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Sample records for morphology hplc profiles

  1. Recognition of hypoxyloid and xylarioid Entonaema species and allied Xylaria species from a comparison of holomorphic morphology, HPLC profiles, andribosomal DNA sequences

    DEFF Research Database (Denmark)

    Stadler, M.; Fournier, J.; Læssøe, Thomas

    2008-01-01

    pallidum is thus regarded as a later synonym of E. mesentericum. Therefore, the latter name is transferred to Xylaria. A key to entonaemoid Xylariaceae is provided. Colour reactions (NH3, KOH) of the ectostroma were applied to a limited number of Xylaria spp., but metabolite profiles of cultures appear......The genus Entonaema comprises Xylariaceae with hollow, gelatinous stromata that accumulate liquid. Some of its species, including the type species, appear related to Daldinia from a polyphasic approach, comprising morphological studies, comparisons of ribosomal DNA sequences, and high performance...

  2. HPLC based activity profiling for 5-lipoxygenase inhibitory activity in Isatis tinctoria leaf extracts.

    Science.gov (United States)

    Oberthür, C; Jäggi, R; Hamburger, M

    2005-06-01

    In the pursuit of the anti-inflammatory constituents in lipophilic woad extracts, the 5-lipoxygenase (5-LOX) inhibitory activity was investigated by HPLC-based activity profiling. In a low-resolution profiling, two time windows with peaks of activity were found. The first coincided with tryptanthrin, a known dual inhibitor of cyclooxygenase-2 (COX-2) and 5-LOX, whereas the major inhibitory fraction was towards the end of the HPLC run. The active fractions were profiled in a peak-resolved manner, and the compounds analyzed by LC-MS, GC and TLC. The activity in the lipophilic fractions of the Isatis extract could be linked to an unsaturated fatty acid, alpha-linolenic acid.

  3. Metabolite profiling of leek (Allium porrum L) cultivars by (1) H NMR and HPLC-MS.

    Science.gov (United States)

    Soininen, Tuula H; Jukarainen, Niko; Soininen, Pasi; Auriola, Seppo O K; Julkunen-Tiitto, Riitta; Oleszek, Wieslaw; Stochmal, Anna; Karjalainen, Reijo O; Vepsäläinen, Jouko J

    2014-01-01

    Leek (Allium ampeloprasum var. porrum) is consumed as a vegetable throughout the world. However, little is known about the metabolites of leek cultivars, especially those with potentially important beneficial properties for human health. We provide new information for the overall metabolite composition of several leek cultivars grown in Europe by using HPLC-MS and (1) H NMR. The use of a novel CTLS/NMR (constrained total-line-shape nuclear magnetic resonance) approach was found to be capable of reliable quantification, even with overlapping metabolite signals in the (1) H NMR of plant metabolites. Additionally, a new application for leek flavonoids was optimised for HPLC-MS. The total concentration of carbohydrates (glucose, fructose, kestose/nystose and sucrose) and nine amino acids varied by fourfold in leek juice from different cultivars, while the total concentrations of four organic acids were similar in all cultivars. All the quantified flavonols were kaempferol derivatives or quercetin derivatives and threefold differences in flavonol concentrations were detected between cultivars. In this study, various phytochemical profiles were determined for several leek cultivars by (1) H NMR spectroscopy with CTLS combined with HPLC-MS. The wide variation in bioactive compounds among commercial leek cultivars offers promising opportunities for breeders to raise the levels of important biochemical compounds in leek breeding lines, and also provides some objective measure for quality assurance for the leek industry. Copyright © 2014 John Wiley & Sons, Ltd.

  4. Cervical column morphology and craniofacial profiles in monozygotic twins.

    Science.gov (United States)

    Sonnesen, Liselotte; Pallisgaard, Carsten; Kjaer, Inger

    2008-02-01

    Previous studies have described the relationships between cervical column morphology and craniofacial morphology. The aims of the present study were to describe cervical column morphology in 38 pairs of adult monozygotic (MZ) twins, and compare craniofacial morphology in twins with fusions with craniofacial morphology in twins without fusion. Visual assessment of cervical column morphology and cephalometric measurements of craniofacial morphology were performed on profile radiographs. In the cervical column, fusion between corpora of the second and third vertebrae was registered as fusion. In the twin group, 8 twin pairs had fusion of the cervical column in both individuals within the pair (sub-group A), 25 pairs had no fusions (subgroup B), and in 5 pairs, cervical column morphology was different within the pair (subgroup C), as one twin had fusion and the other did not. Comparison of craniofacial profiles showed a tendency to increased jaw retrognathia, larger cranial base angle, and larger mandibular inclination in subgroup A than in subgroup B. The same tendency was observed within subgroup C between the individual twins with fusion compared with those without fusion. These results confirm that cervical fusions and craniofacial morphology may be interrelated in twins when analysed on profile radiographs. The study also documents that differences in cervical column morphology can occur in individuals within a pair of MZ twins. It illustrates that differences in craniofacial morphology between individuals within a pair of MZ twins can be associated with cervical fusion.

  5. MORPHOLOGICAL EVALUATION AND PROTEIN PROFILING OF ...

    African Journals Online (AJOL)

    Owner

    characterizing Nigerian Corchorus species. Keywords: Vegetative characters, SDS-PAGE, Corchorus ... In regions like China, India, Nepal and Bangladesh. Corchorus species is of great economic importance and bulk of ... The morphological characterization of the. Corchorus samples was conducted in the experimental.

  6. CZE/PAD and HPLC-UV/PAD Profile of Flavonoids from Maytenus aquifolium and Maytenus ilicifolia “espinheira santa” Leaves Extracts

    OpenAIRE

    Diagone, Cristina A.; Colombo, Renata; Lanças, Fernando M.; Yariwake, Janete H.

    2012-01-01

    This paper describes the application of HPLC and CZE to analyze flavonoids in the leaves of Maytenus ilicifolia and Maytenus aquifolium, which are species widely used in Brazilian folk medicine. The two species showed different flavonoid profiles, but acidic hydrolysis of the Maytenus extracts confirmed that all these compounds are quercetin or kaempferol derivatives. A comparison of the CZE and HPLC profiles of Maytenus extracts showed numerous flavonoid peaks using HPLC. However, the advant...

  7. HPLC-ICP-MS compared with radiochemical detection for metabolite profiling of H-3-bromohexine in rat urine and faeces

    DEFF Research Database (Denmark)

    Jensen, B.P.; Gammelgaard, B.; Hansen, S.H.

    2005-01-01

    H-3-Bromohexine was dosed to rats as a model compound to allow comparison of HPLC-ICP-MS detection on bromine to radiochemical detection in an in vivo drug metabolism study. Metabolite profiles were obtained in urine and faeces extracts. No influence of the methanol gradient on the bromine response...... was observed in the range of 18 - 75% methanol. The sensitivity obtained by HPLC- ICP-MS was almost two orders of magnitude better than on-line H-3 radiochemical detection. For ICP- MS, the limit of detection was calculated to be 69 nM Br ( injection volume 100 mu l), corresponding to an absolute limit...

  8. Cytotoxic activity of abietane diterpenoids from roots of Salvia sahendica by HPLC-based activity profiling

    Directory of Open Access Journals (Sweden)

    Fahimeh Moradi-Afrapoli

    Full Text Available ABSTRACT Screening of medicinal plants from Iranian flora against human cancer cell-lines have shown that an hexane extract from roots of Salvia sahendica Boiss. & Buhse, Lamiaceae, is active against human cervical cancer (HeLa and colorectal adenocarcinoma (Caco-2 cell-lines at the test concentration of 100 µg/ml (100% inhibition. Cytotoxicity of the extract was localized with the aid of HPLC-time-based activity profiling adapted to the tetrazolium colorimetric bioassay. Four abietane-type diterpenoids in active time-windows were identified as cytotoxic compounds namely: sahandone (1, sahandol (2, 12-deoxy-salvipisone (3 and sahandinone (4. Compound 1 showed the highest toxicity against HeLa cells (IC50 = 5.6 ± 0.1 µg/ml, which was comparable with betulinic acid (IC50 = 4.3 ± 1.2 µg/ml, the positive control. Compound 2 was active against the HeLa cells (IC50 = 8.9 ± 0.7 µg/ml but not the Caco-2 cell-line. Compounds 1, 3 and 4 exhibited moderate activity (IC50 = 22.9–41.4 µg/ml against the Caco-2 cells. This study reveals that the HeLa cells are more sensitive to all tested compounds than the Caco-2 cells. In silico molecular docking study showed a rigid binding of the compounds to tyrosine kinase pp60src, and proved their cytotoxic activity.

  9. Simultaneous HPLC determination of flavonoids and phenolic acids profile in Pêra-Rio orange juice.

    Science.gov (United States)

    Mesquita, E; Monteiro, M

    2018-04-01

    The aim of this study was to develop and validate an HPLC-DAD method to evaluate the phenolic compounds profile of organic and conventional Pêra-Rio orange juice. The proposed method was validated for 10 flavonoids and 6 phenolic acids. A wide linear range (0.01-223.4μg·g -1 ), good accuracy (79.5-129.2%) and precision (CV≤3.8%), low limits of detection (1-22ng·g -1 ) and quantification (0.7-7.4μg), and overall ruggedness were attained. Good recovery was achieved for all phenolic compounds after extraction and cleanup. The method was applied to organic and conventional Pêra-Rio orange juices from beginning, middle and end of the 2016 harvest. Flavones rutin, nobiletin and tangeretin, and flavanones hesperidin, narirutin and eriocitrin were identified and quantified in all organic and conventional juices. Identity was confirmed by mass spectrometry. Nineteen non-identified phenolic compounds were quantified based on DAD spectra characteristic of the chemical class: 7 cinnamic acid derivatives, 6 flavanones and 6 flavones. The phenolic compounds profile of Pêra-Rio orange juices changed during the harvest; levels increased in organic orange juices, and decreased or were about the same in conventional orange juices. Phenolic compounds levels were higher in organic (0.5-1143.7mg·100g -1 ) than in conventional orange juices (0.5-689.7mg·100g -1 ). PCA differentiated organic from conventional FS and NFC juices, and conventional FCOJ from conventional FS and NFC juices, thus differentiating cultivation and processing. Copyright © 2017. Published by Elsevier Ltd.

  10. Reversed Phase HPLC-DAD Profiling of Carotenoids, Chlorophylls and Phenolic Compounds in Adiantum capillus-veneris Leaves

    OpenAIRE

    Zeb, Alam; Ullah, Fareed

    2017-01-01

    Adiantum capillus-veneris is important endangered fern species with several medicinal properties. In this study, the leaves samples were extracted and separated using reversed phase HPLC with DAD for carotenoids, chlorophylls and phenolic compounds. Separation of carotenoids and chlorophylls were carried out using a tertiary gradient system of water, MTBE and methanol-water, while a binary gradient system of methanol-water-acetic acid was used for phenolic profiling. Results revealed eight ca...

  11. HPLC profiling, antioxidant and in vivo anti-inflammatory activity of the ethanol extract of Syzygium jambos available in Bangladesh.

    Science.gov (United States)

    Hossain, Hemayet; Rahman, Shaikh Emdadur; Akbar, Proity Nayeeb; Khan, Tanzir Ahmed; Rahman, Md Mahfuzur; Jahan, Ismet Ara

    2016-03-28

    Syzygium jambos has been used as a traditional medicine for the treatment of inflammatory diseases in Bangladesh. The study investigates the high performance liquid chromatography (HPLC) profiling of phenolic compounds, and evaluates the antioxidant and anti-inflammatory activities of ethanol extract of S. jambos available in Bangladesh. The extract was subjected to HPLC for the identification and quantification of the major bioactive polyphenols present in S. jambos. Antioxidant activity was determined using 2, 2'-azino bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) radical scavenging, reducing power assay, total antioxidant capacity, total phenolic and flavonoid content. Furthermore, the anti-inflammatory effect of the extract in rats for two different test models: carrageenan and histamine-induced paw edema was inspected. High levels of catechin hydrate and rutin hydrate (99.00 and 79.20 mg/100 g extract, respectively) and moderate amounts of ellagic acid and quercetin (59.40 and 69.30 mg/100 g extract, respectively) were quantified in HPLC. Catechin hydrate from this plant extract was determined for the first time through HPLC. For ABTS scavenging assay, the median inhibition concentration (IC50) value of S. jambos was 57.80 µg/ml, which was significant to that of ascorbic acid (12.01 µg/ml). The maximum absorbance for reducing power assay was found to be 0.4934. The total antioxidant capacity, phenolic and flavonoid contents were calculated to be 628.50 mg/g of ascorbic acid, 230.82 mg/g of gallic acid and 11.84 mg/g of quercetin equivalent, respectively. At a dose of 400 mg/kg, a significant acute anti-inflammatory activity (P antioxidant activities of S. jambos.

  12. Phytochemical profile of morphologically selected yerba-mate progenies

    Directory of Open Access Journals (Sweden)

    Alice Teresa Valduga

    2016-02-01

    Full Text Available ABSTRACT Yerba-mate (Ilex paraguariensis St. Hil is a native South American species. Plant progenies are populations that differ in terms of their productivity, morphology and phytochemical profile. This study aimed to determine the concentration of primary and secondary metabolites, such as antioxidants, in leaves, of yerba-mate progenies selected based on morphological characteristics. We evaluated the centesimal composition of secondary metabolites in the leaves of five yerba-mate plants. Methylxanthines and phenolic compounds were determined by UPLC-PDA, and antioxidant activity by measuring DPPH scavenging. Significant differences were found in centesimal composition and the contents of caffeine, theobromine, rutin and chlorogenic acid, as well as antioxidant activities, in selected progenies. The IC50 values were correlated with the chlorogenic acid levels (r2 = 0.5242 and soluble content (r2 = 0.7686. The morphological characteristics observed in yerba-mate leaves can be used as a tool for plant selection, to obtain matrices with different phytochemical profiles as a genetic material source.

  13. HPLC-UV Polyphenolic Profiles in the Classification of Olive Oils and Other Vegetable Oils via Principal Component Analysis

    Directory of Open Access Journals (Sweden)

    Mireia Farrés-Cebrián

    2016-12-01

    Full Text Available High performance liquid chromatography-ultraviolet (HPLC-UV was applied to the analysis and characterization of olive oils and other vegetable oils. A chromatographic separation on a Zorbax Eclipse XDB-C8 reversed-phase column was proposed under gradient elution, employing 0.1% formic acid aqueous solution and methanol as mobile phase, for the determination of 14 polyphenols and phenolic acids, allowing us to obtain compositional profiles in less than 20 min. Acceptable sensitivity (limit of detection (LOD values down to 80 µg/L in the best of cases, linearity (r2 higher than 0.986, good run-to-run and day-to-day precisions (relative standard deviation (RSD values lower than 11.5%, and method trueness (relative errors lower than 6.8% were obtained. The proposed HPLC-UV method was then applied to the analysis of 72 oil samples (47 olive oils and 27 vegetable oils including sunflower, soy, corn, and mixtures of them. Analytes were recovered using a liquid–liquid extraction method employing ethanol:water 70:30 (v/v solution and hexane as extracting and defatting solvents, respectively. HPLC-UV polyphenolic profiles using peak areas were then analysed by principal component analysis (PCA to extract information from the most significant data contributing to the characterization and classification of olive oils against other vegetable oils, as well as among Arbequina and Picual olive oil varieties. PCA results showed a noticeable difference between olive oils and the other classes. In addition, a reasonable discrimination of olive oils as a function of fruit varieties was also encountered.

  14. Metabolic profiling using HPLC allows classification of drugs according to their mechanisms of action in HL-1 cardiomyocytes

    International Nuclear Information System (INIS)

    Strigun, Alexander; Wahrheit, Judith; Beckers, Simone; Heinzle, Elmar; Noor, Fozia

    2011-01-01

    Along with hepatotoxicity, cardiotoxic side effects remain one of the major reasons for drug withdrawals and boxed warnings. Prediction methods for cardiotoxicity are insufficient. High content screening comprising of not only electrophysiological characterization but also cellular molecular alterations are expected to improve the cardiotoxicity prediction potential. Metabolomic approaches recently have become an important focus of research in pharmacological testing and prediction. In this study, the culture medium supernatants from HL-1 cardiomyocytes after exposure to drugs from different classes (analgesics, antimetabolites, anthracyclines, antihistamines, channel blockers) were analyzed to determine specific metabolic footprints in response to the tested drugs. Since most drugs influence energy metabolism in cardiac cells, the metabolite 'sub-profile' consisting of glucose, lactate, pyruvate and amino acids was considered. These metabolites were quantified using HPLC in samples after exposure of cells to test compounds of the respective drug groups. The studied drug concentrations were selected from concentration response curves for each drug. The metabolite profiles were randomly split into training/validation and test set; and then analysed using multivariate statistics (principal component analysis and discriminant analysis). Discriminant analysis resulted in clustering of drugs according to their modes of action. After cross validation and cross model validation, the underlying training data were able to predict 50%-80% of conditions to the correct classification group. We show that HPLC based characterisation of known cell culture medium components is sufficient to predict a drug's potential classification according to its mode of action.

