as compared with rigid liposomes. These ex vivo findings proved that a raloxifene hydrochloride

  17. Natural oils as skin permeation enhancers for transdermal delivery of olanzapine: in vitro and in vivo evaluation.

    Science.gov (United States)

    Aggarwal, Geeta; Dhawan, Sanju; HariKumar, S L

    2012-03-01

    The feasibility of development of transdermal delivery system of olanzapine utilizing natural oils as permeation enhancers was investigated. Penetration enhancing potential of corn (maize) oil, gr