  15. HPLC fucoxanthin profiles of a microalga, a macroalga and a pure fucoxanthin standard

    Directory of Open Access Journals (Sweden)

    Su Chern Foo

    2017-02-01

    Full Text Available Data in this article illustrate representative fucoxanthin chromatograms of a microalga, Chaetoceros calcitrans; a macroalga, Saccharina japonica and; a pure fucoxanthin standard. High performance liquid chromatography (HPLC eluted fucoxanthin at the 7.008±0.024th min. This data article refers to the research article ‘‘Antioxidant capacities of fucoxanthin-producing algae as influenced by their carotenoid and phenolic contents’’ Foo et al. [1]; where a more comprehensive data interpretation and analysis is explained.

  16. Reversed Phase HPLC-DAD Profiling of Carotenoids, Chlorophylls and Phenolic Compounds in Adiantum capillus-veneris Leaves

    Directory of Open Access Journals (Sweden)

    Alam Zeb

    2017-04-01

    Full Text Available Adiantum capillus-veneris is important endangered fern species with several medicinal properties. In this study, the leaves samples were extracted and separated using reversed phase HPLC with DAD for carotenoids, chlorophylls and phenolic compounds. Separation of carotenoids and chlorophylls were carried out using a tertiary gradient system of water, MTBE and methanol-water, while a binary gradient system of methanol-water-acetic acid was used for phenolic profiling. Results revealed eight carotenoids, four pheophytins, and two chlorophylls. Lutein (806.0 μg/g, chlorophyll b′ (410.0 μg/g, chlorophyll a (162.4 μg/g, 9′-Z-neoxanthin (142.8 μg/g and all-E-violaxanthin (82.2 μg/g were present in higher amounts. The relatively high amounts of lutein may be one of the key indicator of beneficial antioxidant properties. The phenolic profile revealed a total of 13 compounds, namely 4-hydroxybenzoic acid, chlorogenic acid, caftaric acid, kaempferol glycosides, p-coumaric acid, rosmarinic acid, 5-caffeoylquinic acid, and quercetin glycosides. Kaempferol-3-sophorotrioside (58.7 mg/g, chlorogenic acid (28.5 mg/g, 5-O-caffeoylquinic acid (18.7 mg/g, coumaric acid (11.2 mg/g, and its derivative (33.1 mg/g were present in high amounts. These results suggest that the reversed phase HPLC profiling of Adiantum leaves provides a better understanding in to the actual composition of bioactive compounds, which may be responsible for the potential medicinal properties. Adiantum leaves rich in important bioactive phytochemicals can be used as a possible source of nutraceuticals or as a functional food ingredient.

  17. Reversed Phase HPLC-DAD Profiling of Carotenoids, Chlorophylls and Phenolic Compounds in Adiantum capillus-veneris Leaves

    Science.gov (United States)

    Zeb, Alam; Ullah, Fareed

    2017-04-01

    Adiantum capillus-veneris is important endangered fern species with several medicinal properties. In this study, the leaves samples were extracted and separated using reversed phase HPLC with DAD for carotenoids, chlorophylls and phenolic compounds. Separation of carotenoids and chlorophylls were carried out using a tertiary gradient system of water, MTBE and methanol-water, while a binary gradient system of methanol-water-acetic acid was used for phenolic profiling. Results revealed eight carotenoids, four pheophytins and two chlorophylls. Lutein (806.0 µg/g), chlorophyll b' (410.0 µg/g), chlorophyll a (162.4 µg/g), 9'-Z-neoxanthin (142.8 µg/g) and all-E-violaxanthin (82.2 µg/g)) were present in higher amounts. The relatively high amounts of lutein may be one of the key indicator of beneficial antioxidant properties. The phenolic profile revealed a total of thirteen compounds, namely p-hydroxybenzoic acid, chlorogenic acid, caftaric acid, kaempferol glycosides, p-coumaric acid, rosmarinic acid, 5-caffeoylquinic acid, and quercetin glycosides. Kaempferol-3-sophorotrioside (58.7 mg/g), chlorogenic acid (28.5 mg/g), 5-O-caffeoylquinic acid (18.7 mg/g), coumaric acid (11.2 mg/g) and its derivative (33.1 mg/g) were present in high amounts. These results suggest that the reversed phase HPLC profiling of adiantum leaves provides a better understanding in to the actual composition of bioactive compounds, which may be responsible for possible medicinal properties. Adiantum leaves rich in important bioactive phytochemicals can be used as a potential source of nutraceuticals or as a functional food ingredient.

  18. NMR, HS-SPME-GC/MS, and HPLC/MSn Analyses of Phytoconstituents and Aroma Profile of Rosmarinus eriocalyx.

    Science.gov (United States)

    Bendif, Hamdi; Miara, Mohamed Djamel; Peron, Gregorio; Sut, Stefania; Dall'Acqua, Stefano; Flamini, Guido; Maggi, Filippo

    2017-10-01

    In this work, a comprehensive study on the chemical constituents of the aerial parts of Rosmarinus eriocalyx (Lamiaceae), an aromatic shrub traditionally consumed as a food and herbal remedy in Algeria, is presented. The aroma profile was analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC/MS), whereas the crude extract constituents were analyzed by 1 H-NMR and by high performance liquid chromatography coupled with mass spectrometry (HPLC/MS n ). Thirty-nine volatile compounds, most of them being monoterpenes, have been identified, with camphor, camphene, and α-pinene as the most abundant constituents. 1 H-NMR analysis revealed the presence of phenolic compounds and betulinic acid while HPLC/MS n allowed the identification of glycosilated and aglyconic flavonoids as well as phenylpropanoid derivatives. Some of these constituents, namely as betulinic acid, rosmanol, and cirsimaritin were reported for the first time in R. eriocalyx. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

  19. Gc-ms, hplc profiling, antioxidant, antimicrobial and cytotoxicity studies of malcolmia africana leaves

    International Nuclear Information System (INIS)

    Bokhari, T.H.; Rasool, N.; Riaz, M.; Riaz, M.

    2014-01-01

    Plants are known to be the richest source of natural antioxidant and antimicrobial properties. The use of herbs and medicinal plants as the first medicines is a universal phenomenon. The present study was carried out to examine the antioxidant, antimicrobial and cytotoxicity potential Malcolmia africana leaves extract, fraction, essential oil and fixed oil. The whole plant was extracted with absolute methanol and further fractionated with increasing polarity based absolute solvents. Different fractions were taken by solvent extraction method and their antimicrobial activities were determined. The IC50 and % inhibition by linoleic acid oxidation was evaluated for the antioxidant studies. The cytotoxicity of the plant extract and fractions were assayed against human blood erythrocytes (RBCs). The DPPH scavenging and linoleic acid oxidation assays were carried out. Qualitative and quantitative analysis of secondary metabolites was also carried out. The presence of phenolics was also studied by HPLC. The GC-MS analysis of Malcolmia africana essential oil and fixed oil was also carried out. (author)

  20. ¹H NMR and HPLC/DAD for Cannabis sativa L. chemotype distinction, extract profiling and specification.

    Science.gov (United States)

    Peschel, Wieland; Politi, Matteo

    2015-08-01

    The medicinal use of different chemovars and extracts of Cannabis sativa L. requires standardization beyond ∆9-tetrahydrocannabinol (THC) with complementing methods. We investigated the suitability of (1)H NMR key signals for distinction of four chemotypes measured in deuterated dimethylsulfoxide together with two new validated HPLC/DAD methods used for identification and extract profiling based on the main pattern of cannabinoids and other phenolics alongside the assayed content of THC, cannabidiol (CBD), cannabigerol (CBG) their acidic counterparts (THCA, CBDA, CBGA), cannabinol (CBN) and cannflavin A and B. Effects on cell viability (MTT assay, HeLa) were tested. The dominant cannabinoid pairs allowed chemotype recognition via assignment of selective proton signals and via HPLC even in cannabinoid-low extracts from the THC, CBD and CBG type. Substantial concentrations of cannabinoid acids in non-heated extracts suggest their consideration for total values in chemotype distinction and specifications of herbal drugs and extracts. Cannflavin A/B are extracted and detected together with cannabinoids but always subordinated, while other phenolics can be accumulated via fractionation and detected in a wide fingerprint but may equally serve as qualitative marker only. Cell viability reduction in HeLa was more determined by the total cannabinoid content than by the specific cannabinoid profile. Therefore the analysis and labeling of total cannabinoids together with the content of THC and 2-4 lead cannabinoids are considered essential. The suitability of analytical methods and the range of compound groups summarized in group and ratio markers are discussed regarding plant classification and pharmaceutical specification. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Improvement in HPLC separation of acetic acid and levulinic acid in the profiling of biomass hydrolysate.

    Science.gov (United States)

    Xie, Rui; Tu, Maobing; Wu, Yonnie; Adhikari, Sushil

    2011-04-01

    5-Hydroxymethylfurfural (HMF) and furfural could be separated by the Aminex HPX-87H column chromatography, however, the separation and quantification of acetic acid and levulinic acid in biomass hydrolysate have been difficult with this method. In present study, the HPLC separation of acetic acid and levulinic acid on Aminex HPX-87H column has been investigated by varying column temperature, flow rate, and sulfuric acid content in the mobile phase. The column temperature was found critical in resolving acetic acid and levulinic acid. The resolution for two acids increased dramatically from 0.42 to 1.86 when the column temperature was lowered from 60 to 30 °C. So did the capacity factors for levulinic acid that was increased from 1.20 to 1.44 as the column temperature dropped. The optimum column temperature for the separation was found at 45 °C. Variation in flow rate and sulfuric acid concentration improved not as much as the column temperature did. Published by Elsevier Ltd.

  2. HPLC-DAD-MS/MS profiling of antioxidant flavonoid glycosides in sea buckthorn (Hippophae rhamnoides L.) seeds.

    Science.gov (United States)

    Arimboor, Ranjith; Arumughan, C

    2012-09-01

    This study was aimed at the chemical profiling of flavonoid glycosides in antioxidant (AO) fractions of sea buckthorn (Hippophae rhamnoides) seed. Seed fractions were evaluated for their DPPH, ABTS, superoxide and hydroxyl radical scavenging, ferric reduction, ferrous chelation and xanthine oxidase inhibitory capacities. HPLC-DAD-ESI-MS/MS analytical conditions for the profiling of seed flavonoids were optimized and the AO-rich fraction was analysed. Quercetin-3-O-rutinoside (5.9%), isorhamnetin-3-O-rutinoside (4.9%) and isorhamnetin-3-O-sophroside-7-O-rhamnoside (3.7%) were found as the major flavonoid glycosides in the fraction. Significant amounts of isorhamnetin-3-O-glucoside (2.8%), 3-O-sophroside-7-O-rhamnosides of quercetin (2.4%) and kaempherol (1.3%), and 3-O-glucoside-7-O-rhamnosides of quercetin (1.1%) and isorhamnetin (1.1%) along with their free forms: isorhamnetin (2.7%), quercetin (1.1%) and kaempherol (0.6%) were also found in the fraction. The identification of flavonoids as the major less polar AO phenolics in the seeds was rationalized by demonstrating the high AO activity of isorhamnetin, quercetin, kaempherol and quercetin-3-O-rutinoside.

  3. HPLC Evaluation of Phenolic Profile, Nutritive Content, and Antioxidant Capacity of Extracts Obtained from Punica granatum Fruit Peel

    Science.gov (United States)

    Middha, Sushil Kumar; Usha, Talambedu; Pande, Veena

    2013-01-01

    This study revealed polyphenolic content, nutritive content, antioxidant activity, and phenolic profile of methanol and aqueous extracts of Punica granatum peel extract. For this, extracts were screened for possible antioxidant activities by free radical scavenging activity (DPPH), hydrogen peroxide scavenging activity and ferric-reducing antioxidant power (FRAP) assays. The total phenolics and flavonoid recovered by methanolic (MPE) and the water extract (AQPE) were ranged from 185 ± 12.45 to 298.00 ± 24.86 mg GAE (gallic acid equivalents)/gm and 23.05 ± 1.54 to 49.8 ± 2.14 quercetin (QE) mg/g, respectively. The EC50 of herbal extracts ranged from 100 µg/ml (0.38 quercetin equivalents), for AQPE, 168 µg/ml (0.80 quercetin equivalents), for MPE. The phenolic profile in the methanolic extracts was investigated by chromatographic (HPLC) method. About 5 different flavonoids, phenolic acids, and their derivatives including quercetin (1), rutin (2), gallic acid (3), ellagic acid (4), and punicalagin as a major ellagitannin (5) have been identified. Among both extracts, methanolic extract was the most effective. This report may be the first to show nutritive content and correlation analysis to suggest that phenols and flavonoids might contribute the high antioxidant activity of this fruit peel and establish it as a valuable natural antioxidant source applicable in the health food industry. PMID:23983682

  4. Morphological profiles of neutron and X-irradiated small intestine

    International Nuclear Information System (INIS)

    Carr, K.E.; O'Shea, O.; Hazzard, R.A.; McCullough, J.S.; Hume, S.P.; Nelson, A.C.

    1996-01-01

    This paper describes the response of mouse small intestine, at several time points after treatment with neutron or X-irradiation, using doses expected to give similar effects in terms of crypt/microcolony survival. Using resin histology, the effects of radiation on the numbers of duodenal cell types and measurements of tissue areas were assessed. The results for individual parameters and for an estimate of overall damage are given in a data display, which summarises the morphological profile of the organ after both types of radiation. Damage and recovery were seen for many of the parameters studied but there was no standard response pattern applicable for all parameters. In particular, the response of individual crypt cell types could not be predicted from knowledge of the change in crypt numbers. With regard to the holistic response of the gut, neutron irradiation appeared to have caused more damage and produced more early effects than the X-irradiation. More specifically, neutron treatment led to more damage to the neuromuscular components of the wall, while X-irradiation produced early vascular changes. (author)

  5. Enantioselective Effects of Metalaxyl Enantiomers on Breast Cancer Cells Metabolic Profiling Using HPLC-QTOF-Based Metabolomics

    Directory of Open Access Journals (Sweden)

    Ping Zhang

    2017-01-01

    Full Text Available In this study, an integrative high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-QTOF based metabolomics approach was performed to evaluate the enantioselective metabolic perturbations in MCF-7 cells after treatment with R-metalaxyl and S-metalaxyl, respectively. Untargeted metabolomics profile, multivariate pattern recognition, metabolites identification, and pathway analysis were determined after metalaxyl enantiomer exposure. Principal component analysis (PCA and partitial least-squares discriminant analysis (PLS-DA directly reflected the enantioselective metabolic perturbations induced by metalaxyl enantiomers. On the basis of multivariate statistical results, a total of 49 metabolites including carbohydrates, amino acids, nucleotides, fatty acids, organic acids, phospholipids, indoles, derivatives, etc. were found to be the most significantly changed metabolites and metabolic fluctuations caused by the same concentration of R-metalaxyl and S-metalaxyl were enantioselective. Pathway analysis indicated that R-metalaxyl and S-metalaxyl mainly affected the 7 and 10 pathways in MCF-7 cells, respectively, implying the perturbed pathways induced by metalaxyl enantiomers were also enantioselective. Furthermore, the significantly perturbed metabolic pathways were highly related to energy metabolism, amino acid metabolism, lipid metabolism, and antioxidant defense. Such results provide more specific insights into the enantioselective metabolic effects of chiral pesticides in breast cancer progression, reveal the underlying mechanisms, and provide available data for the health risk assessments of chiral environmental pollutants at the molecular level.

  6. Piper betle leaves: profiling phenolic compounds by HPLC/DAD-ESI/MS(n) and anti-cholinesterase activity.

    Science.gov (United States)

    Ferreres, Federico; Oliveira, Andreia P; Gil-Izquierdo, Angel; Valentão, Patrícia; Andrade, Paula B

    2014-01-01

    Piper betle L. is a widely distributed plant in the tropical and subtropical regions, its leaves being largely consumed as a masticator and mouth freshener. The purposes of this work were to characterise the phenolic profile of this species and to improve knowledge of its anti-cholinesterase properties. The phenolic composition of P. betle leaf aqueous and ethanol extracts was characterised by HPLC coupled with a diode-array detector and combined with electrospray ionisation tandem MS, and in vitro cholinesterase inhibitory capacity of both extracts was assessed by spectrophotometric microassays. The effect on neuronal cells (SH-SY5Y) viability was evaluated by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide reduction and lactate dehydrogenase leakage. Twelve phenolic compounds, comprising a phenylpropanoid, five cinnamoyl and six flavonoids derivatives were identified in P. betle leaves. Hydroxychavicol was the major compound in both extracts; however, the aqueous extract presented a greater diversity of compounds. Both extracts showed strong activity against both acetyl- and butyrylcholinesterase, which can be due, at least partially, to the phenolic composition. Furthermore, the aqueous extract proved to be cytotoxic to human neuroblastoma cells at concentrations higher than 500 µg/mL. The results suggest that the consumption of P. betle leaves as an infusion can have a positive impact in the prevention and treatment of neurodegenerative diseases. Apigenin and luteolin derivatives are reported for the first time in this species. Copyright © 2014 John Wiley & Sons, Ltd.

  7. Stability-indicating HPLC-DAD/UV-ESI/MS impurity profiling of the anti-malarial drug lumefantrine.

    Science.gov (United States)

    Verbeken, Mathieu; Suleman, Sultan; Baert, Bram; Vangheluwe, Elien; Van Dorpe, Sylvia; Burvenich, Christian; Duchateau, Luc; Jansen, Frans H; De Spiegeleer, Bart

    2011-02-28

    Lumefantrine (benflumetol) is a fluorene derivative belonging to the aryl amino alcohol class of anti-malarial drugs and is commercially available in fixed combination products with β-artemether. Impurity characterization of such drugs, which are widely consumed in tropical countries for malaria control programmes, is of paramount importance. However, until now, no exhaustive impurity profile of lumefantrine has been established, encompassing process-related and degradation impurities in active pharmaceutical ingredients (APIs) and finished pharmaceutical products (FPPs). Using HPLC-DAD/UV-ESI/ion trap/MS, a comprehensive impurity profile was established based upon analysis of market samples as well as stress, accelerated and long-term stability results. In-silico toxicological predictions for these lumefantrine related impurities were made using Toxtree® and Derek®. Several new impurities are identified, of which the desbenzylketo derivative (DBK) is proposed as a new specified degradant. DBK and the remaining unspecified lumefantrine related impurities are predicted, using Toxtree® and Derek®, to have a toxicity risk comparable to the toxicity risk of the API lumefantrine itself. From unstressed, stressed and accelerated stability samples of lumefantrine API and FPPs, nine compounds were detected and characterized to be lumefantrine related impurities. One new lumefantrine related compound, DBK, was identified and characterized as a specified degradation impurity of lumefantrine in real market samples (FPPs). The in-silico toxicological investigation (Toxtree® and Derek®) indicated overall a toxicity risk for lumefantrine related impurities comparable to that of the API lumefantrine itself.

  8. Sugars profiles of different chestnut (Castanea sativa Mill.) and almond (Prunus dulcis) cultivars by HPLC-RI.

    Science.gov (United States)

    Barreira, João C M; Pereira, José Alberto; Oliveira, M Beatriz P P; Ferreira, Isabel C F R

    2010-03-01

    Sugar profiles of different almond and chestnut cultivars were obtained by high-performance liquid chromatography (HPLC), by means of a refractive index (RI) detector. A solid-liquid extraction procedure was used in defatted and dried samples. The chromatographic separation was achieved using a Eurospher 100-5 NH(2) column using an isocratic elution with acetonitrile/water (70:30, v/v) at a flow rate of 1.0 ml/min. All the compounds were separated in 16 min. The method was optimized and proved to be reproducible and accurate. Generally, more than 95% of sugars were identified for both matrixes. Sugars profiles were quite homogeneous for almond cultivars; sucrose was the main sugar (11.46 +/- 0.14 in Marcona to 22.23 +/- 0.59 in Ferragnes g/100 g of dried weight), followed by raffinose (0.71 +/- 0.05 in Ferraduel to 2.11 +/- 0.29 in Duro Italiano), glucose (0.42 +/- 0.12 in Pegarinhos two seeded to 1.47 +/- 0.19 in Ferragnes) and fructose (0.11 +/- 0.02 in Pegarinhos two seeded to 0.59 +/- 0.05 in Gloriette). Commercial cultivars proved to have higher sucrose contents, except in the case of Marcona. Nevertheless, chestnut cultivars revealed a high heterogeneity. Sucrose was the main sugar in Aveleira (22.05 +/- 1.48), Judia (23.30 +/- 0.83) and Longal (9.56 +/- 0.91), while glucose was slightly prevalent in Boa Ventura (6.63 +/- 0.49). The observed variance could serve for inter-cultivar discrimination.

  9. Metabolite profiling with HPLC-ICP-MS as a tool for in vivo characterization of imaging probes.

    Science.gov (United States)

    Boros, Eszter; Pinkhasov, Omar R; Caravan, Peter

    2018-01-01

    Current analytical methods for characterizing pharmacokinetic and metabolic properties of positron emission tomography (PET) and single photon emission computed tomography (SPECT) probes are limited. Alternative methods to study tracer metabolism are needed. The study objective was to assess the potential of high performance liquid chromatography - inductively coupled plasma - mass spectrometry (HPLC-ICP-MS) for quantification of molecular probe metabolism and pharmacokinetics using stable isotopes. Two known peptide-DOTA conjugates were chelated with nat Ga and nat In. Limit of detection of HPLC-ICP-MS for 69 Ga and 115 In was determined. Rats were administered 50-150 nmol of Ga- and/or In-labeled probes, blood was serially sampled, and plasma analyzed by HPLC-ICP-MS using both reverse phase and size exclusion chromatography. The limits of detection were 0.16 pmol for 115 In and 0.53 pmol for 69 Ga. Metabolites as low as 0.001 %ID/g could be detected and transchelation products identified. Simultaneous administration of Ga- and In-labeled probes allowed the determination of pharmacokinetics and metabolism of both probes in a single animal. HPLC-ICP-MS is a robust, sensitive and radiation-free technique to characterize the pharmacokinetics and metabolism of imaging probes.

  10. Dual High-Resolution α-Glucosidase and Radical Scavenging Profiling Combined with HPLC-HRMS-SPE-NMR for Identification of Minor and Major Constituents Directly from the Crude Extract of Pueraria lobata

    DEFF Research Database (Denmark)

    Liu, Bingrui; Kongstad, Kenneth Thermann; Qinglei, Sun

    2015-01-01

    The crude methanol extract of Pueraria lobata was investigated by dual high-resolution α-glucosidase inhibition and radical scavenging profiling combined with hyphenated HPLC-HRMS-SPE-NMR. Direct analysis of the crude extract without preceding purification was facilitated by combining chromatograms...... from two analytical-scale HPLC separations of 120 and 600 μg on-column, respectively. High-resolution α-glucosidase and radical scavenging profiles were obtained after microfractionation of the eluate in 96-well microplates. This allowed full bioactivity profiling of individual peaks in the HPLC...... chromatogram of the crude methanol extract. Subsequent HPLC-HRMS-SPE-NMR analysis allowed identification of 21 known compounds in addition to two new compounds, i.e., 3′-methoxydaidzein 8-C-[α-d-apiofuranosyl-(1→6)]-β-d-glucopyranoside and 6″-O-malonyl-3′-methoxydaidzin, as well as an unstable compound...

  11. Morphological and physiological profile of elite basketball players in Belgium

    OpenAIRE

    Boone, Jan; Bourgois, Jan

    2013-01-01

    PURPOSE: The present study aimed to gain insight into the physiological profile of elite basketball players in Belgium in relation to their position on the field. METHODS: The group consisted of 144 players, divided into 5 groups according to position (point guards [PG], shooting guards [SG], small forwards [SF], power forwards [PF] and centers [C]). The anthropometrics were measured and the subjects underwent fitness tests (incremental running test, 10m-sprint,5x10m,Squat and Counter Move...

  12. High-resolution α-glucosidase inhibition profiling combined with HPLC-HRMS-SPE-NMR for identification of anti-diabetic compounds in Eremanthus crotonoides (Asteraceae)

    DEFF Research Database (Denmark)

    Lana e Silva, Eder; Felipe Revoredo Lobo, Jonathas; Vinther, Joachim Møllesøe

    2016-01-01

    with an inhibitory concentration (IC50) of 34.5 μg/mL towards α-glucosidase was investigated by high-resolution α-glucosidase inhibition profiling combined with HPLC-HRMS-SPE-NMR. This led to identification of six α-glucosidase inhibitors, namely quercetin (16), trans-tiliroside (17), luteolin (19), quercetin-3.......93 and 5.20 μM, respectively. This is the first report of the α-glucosidase inhibitory activity of compounds 20, 26, and 29, and the findings support the important role of Eremanthus species as novel sources of new drugs and/or herbal remedies for treatment of type 2 diabetes....

  13. Dissolution profiles of perindopril and indapamide in their fixed-dose formulations by a new HPLC method and different mathematical approaches

    Directory of Open Access Journals (Sweden)

    Gumieniczek Anna

    2015-09-01

    Full Text Available A new HPLC method was introduced and validated for simultaneous determination of perindopril and indapamide. Validation procedure included specificity, sensitivity, robustness, stability, linearity, precision and accuracy. The method was used for the dissolution test of perindopril and indapamide in three fixed-dose formulations. The dissolution procedure was optimized using different media, different pH of the buffer, surfactants, paddle speed and temperature. Similarity of dissolution profiles was estimated using different model-independent and model-dependent methods and, additionally, by principal component analysis (PCA. Also, some kinetic models were checked for dissolved amounts of drugs as a function of time.

  14. Characterization of Jamaican agro-industrial wastes. Part II, fatty acid profiling using HPLC: precolumn derivatization with phenacyl bromide.

    Science.gov (United States)

    Bailey-Shaw, Y A; Golden, K D; Pearson, A G M; Porter, R B R

    2012-09-01

    This paper describes the determination of fatty acid composition of coffee, citrus and rum distillery wastes using reversed-phase high-performance liquid chromatography (RP-HPLC). Lipid extracts of the waste samples are derivatized with phenacyl bromide and their phenacyl esters are separated on a C8 reversed-phase column by using continuous gradient elution with water and acetonitrile. The presence of saturated and unsaturated fatty acids in quantifiable amounts in the examined wastes, as well as the high percentage recoveries, are clear indications that these wastes have potential value as inexpensive sources of lipids. The HPLC procedures described here could be adopted for further analysis of materials of this nature.

  15. Phenolic Profiling of the South American “Baylahuen” Tea (Haplopappus spp., Asteraceae by HPLC-DAD-ESI-MS

    Directory of Open Access Journals (Sweden)

    Guillermo Schmeda-Hirschmann

    2015-01-01

    Full Text Available The aerial parts of several Haplopappus species (Asteraceae, known under the common name “baylahuen”, are used as herbal teas in Chile and Argentina. In Chile, “baylahuen” comprises H. multifolius, H. taeda, H. baylahuen and H. rigidus. Little is known about the chemical identity of the infusion constituents in spite of widespread consumption. The aim of the present work was the characterization of phenolics occurring in the infusions and methanol extracts of “baylahuen” by HPLC-DAD-ESI-MS. A simple HPLC-DAD-ESI-MS method was developed for the fast identification and differentiation of Haplopappus spp. used as a tea source, based on the phenolics from the tea and methanol extracts. Some 27 phenolics were tentatively identified in the infusions and methanol extract, including 10 caffeoyl quinic and feruloyl quinic acid derivatives and 17 flavonoids. The HPLC patterns of the Haplopappus tea and methanol extract allow a clear differentiation at the species level. The occurrence of hydroxycinnamic acid derivatives and flavonoids can explain the reputed nutraceutical and health beneficial properties of this herbal tea.

  16. HPLC PROFILING OF PHENOLIC ACIDS AND FLAVONOIDS AND EVALUATION OF ANTI-LIPOXYGENASE AND ANTIOXIDANT ACTIVITIES OF AQUATIC VEGETABLE LIMNOCHARIS FLAVA.

    Science.gov (United States)

    Ooh, Keng-fei; Ong, Hean-Chooi; Wong, Fai-Chu; Chai, Tsun-Thai

    2015-01-01

    Limnocharis flava is an edible wetland plant, whose phenolic acid and flavonoid compositions as well as bioactivities were underexplored. This study analyzed the profiles of selected hydroxybenzoic acids, hydroxycinnamic acids and flavonoids in the aqueous extracts of L. flava leaf, rhizome and root by high performance liquid chromatography (HPLC). Anti-lipoxygenase and antioxidant (iron chelating, 2,2-diphenyl-l-picrylhydrazyl (DPPH) radical scavenging, and nitric oxide (NO) scavenging) activities of the extracts were also evaluated. Leaf extract had the highest phenolic contents, being most abundant in p-hydroxybenzoic acid (3861.2 nmol/g dry matter), ferulic acid (648.8 nmol/g dry matter), and rutin (4110.7 nmol/g dry matter). Leaf extract exhibited the strongest anti-lipoxygenase (EC50 6.47 mg/mL), iron chelating (EC50 6.65 mg/mL), DPPH scavenging (EC50 15.82 mg/mL) and NO scavenging (EC50 3.80 mg/mL) activities. Leaf extract also had the highest ferric reducing ability. This is the most extensive HPLC profiling of phenolic acids and flavonoids in L.flava to date. In conclusion, L. flava leaf is a source of health-promoting phenolics, anti-lipoxygenase agents and antioxidants.

  17. Comparative evaluation of ICP sample introduction systems to be used in the metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS.

    Science.gov (United States)

    Klencsár, Balázs; Sánchez, Carlos; Balcaen, Lieve; Todolí, José; Lynen, Frederic; Vanhaecke, Frank

    2018-05-10

    A systematic evaluation of four different ICP sample introduction systems to be used in the context of metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS was carried out using diclofenac and its major metabolite, 4'-hydroxy-diclofenac, as model compounds. The strict requirements for GMP validation of chromatographic methods in the pharmaceutical industry were adhered to in this context. The final aim of this investigation is an extension of the applicability and validatability of HPLC-ICP-MS in the field of pharmaceutical R&D. Five different gradient programmes were tested while the baseline peak width (w b ), peak capacity (P), USP tailing factor (A s ) and USP signal-to-noise ratio (USP S/N) were determined as major indicators of the chromatographic performance and the values obtained were compared to the corresponding FDA recommendations (if applicable). Four different ICP-MS sample introductions systems were investigated involving two units typically working at higher flow rates (∼1.0 mL min -1 ) and another two systems working at lower flow rates (∼0.1 mL min -1 ). Optimal conditions with potential for applicability under GMP conditions were found at a mobile phase flow rate of 1.0 mL min -1 by using a pneumatic micro-flow LC nebulizer mounted onto a Peltier-cooled cyclonic spray chamber cooled to -1 °C for sample introduction. Under these conditions, HPLC-ICP-MS provided a chromatographic performance similar to that of HPLC with UV detection. The peak shape (USP tailing factor = 1.1-1.4) was significantly improved compared to that obtained with the Peltier-cooled Scott-type spray chamber. Two alternative sample introduction systems - a POINT ® and a High-Temperature Torch-Integrated Sample Introduction System (hTISIS) - were also tested at a flow rate of 0.1 mL min -1 using a chromatographic column with 1.0 mm ID. Although these systems allowed the peak shape to be improved compared to that obtained with

  18. HPLC-DAD PROFILE OF PHENOLIC COMPOUNDS, CYTOTOXICITY, ANTIOXIDANT AND ANTI-INFLAMMATORY ACTIVITIES OF THE AMAZON FRUIT Caryocar villosum

    Directory of Open Access Journals (Sweden)

    Klenicy K. L. Yamaguchi

    Full Text Available Piquiá (Caryocar villosum - Caryocaraceae is a native fruit from the Amazon region rich in bioactive substances. Fruit pulp extracts were analyzed by HPLC, together with extracts obtained from fruit pulp industry residual parts, byproducts such as husks (shells and seeds. Extracts were prepared with two ethanolic solvent systems. Phenolic substances ellagic and gallic acids were detected with standards and quantified by HPLC. Cytotoxic, antioxidant and anti-inflammatory activities in vitro were also evaluated. Shell extracts showed free radicals scavenger capacity in ABTS (IC50: 3.93 ± 0.12 µg mL-1 and DPPH models (IC50: 7.81 ± 0.34 µg mL-1, low cytotoxicity in human fibroblasts, but high at tumor strains, and also a high anti-inflammatory potential observed by the inhibition of nitric oxide production. At low concentrations (20 µg mL-1, excellent antioxidant activities were verified in cellular assays, with percentages of 70.69 ± 2.77%, 79.89 ± 6.50% and 79.48 ± 8.6% for shell, pulp and seed extracts, respectively. With this set of results, C. villosum fruit extracts become a high potential raw material to be used in pharmaceutical and cosmetic applications.

  19. Nose profile morphology and accuracy study of nose profile estimation method in Scottish subadult and Indonesian adult populations.

    Science.gov (United States)

    Sarilita, Erli; Rynn, Christopher; Mossey, Peter A; Black, Sue; Oscandar, Fahmi

    2018-05-01

    This study investigated nose profile morphology and its relationship to the skull in Scottish subadult and Indonesian adult populations, with the aim of improving the accuracy of forensic craniofacial reconstruction. Samples of 86 lateral head cephalograms from Dundee Dental School (mean age, 11.8 years) and 335 lateral head cephalograms from the Universitas Padjadjaran Dental Hospital, Bandung, Indonesia (mean age 24.2 years), were measured. The method of nose profile estimation based on skull morphology previously proposed by Rynn and colleagues in 2010 (FSMP 6:20-34) was tested in this study. Following this method, three nasal aperture-related craniometrics and six nose profile dimensions were measured from the cephalograms. To assess the accuracy of the method, six nose profile dimensions were estimated from the three craniometric parameters using the published method and then compared to the actual nose profile dimensions.In the Scottish subadult population, no sexual dimorphism was evident in the measured dimensions. In contrast, sexual dimorphism of the Indonesian adult population was evident in all craniometric and nose profile dimensions; notably, males exhibited statistically significant larger values than females. The published method by Rynn and colleagues (FSMP 6:20-34, 2010) performed better in the Scottish subadult population (mean difference of maximum, 2.35 mm) compared to the Indonesian adult population (mean difference of maximum, 5.42 mm in males and 4.89 mm in females).In addition, regression formulae were derived to estimate nose profile dimensions based on the craniometric measurements for the Indonesian adult population. The published method is not sufficiently accurate for use on the Indonesian population, so the derived method should be used. The accuracy of the published method by Rynn and colleagues (FSMP 6:20-34, 2010) was sufficiently reliable to be applied in Scottish subadult population.

  20. An HPLC-MS characterization of the changes in sweet orange leaf metabolite profile following infection by the bacterial pathogen Candidatus Liberibacter asiaticus.

    Science.gov (United States)

    Hijaz, Faraj M; Manthey, John A; Folimonova, Svetlana Y; Davis, Craig L; Jones, Shelley E; Reyes-De-Corcuera, José I

    2013-01-01

    Huanglongbing (HLB) presumably caused by Candidatus Liberibacter asiaticus (CLas) threatens the commercial U.S. citrus crop of an annual value of $3 billion. The earliest shift in metabolite profiles of leaves from greenhouse-grown sweet orange trees infected with Clas, and of healthy leaves, was characterized by HPLC-MS concurrently with PCR testing for the presence of Clas bacteria and observation of disease symptoms. Twenty, 8-month-old 'Valencia' and 'Hamlin' trees were grafted with budwood from PCR-positive HLB source trees. Five graft-inoculated trees of each variety and three control trees were sampled biweekly and analyzed by HPLC-MS and PCR. Thirteen weeks after inoculation, Clas was detected in newly growing flushes in 33% and 55% of the inoculated 'Hamlin' and 'Valencia' trees, respectively. Inoculated trees remained asymptomatic in the first 20 weeks, but developed symptoms 30 weeks after grafting. No significant differences in the leaf metabolite profiles were detected in Clas-infected trees 23 weeks after inoculation. However, 27 weeks after inoculation, differences in metabolite profiles between control leaves and those of Clas-infected trees were evident. Affected compounds were identified with authentic standards or structurally classified by their UV and mass spectra. Included among these compounds are flavonoid glycosides, polymethoxylated flavones, and hydroxycinnamates. Four structurally related hydroxycinnamate compounds increased more than 10-fold in leaves from 'Hamlin' and 'Valencia' sweet orange trees in response to Clas infection. Possible roles of these hydroxycinnamates as plant defense compounds against the Clas infection are discussed.

  1. Investigation of the profile and kinetics of degradation of rivaroxaban using HPLC, TLC-densitometry and LC/MS/MS: Application to pre-formulation studies

    Directory of Open Access Journals (Sweden)

    Mohamed A. Abdallah

    2015-06-01

    Full Text Available Rivaroxaban (RIVA, an amide group-containing oral anticoagulant was subjected to stress conditions commonly required for the registration of pharmaceuticals: base and acid-catalyzed hydrolysis (0.1 M, 60 °C, 3–6 h, oxidation (10% H2O2, 24 h, photodegradation (300–800 nm, 24 h and thermal decomposition (50 °C, 6 h. Two major degradation products were separated and identified using TLC and LC/MS/MS, respectively. An orthogonal stability-indicating testing protocol (RP-HPLC and NP-TLC-densitometry was developed and validated according to ICH guidelines. Both assays enabled the determination of RIVA in the presence of its degradation products as well as the kinetics of degradation. Determination was carried out over a concentration range of (5.00–50.00 μg/mL and (0.40–12.00 μg/band with an accuracy of (100.81% ± 1.03 and (100.29% ± 1.08 for HPLC and TLC-densitometry, respectively. Results indicated that RIVA was stable towards oxidation, photodegradation and thermal decomposition but extremely sensitive to hydrolysis. Two major degradation products were detected in the case of base-catalyzed hydrolysis while only one degradation product was detected upon acid-catalyzed hydrolysis. This could be attributed to the presence of amide groups in RIVA structure of different stability profiles. The kinetics of hydrolysis was investigated in more detail and the reaction was found to follow the pseudo first order kinetics, as confirmed by the results of both HPLC and TLC-densitometric assays. The applicability of the assay for the determination of RIVA content and dissolution pattern of the innovator product as well as three generic formulations was demonstrated.

  2. Chemical profiling of anti-hepatocellular carcinoma constituents from Caragana tangutica Maxim. by off-line semi-preparative HPLC-NMR.

    Science.gov (United States)

    Yang, Xinzhou; Huang, Mi; Cai, Jinyan; Lv, Dan; Lv, Jingnan; Zheng, Sijian; Ma, Xinhua; Zhao, Ping; Wang, Qiang

    2017-05-01

    An EtOAc fraction from the roots of Caragana tangutica Maxim. (CTEA) displayed promising anti-hepatocellular carcinoma (HCC) activity during screening of a traditional Chinese ethnic herb library against HepG2 and Hep3B cell lines. HPLC-based activity profiling of CTEA by combination of MS-guided large-scale semi-preparative HPLC and NMR methods led to the identification of a new pterocarpan glycoside, (-)-maackiain 3-O-6'-O-methyl malonyl-β-d-glucopyranoside (1), together with three known pterocarpan glycosides, (-)-maackiain 3-O-β-d-glucopyranoside (2), 3-O-6'-O-acrylyl-β-d-galactopyranoside (3), and (-)-maackiain 3-O-6'-O-acetyl-β-d-glucopyranoside (4). Compound 1 was isolated during a drug discovery programme aimed at identifying new anti-HCC leads from a natural product library. Anti-HCC study showed that all four compounds exhibited cytotoxic activity with IC 50 values range of 29.1-53.5 μg/mL against HepG2 and Hep3B cell lines.

  3. Impurity profiling of liothyronine sodium by means of reversed phase HPLC, high resolution mass spectrometry, on-line H/D exchange and UV/Vis absorption.

    Science.gov (United States)

    Ruggenthaler, M; Grass, J; Schuh, W; Huber, C G; Reischl, R J

    2017-09-05

    For the first time, a comprehensive investigation of the impurity profile of the synthetic thyroid API (active pharmaceutical ingredient) liothyronine sodium (LT 3 Na) was performed by using reversed phase HPLC and advanced structural elucidation techniques including high resolution tandem mass spectrometry (HRMS/MS) and on-line hydrogen-deuterium (H/D) exchange. Overall, 39 compounds were characterized and 25 of these related substances were previously unknown to literature. The impurity classification system recently developed for the closely related API levothyroxine sodium (LT 4 Na) could be applied to the newly characterized liothyronine sodium impurities resulting in a wholistic thyroid API impurity classification system. Furthermore, the mass-spectrometric CID-fragmentation of specific related substances was discussed and rationalized by detailed fragmentation pathways. Moreover, the UV/Vis absorption characteristics of the API and selected impurities were investigated to corroborate chemical structure assignments derived from MS data. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Free radicals quenching potential, protective properties against oxidative mediated ion toxicity and HPLC phenolic profile of a Cameroonian spice: Piper guineensis.

    Science.gov (United States)

    Moukette Moukette, Bruno; Constant Anatole, Pieme; Nya Biapa, Cabral Prosper; Njimou, Jacques Romain; Ngogang, Jeanne Yonkeu

    2015-01-01

    Considerations on antioxidants derived from plants have continuously increased during this decade because of their beneficial effects on human health. In the present study we investigated the free radical scavenging properties of extracts from Piper guineense ( P. guineense ) and their inhibitory potentials against oxidative mediated ion toxicity. The free radical quenching properties of the extracts against [1,1-diphenyl-2-picrylhydrazyl (DPPH•), 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS•), hydroxyl radical (HO•), nitric oxide (NO•)] radical and their antioxidant potentials by FRAP and phosphomolybdenum were determined as well as their protective properties on liver enzymes. The phenolic profile was also investigated by HPLC. The results obtained, revealed that the extracts significantly inhibited the DPPH, NO, HO and ABTS radicals in a concentration depending manner. They also showed a significant ferrous ion chelating ability through FRAP and phosphomolybdenum antioxidant potential. Their polyphenol contents varied depending on the type of extracts and the solvent used. The hydroethanolic extracts (FFH) and the ethanolic extracts (FFE) of P. guineense leaves showed the higher level of phenolic compounds respectively of 21.62 ± 0.06 mg caffeic acid/g dried extract (CAE/g DE) and 19.01 ± 0.03 CAE/g DE. The HPLC phenolic compounds profile revealed a higher quantity of Eugenol, quercetin, rutin and catechin in the stem than in the leaves. The presence of these molecules could be responsible of the protective potentials of P. guineense extracts against lipid peroxidation and SOD, catalase and peroxidase. In conclusion, P. guineense extracts demonstrated significant antioxidant property and may be used as a prospective protector against metal related toxicity.

  5. Genetic transformation of the endangered Tibetan medicinal plant Przewalskia tangutica Maxim and alkaloid production profiling revealed by HPLC.

    Science.gov (United States)

    Lei, Tianxiang; Wang, Huan; Li, Songling; Shen, Jianwei; Chen, Shilong; Cai, Xiaojian; Zhou, Dangwei

    2018-03-01

    To achieve a high yield of tropane alkaloids (TA) and exploit the alpine plant sustainably, an optimized protocol for induction and establishment of hairy roots culture of Prezwalskia tangutica Maxim was developed through selection of appropriate Agrobacterium strain and the explant type. The hypocotyl is more readily facile to induce the HR than the cotyledon is when infected with the three different agrobacterium strains. MUS440 has an efficiency (of up to 20%), whereas the ATCC10060 (A4) can induce HR on both types of explants with the highest frequency (33.33%), root length (21.17 ± 2.84 cm), and root number (10.83 ± 1.43) per explant than the other strains. The highest HR production resulted from using hypocotyl as explants. Independent transformed HR was able to grow vigorously and to propagate on a no-hormone 1/2MS liquid medium. The presence of pRi rol B gene in transformation of HR was confirmed by PCR amplification. In the liquid medium, the HR growth curve appeared to be "S" shaped, and ADB had increased to 4.633 g/l. Moreover, HPLC analysis showed that HR lines have an extraordinary ability to produce atropine (229.88 mg/100 g), anisodine (4.09 mg/100 g), anisodamine (12.85 mg/100 g), and scopolamine (10.69 mg/100 g), which were all more significant than the control roots. In conclusion, our study optimized the culture condition and established a feasible genetics reactor for P. tangutica green exploration and biological study in the alpine region.

  6. Chemical profile analysis and comparison of two versions of the classic TCM formula Danggui Buxue Tang by HPLC-DAD-ESI-IT-TOF-MSn.

    Science.gov (United States)

    Zhang, Ya-Zhou; Xu, Feng; Yi, Tao; Zhang, Jian-Ye; Xu, Jun; Tang, Yi-Na; He, Xi-Chen; Liu, Jing; Chen, Hu-Biao

    2014-04-30

    Danggui Buxue Tang (DBT) is a Traditional Chinese Medicine (TCM) formula primarily used to treat symptoms associated with menopause in women. Usually, DBT is composed of one portion of Radix Angelicae Sinensis (RAS) and five portions of Radix Astragali (RA). Clinically, Radix Hedysari (RH) is sometimes used by TCM physicians to replace RA in DBT. In order to verity whether the chemical constituents of the DBT1 (RA:RAS = 5:1, w/w) and DBT2 (RH:RAS = 5:1, w/w) share similarities the chemical profiles of the two DBTs crude extracts and urine samples were analyzed and compared with the aid of HPLC-DAD-ESI-IT-TOF-MSn, which determines the total ion chromatogram (TIC) and multi-stage mass spectra (MSn). Then, the DBT1 and DBT2 were identified and compared on the basis of the TIC and the MSn. In the first experiment (with crude extracts), 69 compounds (C1-C69) were identified from the DBT1; 46 compounds (c1-c46) were identified from the DBT2. In the second experiment(with urine samples), 44 compounds (M1-M44) were identified from the urine samples of rats that had been administered DBT1, and 34 compounds (m1-m34) were identified from the urine samples of rats that had been administered DBT2. Identification and comparison of the chemical compositions were carried out between the DBT1 and DBT2 of the crude extracts and urine samples respectively. Our results showed that the two crude extracts of the DBTs have quite different chemical profiles. The reasons for their differences were that the special astragalosides in DBT1 and the isoflavonoid glycosides formed the malonic acid esters undergo single esterification and acetyl esters undergo acetylation in DBT1. In contrast, the urine from DBT1-treated rats strongly resembled that of DBT2-treated rats. These metabolites originate mainly from formononetin, calycosin and their related glycosides, and they were formed mainly by the metabolic process of reduction, deglycosylation, demethylation, hydrogenation and sulfation. The

  7. HPLC-DAD-MS/MS profiling of phenolics from Securigera securidaca flowers and its anti-hyperglycemic and anti-hyperlipidemic activities

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    Rana M. Ibrahim

    Full Text Available Abstract Securigera securidaca (L. Degen & Döefl., Fabaceae, has been widely used in the Iranian, Indian and Egyptian folk medicine as antidiabetic and anti-hyperlipidemic remedy. Phenolic profiling of the ethanolic extract (90% of the flowers of S. securidaca was performed via HPLC-DAD-MS/MS analysis in the positive and negative ion modes. The total polyphenols and flavonoids in the flowers were determined colorimetrically, and the quantification of their components was carried out using HPLC-UV. Total phenolics and flavonoids estimated as gallic acid and rutin equivalents were 82.39 ± 2.79 mg/g and 48.82 ± 1.95 mg/g of the dried powdered flowers, respectively. HPLC-DAD-MS/MS analysis of the extract allowed the identification of 39 flavonoids and eight phenolic acids. Quantitative analysis of some flavonoids and phenolics (mg/100 g powdered flowers revealed the presence of isoquercetrin (3340 ± 2.1, hesperidin (32.09 ± 2.28, naringin (197.3 ± 30.16, luteolin (10.247 ± 0.594, chlorogenic acid (84.22 ± 2.08, catechin (3.94 ± 0.57 and protocatechuic acid (34.4 ± 0.15, in the extract. Moreover, the acute toxicity, hypoglycemic and hypolipidemic effects of the extract were investigated using alloxan induced diabetes in rats in a dose of 100, 200, and 400 mg/kg bwt. The ethanolic extract was safe up to a dose of 2000 mg/kg. All tested doses of the flower extract showed marked decrease in blood glucose level by 31.78%, 66.41% and 63.8% at 100, 200 and 400 mg/kg bwt, respectively, at p < 0.05. Regarding the anti-hyperlipidemic effect, a dose of 400 mg/kg of the flower extract showed the highest reduction in serum triacylglycerides and total cholesterol levels (68.46% and 51.50%, respectively at p < 0.05. The current study proved the folk use of the flowers of S. securidaca as anti-diabetic and anti-hyperlipidemic agent which could be attributed to its high phenolic content.

  8. RP-HPLC-DAD-ESI-QTOF-MS based metabolic profiling of the potential Olea europaea by-product "wood" and its comparison with leaf counterpart.

    Science.gov (United States)

    Ammar, Sonda; Contreras, Maria Del Mar; Gargouri, Boutheina; Segura-Carretero, Antonio; Bouaziz, Mohamed

    2017-05-01

    Olea europaea L. organs such as leaves, stems and roots have been associated with numerous in vivo and in vitro biological activities and used for traditional medicinal purposes. However, tree wood is an untapped resource with little information about their chemical composition. That is why, the objective of this study is to increase the knowledge about phytochemicals from 'Chemlali' olive wood by means of mass spectrometry-based analyses. Its comparison with by-products derived from leaves was also studied. Hydromethanol extracts from wood and leaves with stems of 'Chemlali' olive cultivar were analysed using reversed-phase (RP) high-performance liquid chromatography (HPLC) coupled to two detection systems: diode-array detection (DAD) and quadrupole time-of-flight (QTOF) mass spectrometry (MS) in negative ion mode. Tandem MS experiments were performed to establish the chemical structure of olive phytochemicals. A total of 85 compounds were characterised in the studied olive parts and classified as: sugars (3), organic acids (5), one phenolic aldehyde, simple phenolic acids (6), simple phenylethanoids (5), flavonoids (14), coumarins (3), caffeoyl phenylethanoid derivatives (6), iridoids (5), secoiridoids (32), and lignans (5). To our knowledge, the major part of these metabolites was not previously reported in olive tree wood, and 10 olive chemical constituents were identified for the first time in the Oleaceae family. The results presented here demonstrated the usefulness of the methodology proposed, based on RP-HPLC-DAD-ESI-QTOF-MS and MS/MS, to develop an exhaustive metabolic profiling and to recover new biologically active compounds in olive wood with pharmacologic and cosmetic potential. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  9. Phenolic Profiling of Duchesnea indica Combining Macroporous Resin Chromatography (MRC with HPLC-ESI-MS/MS and ESI-IT-MS

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    Mingzhi Zhu

    2015-12-01

    Full Text Available Duchesnea indica (D. indica is an important traditional Chinese medicine, and has long been clinically used to treat cancer in Asian countries. It has been described previously as a rich source of phenolic compounds with a broad array of diversified structures, which are the major active ingredients. However, an accurate and complete phenolic profiling has not been determined yet. In the present work, the total phenolic compounds in crude extracts from D. indica were enriched and fractionated over a macroporous resin column, then identified by HPLC-ESI-MS/MS and ESI-IT-MS (ion trap MS. A total of 27 phenolic compounds were identified in D. indica, of which 21 compounds were identified for the first time. These 27 phenolic compounds encompassing four phenolic groups, including ellagitannins, ellagic acid and ellagic acid glycosides, hydroxybenzoic acid and hydroxycinnamic acid derivatives, and flavonols, were then successfully quantified using peak areas against those of the corresponding standards with good linearity (R2 > 0.998 in the range of the tested concentrations. As a result, the contents of individual phenolic compounds varied from 6.69 mg per 100 g dry weight (DW for ellagic acid to 71.36 mg per 100 g DW for brevifolin carboxylate. Not only did this study provide the first phenolic profiling of D. indica, but both the qualitative identification and the subsequent quantitative analysis of 27 phenolic compounds from D. indica should provide a good basis for future exploration of this valuable medicinal plant.

  10. Comprehensive Quality Assessment Based Specific Chemical Profiles for Geographic and Tissue Variation in Gentiana rigescens Using HPLC and FTIR Method Combined with Principal Component Analysis

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    Jie Li

    2017-12-01

    Full Text Available Roots, stems, leaves, and flowers of Longdan (Gentiana rigescens Franch. ex Hemsl were collected from six geographic origins of Yunnan Province (n = 240 to implement the quality assessment based on contents of gentiopicroside, loganic acid, sweroside and swertiamarin and chemical profile using HPLC-DAD and FTIR method combined with principal component analysis (PCA. The content of gentiopicroside (major iridoid glycoside was the highest in G. rigescens, regardless of tissue and geographic origin. The level of swertiamarin was the lowest, even unable to be detected in samples from Kunming and Qujing. Significant correlations (p < 0.05 between gentiopicroside, loganic acid, sweroside, and swertiamarin were found at inter- or intra-tissues, which were highly depended on geographic origins, indicating the influence of environmental conditions on the conversion and transport of secondary metabolites in G. rigescens. Furthermore, samples were reasonably classified as three clusters along large producing areas where have similar climate conditions, characterized by carbohydrates, phenols, benzoates, terpenoids, aliphatic alcohols, aromatic hydrocarbons, and so forth. The present work provided global information on the chemical profile and contents of major iridoid glycosides in G. rigescens originated from six different origins, which is helpful for controlling quality of herbal medicines systematically.

  11. Profiling polyphenol composition by HPLC-DAD-ESI/MSn and the antibacterial activity of infusion preparations obtained from four medicinal plants.

    Science.gov (United States)

    Ziani, Borhane E C; Barros, Lillian; Boumehira, Ali Z; Bachari, Khaldoun; Heleno, Sandrina A; Alves, Maria Jose; Ferreira, Isabel C F R

    2018-01-24

    The infusions of Thymus pallescens Noë, Saccocalyx satureioides Coss. et Dur., Ptychotis verticillata Briq. and Limoniastrum guyonianum Boiss. have been used as medicinal remedies for many diseases in Algerian folk medicine. These species have also been well documented as rich sources of phytochemicals, such as phenolic compounds with wide diversified chemical structures, which exhibit far-ranging biological activities. Thus, the phenolic compound profile of the aqueous extracts, obtained by infusing, of the mentioned species was obtained by HPLC-DAD-ESI/MS, and their antibacterial activity was evaluated against clinical isolates. Several phenolic acids were identified and quantified, particularly caffeic acid derivatives along with glycosylated flavonoids. T. pallescens and S. satureioides contain 13 phenolic compounds, where rosmarinic acid was the most abundant phenolic acid present, while L. guyonianum presented myricetin-3-O-glucoside and myricetin-O-rhamnoside as the main compounds among the eight detected molecules. P. verticillata presented a profile of ten phenolic compounds, where 5-O-caffeoylquinic acid was the most abundant phenolic acid, followed by the flavone luteolin-3-O-glucoside. The antibacterial activity of the infusions ranged between 2.5 and 20 mg mL -1 (MIC values), and L. guyonianum showed the highest activity against all of the tested bacteria, Staphylococcus aureus and Pseudomonas aeruginosa being the most sensitive and resistant strains, respectively. Thus, the studied plant species are sources of natural antibacterial substances that can be used to fight against pathogenic microorganisms.

  12. Comprehensive quality assessment based specific chemical profiles for geographic and tissue variation in Gentiana rigescens using HPLC and FTIR method combined with principal component analysis

    Science.gov (United States)

    Li, Jie; Zhang, Ji; Zhao, Yan-Li; Huang, Heng-Yu; Wang, Yuan-Zhong

    2017-12-01

    Roots, stems, leaves and flowers of Longdan (Gentiana rigescens Franch. ex Hemsl) were collected from six geographic origins of Yunnan Province (n = 240) to implement the quality assessment based on contents of gentiopicroside, loganic acid, sweroside and swertiamarin and chemical profile using HPLC-DAD and FTIR method combined with principal component analysis (PCA). The content of gentiopicroside (major iridoid glycoside) was the highest in G. rigescens, regardless of tissue and geographic origin. The level of swertiamarin was the lowest, even unable to be detected in samples from Kunming and Qujing. Significant correlations (p < 0.05) between gentiopicroside, loganic acid, sweroside and swertiamarin were found at inter- or intra-tissues, which were highly depended on geographic origins, indicating the influence of environmental conditions on the conversion and transport of secondary metabolites in G. rigescens. Furthermore, samples were reasonably classified as three clusters along large producing areas where have similar climate conditions, characterized by carbohydrates, phenols, benzoates, terpenoids, aliphatic alcohols, aromatic hydrocarbons, and so forth. The present work provided global information on the chemical profile and contents of major iridoid glycosides in G. rigescens originated from six different origins, which is helpful for controlling quality of herbal medicines systematically.

  13. Characterization of carotenoid profiles in goldenberry (Physalis peruviana L.) fruits at various ripening stages and in different plant tissues by HPLC-DAD-APCI-MSn.

    Science.gov (United States)

    Etzbach, Lara; Pfeiffer, Anne; Weber, Fabian; Schieber, Andreas

    2018-04-15

    Carotenoid profiles of goldenberry (Physalis peruviana L.) fruits differing in ripening states and in different fruit fractions (peel, pulp, and calyx of ripe fruits) were investigated by HPLC-DAD-APCI-MS n . Out of the 53 carotenoids detected, 42 were tentatively identified. The carotenoid profile of unripe fruits is dominated by (all-E)-lutein (51%), whereas in ripe fruits, (all-E)-β-carotene (55%) and several carotenoid fatty acid esters, especially lutein esters esterified with myristic and palmitic acid as monoesters or diesters, were found. In overripe fruits, carotenoid conversion products and a higher proportion of carotenoid monoesters to diesters compared to ripe fruits were observed. Overripe fruits showed a significant decrease in total carotenoids of about 31% due to degradation. The observed conversion and degradation processes included epoxidation, isomerization, and deesterification. The peel of ripe goldenberries showed a 2.8 times higher total carotenoid content of 332.00 µg/g dw compared to the pulp. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Untargeted metabolomic profiling plasma samples of patients with lung cancer for searching significant metabolites by HPLC-MS method

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    Dementeva, N.; Ivanova, K.; Kokova, D.; Kurzina, I.; Ponomaryova, A.; Kzhyshkowska, J.

    2017-09-01

    Lung cancer is one of the most common types of cancer leading to death. Consequently, the search and the identification of the metabolites associated with the risk of developing cancer are very valuable. For the purpose, untargeted metabolic profiling of the plasma samples collected from the patients with lung cancer (n = 100) and the control group (n = 100) was conducted. After sample preparation, the plasma samples were analyzed using LC-MS method. Biostatistics methods were applied to pre-process the data for elicitation of dominating metabolites which responded to the difference between the case and the control groups. At least seven significant metabolites were evaluated and annotated. The most part of identified metabolites are connected with lipid metabolism and their combination could be useful for follow-up studies of lung cancer pathogenesis.

  15. Optimized extraction of polyphenolic antioxidant compounds from Brazil nut (Bertholletia excelsa) cake and evaluation of the polyphenol profile by HPLC.

    Science.gov (United States)

    Gomes, Suellen; Torres, Alexandre G

    2016-06-01

    The solid residue (cake) of pressed Brazil nut oil has high energy value and contains high levels of nutrients and bioactive compounds, such as polyphenols. However, little is known about these components in this by-product. Extraction is the first step in investigating the phenolic compounds in Brazil nut cake because extraction conditions might impact the yields of phenolic compounds and antioxidant capacity. The aim of this study was to select the best phenolic compound extraction conditions for Brazil nut cake by using factorial experimental design and to characterize the phenolic compounds in the extract. The optimal extraction of antioxidant phenolic compounds from Brazil nut cake was achieved under the following conditions: ethanol-water (40:60; v/v); 2.5 min homogenization; and 1 h extraction at 60 °C. The phenolic compound profile of the Brazil nut cake extract using the optimized extraction was determined by high-performance liquid chromatography with photodiode array detection. Six phenolic acids (gallic acid, protocatechuic acid, 2,4-dihydroxybenzoic acid, p-hydroxybenzoic acid, p-coumaric acid and sinapic acid) and one flavonoid ((+)-catechin) were identified, and the contents of the phenolic compounds varied from 70.0 to 421 mg kg(-1) . Knowledge of the potential bioactivity of Brazil nut cake identified in the present study might promote its use in the food industry. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

  16. Profiling of dehydropyrrolizidine alkaloids and their N-oxides in herbarium-preserved specimens of amsinckia species using HPLC-esi(+)MS.

    Science.gov (United States)

    Colegate, Steven M; Welsh, Stanley L; Gardner, Dale R; Betz, Joseph M; Panter, Kip E

    2014-07-30

    Species of the Amsinckia genus (Boraginaceae) are known to produce potentially hepato-, pneumo-, and/or genotoxic dehydropyrrolizidine alkaloids. However, the taxonomic differentiation of Amsinckia species can be very subtle and there seems to be marked differences in toxicity toward grazing livestock. Methanol extracts of mass-limited leaf samples from herbarium specimens (collected from 1899 to 2013) of 10 Amsinckia species and one variety were analyzed using HPLC-esi(+)MS and MS/MS for the presence of potentially toxic dehydropyrrolizidine alkaloids and/or their N-oxides. Dehydropyrrolizidine alkaloids were detected in all specimens examined ranging from about 1 to 4000 μg/g of plant. Usually occurring mainly as their N-oxides, the predominant alkaloids were the epimeric lycopsamine and intermedine. Also sometimes observed in higher concentrations were the 3'- and 7-acetyl derivatives of lycopsamine/intermedine and their N-oxides. Within a designated species, an inconsistent profile was often observed that may be due to natural variation, taxonomic misassignment, or nonuniform degradation due to plant collection and storage differences.

  17. High-Resolution Inhibition Profiling Combined with HPLC-HRMS-SPE-NMR for Identification of PTP1B Inhibitors from Vietnamese Plants.

    Science.gov (United States)

    Trinh, Binh Thi Dieu; Jäger, Anna K; Staerk, Dan

    2017-07-20

    Protein tyrosine phosphatase 1B (PTP1B) plays a key role as a negative regulator in insulin signal transduction by deactivating the insulin receptor. Thus, PTP1B inhibition has emerged as a potential therapeutic strategy for curing insulin resistance. In this study, 40 extracts from 18 different plant species were investigated for PTP1B inhibitory activity in vitro. The most promising one, the EtOAc extract of Ficus racemosa , was investigated by high-resolution PTP1B inhibition profiling combined with HPLC-HRMS-SPE-NMR analysis. This led to the identification of isoderrone ( 1 ), derrone ( 2 ), alpinumisoflavone ( 3 ) and mucusisoflavone B ( 4 ) as PTP1B inhibitors. IC 50 of these compounds were 22.7 ± 1.7, 12.6 ± 1.6, 21.2 ± 3.8 and 2.5 ± 0.2 µM, respectively. Kinetics analysis revealed that these compounds inhibited PTP1B non-competitively with K i values of 21.3 ± 2.8, 7.9 ± 1.9, 14.3 ± 2.0, and 3.0 ± 0.5 µM, respectively. These findings support the important role of F. racemosa as a novel source of new drugs and/or as a herbal remedy for treatment of type 2 diabetes.

  18. High-Resolution Inhibition Profiling Combined with HPLC-HRMS-SPE-NMR for Identification of PTP1B Inhibitors from Vietnamese Plants

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    Binh Thi Dieu Trinh

    2017-07-01

    Full Text Available Protein tyrosine phosphatase 1B (PTP1B plays a key role as a negative regulator in insulin signal transduction by deactivating the insulin receptor. Thus, PTP1B inhibition has emerged as a potential therapeutic strategy for curing insulin resistance. In this study, 40 extracts from 18 different plant species were investigated for PTP1B inhibitory activity in vitro. The most promising one, the EtOAc extract of Ficus racemosa, was investigated by high-resolution PTP1B inhibition profiling combined with HPLC-HRMS-SPE-NMR analysis. This led to the identification of isoderrone (1, derrone (2, alpinumisoflavone (3 and mucusisoflavone B (4 as PTP1B inhibitors. IC50 of these compounds were 22.7 ± 1.7, 12.6 ± 1.6, 21.2 ± 3.8 and 2.5 ± 0.2 µM, respectively. Kinetics analysis revealed that these compounds inhibited PTP1B non-competitively with Ki values of 21.3 ± 2.8, 7.9 ± 1.9, 14.3 ± 2.0, and 3.0 ± 0.5 µM, respectively. These findings support the important role of F. racemosa as a novel source of new drugs and/or as a herbal remedy for treatment of type 2 diabetes.

  19. HPLC-DAD-MS Profiling of Polyphenols Responsible for the Yellow-Orange Color in Apple Juices of Different French Cider Apple Varieties.

    Science.gov (United States)

    Le Deun, Erell; Van der Werf, Remmelt; Le Bail, Gildas; Le Quéré, Jean-Michel; Guyot, Sylvain

    2015-09-09

    The pigments responsible for the yellow-orange coloration of apple juices have remained largely unknown up to now. Four French cider apple juices were produced in conditions similar to those used in the cider-making industry. The oxidized juices, characterized using the CIE L a b parameters, displayed various colors depending on the apple variety and native phenolic composition. HPLC-DAD-MS revealed contrasting pigment profiles related to oxidized tanning and nontanning molecules. The latter were divided into two groups according to their polarity and their visible spectra. With regard to phenolic classes, flavanol monomers and hydroxycinnamic acids played an essential role in the formation of oxidation products. Interestingly, dihydrochalcones appeared to include precursors of some yellow compounds. Indeed, the yellow pigment phloretin xyloglucoside oxidation product (PXGOPj), derived from phloretin xyloglucoside, was clearly identified in apple juices as a xyloglucose analogue of the yellow pigment phloridzin oxidation product (POPj), previously characterized in a model solution by Le Guernevé et al. (Tetrahedron Lett. 2004, 45 (35), 6673-6677).

  20. Metabolic profiling study on potential toxicity and immunotoxicity-biomarker discovery in rats treated with cyclophosphamide using HPLC-ESI-IT-TOF-MS.

    Science.gov (United States)

    Li, Jing; Lin, Wensi; Lin, Weiwei; Xu, Peng; Zhang, Jianmei; Yang, Haisong; Ling, Xiaomei

    2015-05-01

    Despite the recent advances in understanding toxicity mechanism of cyclophosphamide (CTX), the development of biomarkers is still essential. CTX-induced immunotoxicity in rats by a metabonomics approach was investigated using high-performance liquid chromatography coupled with ion trap time-of-flight mass spectrometry (HPLC-ESI-IT-TOF-MS). The rats were orally administered CTX (30 mg/kg/day) for five consecutive days, and on the fifth day samples of urine, thymus and spleen were collected and analyzed. A significant difference in metabolic profiling was observed between the CTX-treated group and the control group by partial least squares-discriminant analysis (PLS-DA), which indicated that metabolic disturbances of immunotoxicity in CTX-treated rats had occurred. One potential biomarker in spleen, three in urine and three in thymus were identified. It is suggested that the CTX-toxicity mechanism may involve the modulation of tryptophan metabolism, phospholipid metabolism and energy metabolism. This research can help to elucidate the CTX-influenced pathways at a low dose and can further help to indicate the patients' pathological status at earlier stages of toxicological progression after drug administration. Copyright © 2014 John Wiley & Sons, Ltd.

  1. High-resolution bioactivity profiling combined with HPLC-HRMS-SPE-NMR: α-Glucosidase inhibitors and acetylated ellagic acid rhamnosides from Myrcia palustris DC. (Myrtaceae).

    Science.gov (United States)

    Wubshet, Sileshi G; Moresco, Henrique H; Tahtah, Yousof; Brighente, Inês M C; Staerk, Dan

    2015-08-01

    Type 2 diabetes (T2D) is an endocrine metabolic disease with a worldwide prevalence of more than 8%, and an expected increase close to 50% in the next 15-20years. T2D is associated with severe and life-threatening complications like retinopathy, neuropathy, nephropathy, and cardiovascular diseases, and therefore improved drug leads or functional foods containing α-glucosidase inhibitors are needed for management of blood glucose. In this study, leaves of Myrcia palustris were investigated by high-resolution α-glucosidase inhibition profiling combined with HPLC-HRMS-SPE-NMR. This led to identification of casuarinin, myricetin 3-O-β-d-(6″-galloyl)galactopyranoside, kaempferol 3-O-β-d-galactopyranoside, myricetin, and quercetin as α-glucosidase inhibitors. In addition, four acetylated ellagic acid rhamnosides, i.e., 4-O-(2″,4″-O-diacetyl-α-l-rhamnopyranosyl)ellagic acid, 4-O-(2″,3″-O-diacetyl-α-l-rhamnopyranosyl)ellagic acid, 4-O-(3″,4″-O-diacetyl-α-l-rhamnopyranosyl)ellagic acid, and 4-O-(2″,3″,4″-O-triacetyl-α-l-rhamnopyranosyl)ellagic acid were identified. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Morphology and composition of gold in a lateritic profile, Fazenda Pison “Garimpo”, Amazon, Brazil

    Science.gov (United States)

    Larizzatti, J. H.; Oliveira, S. M. B.; Butt, C. R. M.

    2008-05-01

    This study describes the morphological evolution of gold grains in a lateritic weathering profile in an equatorial rainforest climate. Primary sources of gold are quartz veins associated with shallow granophyric intrusion. Gold grains were found in fresh ore, saprolite, transition zones, ferruginous duricrust, red latosol, and yellow latosol. Irregularly shaped grains predominate, with smaller proportions of dendritic and prismatic forms. Gold grains are weathered in the uppermost 10 m of the regolith. Mean gold grain size is maximum in the duricrust (>125 μm) and decreases progressively upward into the yellow latosol (duricrust formation may preserve some grains as large aggregates, but subsequent transformation into latosol further modifies them.

  3. Comparison of total phenolic content, scavenging activity and HPLC-ESI-MS/MS profiles of both young and mature leaves and stems of Andrographis paniculata.

    Science.gov (United States)

    Chua, Lee Suan; Yap, Ken Choy; Jaganath, Indu Bala

    2013-12-01

    The total phenolic content and radical scavenging activity of Andrographis paniculata has been investigated to estimate the amount of phenolic compounds and diterpene lactones, respectively in the plant extracts. The stem extracts exhibited higher total phenolic content and scavenging activity than those of the leaf extracts from both young and mature plants. A range of 19.6-47.8 mg extract of A. paniculata from different parts of the plant is equivalent to the scavenging activity exhibited by one mg of standard Trolox. HPLC-ESI-MS/MS was also used to identify simultaneously the phytochemicals from the leaves and stems of both young and mature plant samples. Of the identified compounds, seven of the sixteen diterpene lactones, three of the six flavonoids, five of the six phenolic acids and two cyclic acids are reported here for the first time for this species. Multivariate statistical approaches such as Hierarchiral Component Analysis (HCA) and Principle Component Analysis (PCA) have clustered the plant extracts into the leaf and stem groups, regardless of plant age. Further classification based on the phytochemical profiles revealed that mostly phenolic acids and flavonoids were from the young leaf extracts, and diterpenoids and their glycosides from the mature leaf extracts. However, the phytochemical profiles for the stems of both young and mature plants were not significantly different as presented in the dendrogram of HCA and the score plot of PCA. The marker for mature plants might be the m/z 557 ion (dihydroxyl dimethyl 19-[(beta-D-glucopyranosyl)oxy]-19-oxo-ent-labda-8(17),13-dien-16,15-olide), whereas the m/z 521 ion (propyl neoandrographolide) could be the marker for leaf extracts.

  4. Profiling of tryptophan-related plasma indoles in patients with carcinoid tumors by automated, on-line, solid-phase extraction and HPLC with fluorescence detection.

    Science.gov (United States)

    Kema, I P; Meijer, W G; Meiborg, G; Ooms, B; Willemse, P H; de Vries, E G

    2001-10-01

    Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing matrices as well as the plasma indole concentrations in healthy controls and patients with carcinoid tumors. Plasma, cerebrospinal fluid, and tissue homogenates were prepurified by automated on-line solid-phase extraction (SPE) in Hysphere Resin SH SPE cartridges containing strong hydrophobic polystyrene resin. Analytes were eluted from the SPE cartridge by column switching. Subsequent separation and detection were performed by reversed-phase HPLC combined with fluorometric detection in a total cycle time of 20 min. We obtained samples from 14 healthy controls and 17 patients with metastasized midgut carcinoid tumors for plasma indole analysis. In the patient group, urinary excretion of 5-HIAA and serotonin was compared with concentrations of plasma indoles. Within- and between-series CVs for indoles in platelet-rich plasma were 0.6-6.2% and 3.7-12%, respectively. Results for platelet-rich plasma serotonin compared favorably with those obtained by single-component analysis. Plasma 5-HIAA, but not 5-HTP was detectable in 8 of 17 patients with carcinoid tumors. In the patient group, platelet-rich plasma total tryptophan correlated negatively with platelet-rich plasma serotonin (P = 0.021; r = -0.56), urinary 5-HIAA (P = 0.003; r = -0.68), and urinary serotonin (P manual, single-component analyses.

  5. Two Ganoderma species: profiling of phenolic compounds by HPLC-DAD, antioxidant, antimicrobial and inhibitory activities on key enzymes linked to diabetes mellitus, Alzheimer's disease and skin disorders.

    Science.gov (United States)

    Zengin, Gokhan; Sarikurkcu, Cengiz; Gunes, Erdogan; Uysal, Ahmet; Ceylan, Ramazan; Uysal, Sengul; Gungor, Halil; Aktumsek, Abdurrahman

    2015-08-01

    This work reports the antioxidant, antimicrobial, and inhibitory effects of methanol and water extracts from Ganoderma applanatum (GAM: methanol extract and GAW: water extract) and G. resinaceum (GRM: methanol extract and GRW: water extract) against cholinesterase, tyrosinase, α-amylase and α-glucosidase. The total phenolics, flavonoids contents, and HPLC profile of phenolic components present in the extracts, were also determined. Antioxidant activities were investigated by using different assays, including DPPH, ABTS, FRAP, CUPRAC, phosphomolybdenum and metal chelating assays. Antimicrobial activity of the tested Ganoderma extracts was also studied by the broth microdilution method. Generally, the highest antioxidant (59.24 mg TEs per g extract for DPPH, 41.32 mg TEs per g extract for ABTS, 41.35 mg TEs per g extract for CUPRAC, 49.68 mg TEs per g extract for FRAP, 130.57 mg AAEs per g extract for phosphomolybdenum and 26.92 mg EDTAEs per g extract) and enzyme inhibitory effects (1.47 mg GALAEs per g extract for AChE, 1.51 mg GALAEs per g extract for BChE, 13.40 mg KAEs per g extract for tyrosinase, 1.13 mmol ACEs per g extract for α-amylase and 2.20 mmol ACEs per g extract for α-glucosidase) were observed in GRM, which had the highest concentrations of phenolics (37.32 mg GAEs g(-1) extract). Again, Ganoderma extracts possess weak antibacterial and antifungal activities. Apigenin and protocatechuic acid were determined as the main components in GRM (1761 μg per g extract) and GAM (165 μg per g extract), respectively. The results suggest that the Ganoderma species may be considered as a candidate for preparing new food supplements and can represent a good model for the development of new drug formulations.

  6. Cytokines profile and peripheral blood mononuclear cells morphology in Rett and autistic patients.

    Science.gov (United States)

    Pecorelli, Alessandra; Cervellati, Franco; Belmonte, Giuseppe; Montagner, Giulia; Waldon, PhiAnh; Hayek, Joussef; Gambari, Roberto; Valacchi, Giuseppe

    2016-01-01

    A potential role for immune dysfunction in autism spectrum disorders (ASD) has been well established. However, immunological features of Rett syndrome (RTT), a genetic neurodevelopmental disorder closely related to autism, have not been well addressed yet. By using multiplex Luminex technology, a panel of 27 cytokines and chemokines was evaluated in serum from 10 RTT patients with confirmed diagnosis of MECP2 mutation (typical RTT), 12 children affected by classic autistic disorder and 8 control subjects. The cytokine/chemokine gene expression was assessed by real time PCR on mRNA of isolated peripheral blood mononuclear cells (PBMCs). Moreover, ultrastructural analysis of PBMCs was performed using transmission electron microscopy (TEM). Significantly higher serum levels of interleukin-8 (IL-8), IL-9, IL-13 were detected in RTT compared to control subjects, and IL-15 shows a trend toward the upregulation in RTT. In addition, IL-1β and VEGF were the only down-regulated cytokines in autistic patients with respect to RTT. No difference in cytokine/chemokine profile between autistic and control groups was detected. These data were also confirmed by ELISA real time PCR. At the ultrastructural level, the most severe morphological abnormalities were observed in mitochondria of both RTT and autistic PBMCs. In conclusion, our study shows a deregulated cytokine/chemokine profile together with morphologically altered immune cells in RTT. Such abnormalities were not quite as evident in autistic subjects. These findings indicate a possible role of immune dysfunction in RTT making the clinical features of this pathology related also to the immunology aspects, suggesting, therefore, novel possible therapeutic interventions for this disorder. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Proteome profile of functional mitochondria from human skeletal muscle using one-dimensional gel electrophoresis and HPLC-ESI-MS/MS

    DEFF Research Database (Denmark)

    Lefort, Natalie; Yi, Zhengping; Bowen, Benjamin

    2009-01-01

    were functional as evidenced by their response to carbohydrate and fat-derived fuels. Using one-dimensional gel electrophoresis and HPLC-ESI-MS/MS, 823 unique proteins were detected, and 487 of these were assigned to the mitochondrion, including the newly characterized SIRT5, MitoNEET and RDH13...

  8. The morphologies of breast cancer cell lines in three-dimensionalassays correlate with their profiles of gene expression

    Energy Technology Data Exchange (ETDEWEB)

    Kenny, Paraic A.; Lee, Genee Y.; Myers, Connie A.; Neve, RichardM.; Semeiks, Jeremy R.; Spellman, Paul T.; Lorenz, Katrin; Lee, Eva H.; Barcellos-Hoff, Mary Helen; Petersen, Ole W.; Gray, Joe W.; Bissell, MinaJ.

    2007-01-31

    3D cell cultures are rapidly becoming the method of choice for the physiologically relevant modeling of many aspects of non-malignant and malignant cell behavior ex vivo. Nevertheless, only a limited number of distinct cell types have been evaluated in this assay to date. Here we report the first large scale comparison of the transcriptional profiles and 3D cell culture phenotypes of a substantial panel of human breast cancer cell lines. Each cell line adopts a colony morphology of one of four main classes in 3D culture. These morphologies reflect, at least in part, the underlying gene expression profile and protein expression patterns of the cell lines, and distinct morphologies were also associated with tumor cell invasiveness and with cell lines originating from metastases. We further demonstrate that consistent differences in genes encoding signal transduction proteins emerge when even tumor cells are cultured in 3D microenvironments.

  9. Cell Painting, a high-content image-based assay for morphological profiling using multiplexed fluorescent dyes

    Science.gov (United States)

    Bray, Mark-Anthony; Singh, Shantanu; Han, Han; Davis, Chadwick T.; Borgeson, Blake; Hartland, Cathy; Kost-Alimova, Maria; Gustafsdottir, Sigrun M.; Gibson, Christopher C.; Carpenter, Anne E.

    2016-01-01

    In morphological profiling, quantitative data are extracted from microscopy images of cells to identify biologically relevant similarities and differences among samples based on these profiles. This protocol describes the design and execution of experiments using Cell Painting, a morphological profiling assay multiplexing six fluorescent dyes imaged in five channels, to reveal eight broadly relevant cellular components or organelles. Cells are plated in multi-well plates, perturbed with the treatments to be tested, stained, fixed, and imaged on a high-throughput microscope. Then, automated image analysis software identifies individual cells and measures ~1,500 morphological features (various measures of size, shape, texture, intensity, etc.) to produce a rich profile suitable for detecting subtle phenotypes. Profiles of cell populations treated with different experimental perturbations can be compared to suit many goals, such as identifying the phenotypic impact of chemical or genetic perturbations, grouping compounds and/or genes into functional pathways, and identifying signatures of disease. Cell culture and image acquisition takes two weeks; feature extraction and data analysis take an additional 1-2 weeks. PMID:27560178

  10. Morphological, Physiological and Skating Performance Profiles of Male Age-Group Elite Ice Hockey Players.

    Science.gov (United States)

    Allisse, Maxime; Sercia, Pierre; Comtois, Alain-Steve; Leone, Mario

    2017-09-01

    The purpose of this study was to describe the evolution of morphological, physiological and skating performance profiles of elite age-group ice hockey players based on repeated measures spread over one season. In addition, the results of fitness tests and training programs performed in off-ice conditions and their relationship with skating performance were analyzed. Eighteen high level age-group ice hockey players (13.1 ± 0.6 years) were assessed off and on-ice at the beginning and at the end of the hockey season. A third evaluation was also conducted at the beginning of the following hockey season. The players were taller, heavier, and showed bone breadths and muscle girths above the reference population of the same age. Muscular variables improved significantly during and between the two hockey seasons (p skating performance tests exhibited significant enhancements during the hockey season, but not during the off-season where some degradation was observed. Finally, weak observed variances (generally skating performance tests indicated important gaps, both in the choice of the off-ice assessment tools as well as in training methods conventionally used. The reflection on the best way to assess and train hockey players certainly deserves to be continued.

  11. Morphological, Physiological and Skating Performance Profiles of Male Age-Group Elite Ice Hockey Players

    Directory of Open Access Journals (Sweden)

    Allisse Maxime

    2017-08-01

    Full Text Available The purpose of this study was to describe the evolution of morphological, physiological and skating performance profiles of elite age-group ice hockey players based on repeated measures spread over one season. In addition, the results of fitness tests and training programs performed in off-ice conditions and their relationship with skating performance were analyzed. Eighteen high level age-group ice hockey players (13.1 ± 0.6 years were assessed off and on-ice at the beginning and at the end of the hockey season. A third evaluation was also conducted at the beginning of the following hockey season. The players were taller, heavier, and showed bone breadths and muscle girths above the reference population of the same age. Muscular variables improved significantly during and between the two hockey seasons (p < 0.05. However, maximal aerobic power improved only during the off-season. All skating performance tests exhibited significant enhancements during the hockey season, but not during the off-season where some degradation was observed. Finally, weak observed variances (generally <20% of the explained variance between physiological variables measured off-ice and on-ice skating performance tests indicated important gaps, both in the choice of the off-ice assessment tools as well as in training methods conventionally used. The reflection on the best way to assess and train hockey players certainly deserves to be continued.

  12. PARALLEL IMPLEMENTATION OF MORPHOLOGICAL PROFILE BASED SPECTRAL-SPATIAL CLASSIFICATION SCHEME FOR HYPERSPECTRAL IMAGERY

    Directory of Open Access Journals (Sweden)

    B. Kumar

    2016-06-01

    Full Text Available Extended morphological profile (EMP is a good technique for extracting spectral-spatial information from the images but large size of hyperspectral images is an important concern for creating EMPs. However, with the availability of modern multi-core processors and commodity parallel processing systems like graphics processing units (GPUs at desktop level, parallel computing provides a viable option to significantly accelerate execution of such computations. In this paper, parallel implementation of an EMP based spectralspatial classification method for hyperspectral imagery is presented. The parallel implementation is done both on multi-core CPU and GPU. The impact of parallelization on speed up and classification accuracy is analyzed. For GPU, the implementation is done in compute unified device architecture (CUDA C. The experiments are carried out on two well-known hyperspectral images. It is observed from the experimental results that GPU implementation provides a speed up of about 7 times, while parallel implementation on multi-core CPU resulted in speed up of about 3 times. It is also observed that parallel implementation has no adverse impact on the classification accuracy.

  13. REST-FRAME UV VERSUS OPTICAL MORPHOLOGIES OF GALAXIES USING SERSIC PROFILE FITTING: THE IMPORTANCE OF MORPHOLOGICAL K-CORRECTION

    International Nuclear Information System (INIS)

    Rawat, Abhishek; Wadadekar, Yogesh; De Mello, Duilia

    2009-01-01

    We show a comparison of the rest-frame UV morphologies of a sample of 162 intermediate-redshift (z median = 1.02) galaxies with their rest-frame optical morphologies. We select our sample from the deepest near-UV image obtained with the Hubble Space Telescope (HST) using the Wide Field Planetary Camera 2 (WFPC2; F300W) as part of the parallel observations of the Hubble Ultra Deep Field campaign overlapping with the HST/ACS Great Observatories Origins Deep Survey data set. We perform single-component Sersic fits in both WFPC2/F300W (rest-frame UV) and ACS/F850LP (rest-frame optical) bands and deduce that the Sersic index n is estimated to be smaller in the rest-frame UV compared to the rest-frame optical, leading to an overestimation of the number of merger candidates by ∼40%-100% compared to the rest-frame optical depending upon the cutoff in n employed for identifying merger candidates. This effect seems to be dominated by galaxies with low values of n(F300W) ≤ 0.5 that have a value of n(F850LP) ∼ 1.0. We argue that these objects are probably clumpy star-forming galaxies or minor mergers, both of which are essentially contaminants, if one is interested in identifying major mergers. In addition, we also find evidence that the axis ratio b/a is lower, i.e., ellipticity (1 - b/a) is higher in rest-frame UV compared to the rest-frame optical. Moreover, we find that in the rest-frame UV, the number of high ellipticity (e ≥ 0.8) objects are higher by a factor of ∼2.8 compared to the rest-frame optical. This indicates that the reported dominance of elongated morphologies among high-z Lyman Break Galaxies might just be a bias related to the use of rest-frame UV data sets in high-z studies.

  14. Profiling of adrenocorticotropic hormone and arginine vasopressin in human pituitary gland and tumor thin tissue sections using droplet-based liquid-microjunction surface-sampling-HPLC-ESI-MS-MS.

    Science.gov (United States)

    Kertesz, Vilmos; Calligaris, David; Feldman, Daniel R; Changelian, Armen; Laws, Edward R; Santagata, Sandro; Agar, Nathalie Y R; Van Berkel, Gary J

    2015-08-01

    Described here are the results from the profiling of the proteins arginine vasopressin (AVP) and adrenocorticotropic hormone (ACTH) from normal human pituitary gland and pituitary adenoma tissue sections, using a fully automated droplet-based liquid-microjunction surface-sampling-HPLC-ESI-MS-MS system for spatially resolved sampling, HPLC separation, and mass spectrometric detection. Excellent correlation was found between the protein distribution data obtained with this method and data obtained with matrix-assisted laser desorption/ionization (MALDI) chemical imaging analyses of serial sections of the same tissue. The protein distributions correlated with the visible anatomic pattern of the pituitary gland. AVP was most abundant in the posterior pituitary gland region (neurohypophysis), and ATCH was dominant in the anterior pituitary gland region (adenohypophysis). The relative amounts of AVP and ACTH sampled from a series of ACTH-secreting and non-secreting pituitary adenomas correlated with histopathological evaluation. ACTH was readily detected at significantly higher levels in regions of ACTH-secreting adenomas and in normal anterior adenohypophysis compared with non-secreting adenoma and neurohypophysis. AVP was mostly detected in normal neurohypophysis, as expected. This work reveals that a fully automated droplet-based liquid-microjunction surface-sampling system coupled to HPLC-ESI-MS-MS can be readily used for spatially resolved sampling, separation, detection, and semi-quantitation of physiologically-relevant peptide and protein hormones, including AVP and ACTH, directly from human tissue. In addition, the relative simplicity, rapidity, and specificity of this method support the potential of this basic technology, with further advancement, for assisting surgical decision-making. Graphical Abstract Mass spectrometry based profiling of hormones in human pituitary gland and tumor thin tissue sections.

  15. Antioxidant Properties and Hyphenated HPLC-PDA-MS Profiling of Chilean Pica Mango Fruits (Mangifera indica L. Cv. piqueño

    Directory of Open Access Journals (Sweden)

    Javier E. Ramirez

    2013-12-01

    Full Text Available Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu, 13 in Pica peel (ppe 11 in Tommy Atkins pulp (tpu and 12 in Tommy Atkins peel (tpe. Three procyanidin dimers (peaks 6, 9 and 10, seven acid derivatives (peaks 1–4, 11, 20 and 21 and four xanthones were identified, mainly mangiferin (peak 12 and mangiferin gallate, (peak 7, which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13 was also present in both fruit pulps and dimethylmangiferin (peak 14 was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively. The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  16. Antioxidant properties and hyphenated HPLC-PDA-MS profiling of Chilean Pica mango fruits (Mangifera indica L. Cv. piqueño).

    Science.gov (United States)

    Ramirez, Javier E; Zambrano, Ricardo; Sepúlveda, Beatriz; Simirgiotis, Mario J

    2013-12-31

    Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu), 13 in Pica peel (ppe) 11 in Tommy Atkins pulp (tpu) and 12 in Tommy Atkins peel (tpe). Three procyanidin dimers (peaks 6, 9 and 10), seven acid derivatives (peaks 1-4, 11, 20 and 21) and four xanthones were identified, mainly mangiferin (peak 12) and mangiferin gallate, (peak 7), which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13) was also present in both fruit pulps and dimethylmangiferin (peak 14) was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively) than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively). The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW) measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  17. Morphological characterization and gene expression profiling during bud development in a tropical perennial, Litchi chinensis Sonn.

    Directory of Open Access Journals (Sweden)

    Huifeng Zhang

    2016-10-01

    Full Text Available Tropical evergreen perennials undergo recurrent flush growth, and their terminal buds alternate between growth and dormancy. In sharp contrast to intensive studies on bud development in temperate deciduous trees, there is little information about bud development regulation in tropical trees. In this study, litchi (Litchi chinensis Sonn. was used as a model tropical perennial for morphological characterization and transcriptomic analysis of bud development. Litchi buds are naked with apical meristem embraced by rudimentary leaves, which are brown at dormant stage (Stage I. They swell and turn greenish as buds break (Stage II, and as growth accelerates, the rudimentary leaves elongate and open exposing the inner leaf primodia. With the outgrowth of the needle-like leaflets, bud growth reaches a maximum (Stage III. When leaflets expand, bud growth cease with the abortion of the rudimentary leaves at upper positions (Stage IV. Then buds turn brown and reenter dormant status. Budbreak occurs again when new leaves become hard green. Buds at four stages (Stage I to IV were collected for respiration measurements and in-depth RNA sequencing. Respiration rate was lowest at Stage I and highest at Stage II, decreasing towards growth cessation. RNA sequencing obtained over 5 Gb data from each of the bud samples and de novo assembly generated a total of 59999 unigenes, 40119 of which were annotated. Pair-wise comparison of gene expression between stages, gene profiling across stages, GO/KEGG enrichment analysis, and the expression patterns of 17 major genes highlighted by principal component (PC analysis displayed significant changes in stress resistance, hormone signal pathways, circadian rhythm, photosynthesis, cell division, carbohydrate metabolism, programmed cell death during bud development, which might be under epigenetic control involving chromatin methylation. The qPCR results of 8 selected unigenes with high PC scores agreed with the RPKM values

  18. Time-kill profiles and cell-surface morphological effects of crude ...

    African Journals Online (AJOL)

    MK1201 mycelial extract on the viability and cell surface morphology of methicillin-susceptible Staphylococcus aureus (MSSA) and methicillin-resistant Staphylococcus aureus (MRSA). Methods: Time-kill assays were conducted by incubating test ...

  19. Identification of PTP1B and α-Glucosidase Inhibitory Serrulatanes from Eremophila spp. by Combined use of Dual High-Resolution PTP1B and α-Glucosidase Inhibition Profiling and HPLC-HRMS-SPE-NMR.

    Science.gov (United States)

    Wubshet, Sileshi G; Tahtah, Yousof; Heskes, Allison M; Kongstad, Kenneth T; Pateraki, Irini; Hamberger, Björn; Møller, Birger L; Staerk, Dan

    2016-04-22

    According to the International Diabetes Federation, type 2 diabetes (T2D) has reached epidemic proportions, affecting more than 382 million people worldwide. Inhibition of protein tyrosine phosphatase-1B (PTP1B) and α-glucosidase is a recognized therapeutic approach for management of T2D and its associated complications. The lack of clinical drugs targeting PTP1B and side effects of the existing α-glucosidase drugs, emphasize the need for new drug leads for these T2D targets. In the present work, dual high-resolution PTP1B and α-glucosidase inhibition profiles of Eremophila gibbosa, E. glabra, and E. aff. drummondii "Kalgoorlie" were used for pinpointing α-glucosidase and/or PTP1B inhibitory constituents directly from the crude extracts. A subsequent targeted high-performance liquid chromatography-high-resolution mass spectrometry-solid-phase extraction-nuclear magnetic resonance spectroscopy (HPLC-HRMS-SPE-NMR) analysis and preparative-scale HPLC isolation led to identification of 21 metabolites from the three species, of which 16 were serrulatane-type diterpenoids (12 new) associated with either α-glucosidase and/or PTP1B inhibition. This is the first report of serrulatane-type diterpenoids as potential α-glucosidase and/or PTP1B inhibitors.

  20. Edible seaweed as future functional food: Identification of α-glucosidase inhibitors by combined use of high-resolution α-glucosidase inhibition profiling and HPLC-HRMS-SPE-NMR.

    Science.gov (United States)

    Liu, Bingrui; Kongstad, Kenneth T; Wiese, Stefanie; Jäger, Anna K; Staerk, Dan

    2016-07-15

    Crude chloroform, ethanol and acetone extracts of nineteen seaweed species were screened for their antioxidant and α-glucosidase inhibitory activity. Samples showing more than 60% α-glucosidase inhibitory activity, at a concentration of 1 mg/ml, were furthermore investigated using high-resolution α-glucosidase inhibition profiling combined with high-performance liquid chromatography-high-resolution mass spectrometry-solid-phase extraction-nuclear magnetic resonance spectroscopy (HR-bioassay/HPLC-HRMS-SPE-NMR). The results showed Ascophyllum nodosum and Fucus vesicolosus to be rich in antioxidants, equaling a Trolox equivalent antioxidant capacity of 135 and 108 mM Troloxmg(-1) extract, respectively. HR-bioassay/HPLC-HRMS-SPE-NMR showed the α-glucosidase inhibitory activity of A. nodosum, F. vesoculosus, Laminaria digitata, Laminaria japonica and Undaria pinnatifida to be caused by phlorotannins as well as fatty acids - with oleic acid, linoleic acid and eicosapentaenoic acid being the most potent with IC50 values of 0.069, 0.075 and 0.10 mM, respectively, and showing a mixed-type inhibition mode. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Jackfruit (Artocarpus heterophyllus Lam.) peel: A better source of antioxidants and a-glucosidase inhibitors than pulp, flake and seed, and phytochemical profile by HPLC-QTOF-MS/MS.

    Science.gov (United States)

    Zhang, Lu; Tu, Zong-Cai; Xie, Xing; Wang, Hui; Wang, Hao; Wang, Zhen-Xing; Sha, Xiao-Mei; Lu, Yu

    2017-11-01

    Jackfruit (Artocarpus heterophyllus Lam.) peel is an underutilized by-product in both, the production and processing of jackfruit. This research compared the antioxidant and hypoglycemic potential of jackfruit peel with jackfruit pulp, flake and seed for the first time. The phytochemical profile of peel extract was characterized with HPLC-QTOF-MS/MS. Results revealed that peel extract exhibited the highest total phenolic and total flavonoid content, and the phenolics was 4.65, 4.12 and 4.95 times higher than that of pulp, flake and seed extract, respectively. The strongest DPPH and ABTS + scavenging ability, α-glucosidase inhibition were also found in peel extract, and the α-glucosidase inhibition was about 11.8-fold of that of acarbose. The HPLC-QTOF-MS/MS analysis led to the tentative identification of 53 compounds, prenylflavonoids, hydroxycinnamic acids and glycosides are the predominant bioactive compounds. Above results reveal promising potential of jackfruit peel as a new source of natural antioxidants and hypoglycemic agents. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Profiling of tryptophan-related plasma indoles in patients with carcinoid tumors by automated, on-line, solid-phase extraction and HPLC with fluorescence detection

    NARCIS (Netherlands)

    Kema, IP; Meijer, WG; Meiborg, G; Ooms, B; Willemse, PHB; de Vries, EGE

    2001-01-01

    Background: Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing

  3. Differentiation of Alternaria infectoria and Alternaria alternata based on morphology, metabolite profiles, and cultural characteristics

    DEFF Research Database (Denmark)

    Andersen, Birgitte; Thrane, Ulf

    1996-01-01

    Some small-spored species belonging to the genus Alternaria Nees have been studied according to their chemical, morphological, and cultural characteristics. A data matrix was constructed based on a combination of characters. Cluster analysis of the combined data set showed good resolution of two...

  4. The salivary proteome profile in patients affected by SAPHO syndrome characterized by a top-down RP-HPLC-ESI-MS platform.

    Science.gov (United States)

    Sanna, Monica; Firinu, Davide; Manconi, Paolo Emilio; Pisanu, Maria; Murgia, Giuseppe; Piras, Valentina; Castagnola, Massimo; Messana, Irene; del Giacco, Stefano Renato; Cabras, Tiziana

    2015-06-01

    SAPHO syndrome is a rare and often unrecognized disease with prominent inflammatory cutaneous and articular symptoms characterized by musculoskeletal manifestations (synovitis, hyperostosis, osteomyelitis) associated with dermatological conditions (severe acne and pustulosis). The acidic soluble fraction of whole saliva from 10 adult women affected by SAPHO syndrome and from a group of 28 healthy women was analysed by RP-HPLC-ESI-MS with the aim of discovering salivary biomarkers of the disorder. The levels of the oral proteins and peptides were correlated with clinical data. The following proteins showed a significant decreased concentration in saliva of SAPHO subjects with respect to controls: cystatin S1 and SN, histatins, the major acidic PRPs, P-C and P-B peptides. The cystatin SN abundance lowered according to the disease duration and histatins showed positive correlations with the C reactive protein. Statistical analysis performed excluding one patient with a different pattern of salivary proteins/peptides highlighted a positive relationship between cystatin S1, histatins 3, histatin 5, and the neutrophil count. Moreover, histatin 3 correlated positively with the total white cell count and negatively with the erythrocyte sedimentation rate. Levels and frequency of S100A12 protein showed a trend to increase in SAPHO patients. The high expression of this pro-inflammatory protein is probably related to the inflammatory response and to the altered neutrophil responses to functional stimuli that characterize SAPHO syndrome suggesting a possible application as a salivary biomarker.

  5. Glucosinolate profiles by HPLC-DAD, phenolic compositions and antioxidant activity of Eruca vesicaria longirostris: Impact of plant part and origin

    OpenAIRE

    Bouacida, Saoussen; Koubaier, Hayet Ben Haj; Snoussi, Ahmed; Fauconnier, Marie-Laure; Bouzouita, Nabiha

    2016-01-01

    The glucosinolate profiles, phenol and flavonoid contents and the antioxidant activity of Eruca vesicaria longirostris were studied for different organs and origins. Eleven desulpho-glucosinolates (DS-GLSs) were isolated and quantified by lipid chromatography- DAD. Similarity between profiles was obtained. Total DS-GLS content, expressed as sinigrin equivalents (SE) revealed a certain variabilily ranging between (76.07-45.61), (27.01-13.53), (4.52 -18.01), (9.39-3.37) and (1.16-13.99) µmol /g...

  6. High-resolution bioactivity profiling combined with HPLC-HRMS-SPE-NMR: α-glucosidase inhibitors and acetylated ellagic acid rhamnosides from Myrcia palustris DC. (Myrtaceae)

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Moresco, Henrique H.; Tahtah, Yousof

    2015-01-01

    , and therefore improved drug leads or functional foods containing α-glucosidase inhibitors are needed for management of blood glucose. In this study, leaves of Myrcia palustris were investigated by high-resolution α-glucosidase inhibition profiling combined with HPLC–HRMS–SPE–NMR. This led to identification...

  7. Effects of Different Grinding Methods on Morphological, Textural Properties and Pasting Profiles of MR220 Rice Flour

    International Nuclear Information System (INIS)

    Noorlaila Ahmad; Asmeda Rajab; Norziah Mohd Hani

    2016-01-01

    Three different grinding techniques (dry, semi-wet, and wet) were employed in rice flour production. Investigation on the effects of the grinding techniques on starch damage percentage, particle size distribution, pasting profiles, morphological and textural properties of rice flours produced were evaluated. Wet grinding resulted in significantly (p<0.05) has lower percentage of damaged starch (3.24 %) than other grinding methods. Morphological studies (microscopy and particle size analysis) have reflected significant differences among rice flours granule shapes. The granules displaying different shapes of polygonal, round and angular forms, with some as an individual granule while others tend to attached together. Wet grinding technique also yielded flour that exhibit significantly (p<0.05) with higher gel hardness (16.62 g). Pasting profiles showed that pasting temperature for rice flour produce using these three grinding methods varied between 80.15 - 80.42 degree Celcius. Results revealed that the three grinding techniques clearly affected the physicochemical properties of rice flour. The results from this study play an important role in the selection criteria of rice flour with desirable pasting and textural properties for manufacturing rice-based product. (author)

  8. Classification of Ultra-High Resolution Orthophotos Combined with DSM Using a Dual Morphological Top Hat Profile

    Directory of Open Access Journals (Sweden)

    Qian Zhang

    2015-12-01

    Full Text Available New aerial sensors and platforms (e.g., unmanned aerial vehicles (UAVs are capable of providing ultra-high resolution remote sensing data (less than a 30-cm ground sampling distance (GSD. This type of data is an important source for interpreting sub-building level objects; however, it has not yet been explored. The large-scale differences of urban objects, the high spectral variability and the large perspective effect bring difficulties to the design of descriptive features. Therefore, features representing the spatial information of the objects are essential for dealing with the spectral ambiguity. In this paper, we proposed a dual morphology top-hat profile (DMTHP using both morphology reconstruction and erosion with different granularities. Due to the high dimensional feature space, we have proposed an adaptive scale selection procedure to reduce the feature dimension according to the training samples. The DMTHP is extracted from both images and Digital Surface Models (DSM to obtain complimentary information. The random forest classifier is used to classify the features hierarchically. Quantitative experimental results on aerial images with 9-cm and UAV images with 5-cm GSD are performed. Under our experiments, improvements of 10% and 2% in overall accuracy are obtained in comparison with the well-known differential morphological profile (DMP feature, and superior performance is observed over other tested features. Large format data with 20,000 × 20,000 pixels are used to perform a qualitative experiment using the proposed method, which shows its promising potential. The experiments also demonstrate that the DSM information has greatly enhanced the classification accuracy. In the best case in our experiment, it gives rise to a classification accuracy from 63.93% (spectral information only to 94.48% (the proposed method.

  9. Comparative Three-Dimensional Morphology of Baleen: Cross-Sectional Profiles and Volume Measurements Using CT Images.

    Science.gov (United States)

    Jensen, Megan M; Saladrigas, Amalia H; Goldbogen, Jeremy A

    2017-11-01

    Baleen whales are obligate filter feeders, straining prey-laden seawater through racks of keratinized baleen plates. Despite the importance of baleen to the ecology and natural history of these animals, relatively little work has been done on baleen morphology, particularly with regard to the three-dimensional morphology and structure of baleen. We used computed tomography (CT) scanning to take 3D images of six baleen specimens representing five species, including three complete racks. With these images, we described the three-dimensional shape of the baleen plates using cross-sectional profiles from within the gum tissue to the tip of the plates. We also measured the percentage of each specimen that was composed of either keratinized plate material or was void space between baleen plates, and thus available for seawater flow. Baleen plates have a complex three-dimensional structure with curvature that varies across the anterior-posterior, proximal-distal, and medial-lateral (lingual-labial) axes. These curvatures also vary with location along the baleen rack, and between species. Cross-sectional profiles resemble backwards-facing airfoils, and some specimens display S-shaped, or reflexed, camber. Within a baleen specimen, the intra-baleen void volume correlates with the average bristle diameter for a species, suggesting that essentially, thinner plates (with more space between them for flow) have thinner bristles. Both plate curvature and the relative proportions of plate and void volumes are likely to have implications for the mechanics of mysticete filtration, and future studies are needed to determine the particular functions of these morphological characters. Anat Rec, 300:1942-1952, 2017. © 2017 The Authors The Anatomical Record published by Wiley Periodicals, Inc. on behalf of American Association of Anatomists. © 2017 The Authors The Anatomical Record published by Wiley Periodicals, Inc. on behalf of American Association of Anatomists.

  10. Potential of Polygonum cuspidatum Root as an Antidiabetic Food: Dual High-Resolution α-Glucosidase and PTP1B Inhibition Profiling Combined with HPLC-HRMS and NMR for Identification of Antidiabetic Constituents.

    Science.gov (United States)

    Zhao, Yong; Chen, Martin Xiaoyong; Kongstad, Kenneth Thermann; Jäger, Anna Katharina; Staerk, Dan

    2017-06-07

    The worldwide increasing incidence of type 2 diabetes has fueled an intensified search for food and herbal remedies with preventive and/or therapeutic properties. Polygonum cuspidatum Siebold & Zucc. (Polygonaceae) is used as a functional food in Japan and South Korea, and it is also a well-known traditional antidiabetic herb used in China. In this study, dual high-resolution α-glucosidase and protein-tyrosine phosphatase 1B (PTP1B) inhibition profiling was used for the identification of individual antidiabetic constituents directly from the crude ethyl acetate extract and fractions of P. cuspidatum. Subsequent preparative-scale HPLC was used to isolate a series of α-glucosidase inhibitors, which after HPLC-HRMS and NMR analysis were identified as procyanidin B2 3,3″-O-digallate (3) and (-)-epicatechin gallate (5) with IC 50 values of 0.42 ± 0.02 and 0.48 ± 0.0004 μM, respectively, as well as a series of stilbene analogues with IC 50 value in the range from 6.05 ± 0.05 to 116.10 ± 2.04 μM. In addition, (trans)-emodin-physcion bianthrone (15b) and (cis)-emodin-physcion bianthrone (15c) were identified as potent PTP1B inhibitors with IC 50 values of 2.77 ± 1.23 and 7.29 ± 2.32 μM, respectively. These findings show that P. cuspidatum is a potential functional food for management of type 2 diabetes.

  11. High-resolution bacterial growth inhibition profiling combined with HPLC-HRMS-SPE-NMR for identification of antibacterial constituents in Chinese plants used to treat snakebites

    DEFF Research Database (Denmark)

    Liu, Yueqiu; Nielsen, Mia; Stærk, Dan

    2014-01-01

    Bacillus subtilis, Staphylococcus aureus, Escherichia coli or Pseudomonas aeruginosa. The biochromatograms demonstrated that tannins play a main role for the bacterial growth inhibition observed for all above-mentioned plants except for Polygonum cuspidatum. Furthermore, the high-resolution bacterial...... growth inhibition profiling combined with HPLC–HRMS–SPE–NMR allowed fast identification of three non-tannin active compounds, i.e., piceid, resveratrol and emodin from ethanol extract of Polygonum cuspidatum. Conclusion The high-resolution bacterial growth inhibition profiling allowed fast pinpointing...... of constituents responsible for the bioactivity, e.g., either showing tannins being the main bacterial growth inhibitors as observed for the majority of the active plants, or combined with HPLC–HRMS–SPE–NMR for fast structural identification of non-tannin constituents correlated with antibacterial activity....

  12. Morphological profile of the best pan-american team handball players by game position

    Directory of Open Access Journals (Sweden)

    Maria Fátima Glaner

    1999-12-01

    Full Text Available The purpose of this study was to characterize the morphological variables, by game position (GP, of male athletes who participated on the X Pan-American Games in Team Handball (XPGTH and also to analyze the very same variables of the best athletes in relation to other athletes who played in the same GP. 103 athletes were measured, and the national team coaches who participated in the XPGTH selected the best seven players in the Pan-American Games, for each game position. The morphological variables characterized were: body mass; stature (ST; arm span (AS; lower extremity length (LEL; hand and wrist breadth; forearm perimeter and body composition. The results obtained demonstrated that many athletes had morphological characteristics beyond the ideal for this sport. The Z scores indicate that the best athletes from different GP (goalkeeper, backcourt, wings and circle runner exhibited larger morphological characteristics in relation to the means for the other players in their respective GP. The best goalkeeper and the circle runner were the only ones whose scores were higher in relation to each GP, respectively, when the entire group of morphological variables were considered together. The variables that demonstrated greater morphological development for the best athletesin the 4 GP, compared to the other athletes, were: ST, AS, LEL, % fat and lean body mass. ARESUMO Objetivou-se caracterizar as variáveis morfológicas dos atletas, por posição de jogo (PJ, das seleções participantes dos X Jogos Pan-Americanos de Handebol Masculino (XJPHM, e analisar as variáveis dos melhores atletas de cada PJ em relação aos demais das respectivas PJ. Mensurou-se 103 atletas. Sete deles foram selecionados por PJ, pelos treinadores das seleções participantes dos XJPHM, como os melhores da competição. Caracterizou-se as variáveis morfológicas: massa corporal; estatura (ES; envergadura (ENV; comprimento dos membros inferiores (CMI; diâmetros palmar e r

  13. Biochemical, histopathological and morphological profiling of a rat model of early immune stimulation: relation to psychopathology.

    Directory of Open Access Journals (Sweden)

    Anna Kubesova

    Full Text Available Perinatal immune challenge leads to neurodevelopmental dysfunction, permanent immune dysregulation and abnormal behaviour, which have been shown to have translational validity to findings in human neuropsychiatric disorders (e.g. schizophrenia, mood and anxiety disorders, autism, Parkinson's disease and Alzheimer's disease. The aim of this animal study was to elucidate the influence of early immune stimulation triggered by systemic postnatal lipopolysaccharide administration on biochemical, histopathological and morphological measures, which may be relevant to the neurobiology of human psychopathology. In the present study of adult male Wistar rats we examined the brain and plasma levels of monoamines (dopamine, serotonin, their metabolites, the levels of the main excitatory and inhibitory neurotransmitters glutamate and γ-aminobutyric acid and the levels of tryptophan and its metabolites from the kynurenine catabolic pathway. Further, we focused on histopathological and morphological markers related to pathogenesis of brain diseases--glial cell activation, neurodegeneration, hippocampal volume reduction and dopaminergic synthesis in the substantia nigra. Our results show that early immune stimulation in adult animals alters the levels of neurotransmitters and their metabolites, activates the kynurenine pathway of tryptophan metabolism and leads to astrogliosis, hippocampal volume reduction and a decrease of tyrosine hydroxylase immunoreactivity in the substantia nigra. These findings support the crucial pathophysiological role of early immune stimulation in the above mentioned neuropsychiatric disorders.

  14. Ecological and morphological profile of floating spherical Cladophora socialis aggregations in central Thailand.

    Directory of Open Access Journals (Sweden)

    Isao Tsutsui

    Full Text Available The unique beauty of spherical aggregation forming algae has attracted much attention from both the scientific and lay communities. Several aegagropilous seaweeds have been identified to date, including the plants of genus Cladophora and Chaetomorpha. However, this phenomenon remains poorly understood. In July 2013, a mass occurrence of spherical Cladophora aggregations was observed in a salt field reservoir in Central Thailand. The aims of the present study were to describe the habitat of the spherical aggregations and confirm the species. We performed a field survey, internal and external morphological observations, pyrenoid ultrastructure observations, and molecular sequence analysis. Floating spherical Cladophora aggregations (1-8 cm in diameter were observed in an area ~560 m2, on the downwind side of the reservoir where there was water movement. Individual filaments in the aggregations were entangled in each other; consequently, branches growing in different directions were observed within a clump. We suggest that water movement and morphological characteristics promote the formation of spherical aggregations in this species. The molecular sequencing results revealed that the study species was highly homologous to both C. socialis and C. coelothrix. However, the diameter of the apical cells in the study species was less than that of C. coelothrix. The pyrenoid ultrastructure was more consistent with that of C. socialis. We conclude that the study species is C. socialis. This first record of spherical aggregations in this species advances our understanding of these formations. However, further detailed physical measurements are required to fully elucidate the mechanism behind these spherical formations.

  15. Ecological and morphological profile of floating spherical Cladophora socialis aggregations in central Thailand.

    Science.gov (United States)

    Tsutsui, Isao; Miyoshi, Tatsuo; Sukchai, Halethichanok; Pinphoo, Piyarat; Aue-Umneoy, Dusit; Meeanan, Chonlada; Songphatkaew, Jaruwan; Klomkling, Sirimas; Yamaguchi, Iori; Ganmanee, Monthon; Sudo, Hiroyuki; Hamano, Kaoru

    2015-01-01

    The unique beauty of spherical aggregation forming algae has attracted much attention from both the scientific and lay communities. Several aegagropilous seaweeds have been identified to date, including the plants of genus Cladophora and Chaetomorpha. However, this phenomenon remains poorly understood. In July 2013, a mass occurrence of spherical Cladophora aggregations was observed in a salt field reservoir in Central Thailand. The aims of the present study were to describe the habitat of the spherical aggregations and confirm the species. We performed a field survey, internal and external morphological observations, pyrenoid ultrastructure observations, and molecular sequence analysis. Floating spherical Cladophora aggregations (1-8 cm in diameter) were observed in an area ~560 m2, on the downwind side of the reservoir where there was water movement. Individual filaments in the aggregations were entangled in each other; consequently, branches growing in different directions were observed within a clump. We suggest that water movement and morphological characteristics promote the formation of spherical aggregations in this species. The molecular sequencing results revealed that the study species was highly homologous to both C. socialis and C. coelothrix. However, the diameter of the apical cells in the study species was less than that of C. coelothrix. The pyrenoid ultrastructure was more consistent with that of C. socialis. We conclude that the study species is C. socialis. This first record of spherical aggregations in this species advances our understanding of these formations. However, further detailed physical measurements are required to fully elucidate the mechanism behind these spherical formations.

  16. Profiling and characterization of sialylated N-glycans by 2D-HPLC (HIAX/PGC) with online orbitrap MS/MS and offline MSn.

    Science.gov (United States)

    Hanneman, Andrew J S; Strand, James; Huang, Chi-Ting

    2014-02-01

    Glycosylation is a critical parameter used to evaluate protein quality and consistency. N-linked glycan profiling is fundamental to the support of biotherapeutic protein manufacturing from early stage process development through drug product commercialization. Sialylated glycans impact the serum half-life of receptor-Fc fusion proteins (RFPs), making their quality and consistency a concern during the production of fusion proteins. Here, we describe an analytical approach providing both quantitative profiling and in-depth mass spectrometry (MS)-based structural characterization of sialylated RFP N-glycans. Aiming to efficiently link routine comparability studies with detailed structural characterization, an integrated workflow was implemented employing fluorescence detection, online positive and negative ion tandem mass spectrometry (MS/MS), and offline static nanospray ionization-sequential mass spectrometry (NSI-MS(n)). For routine use, high-performance liquid chromatography profiling employs established fluorescence detection of 2-aminobenzoic acid derivatives (2AA) and hydrophilic interaction anion-exchange chromatography (HIAX) charge class separation. Further characterization of HIAX peak fractions is achieved by online (-) ion orbitrap MS/MS, offering the advantages of high mass accuracy and data-dependent MS/MS. As required, additional characterization uses porous graphitized carbon in the second chromatographic dimension to provide orthogonal (+) ion MS/MS spectra and buffer-free liquid chromatography peak eluants that are optimum for offline (+)/(-) NSI-MS(n) investigations to characterize low-abundance species and specific moieties including O-acetylation and sulfation. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

  17. Vitis International Variety Catalogue (VIVC: A cultivar database referenced by genetic profiles and morphology

    Directory of Open Access Journals (Sweden)

    Maul Erika

    2015-01-01

    Full Text Available The establishment of the Vitis International Variety Catalogue (VIVC dates back to 1984. The idea was to virtually assemble all accessions maintained in the worldwide existing collections to face genetic erosion. In many cases synonymy, homonymy and misnaming hampered the clear assignment of cultivars/accessions to prime names. In the past 15 years nuclear microsatellites, in particular the nine SSR-markers VVS2, VVMD5, VVMD7, VVMD25, VVMD27, VVMD28, VVMD32, VrZAG62 and VrZAG79 were extensively applied for cultivar recognition in combination with ampelography. Genetic fin- gerprints of more than 15,000 cultivars/accessions were collected. They were taken from more than 300 articles and from microsatellite databases on the web. Allele sizes were adapted according to own internal reference varieties. Comparison of profiles revealed new identities like: “Corbeau” = “Sevilhao”, “Gragnelut” = “Fer”, “Beretinjak” = “Bianco d’Alessano”. The activities aim to equip the prime names of VIVC with reliable genetic profiles combined with the validation of their identity by ampelography. Fingerprints from 1,500 cultivars were already uploaded in VIVC. Two distinct search modules were imple- mented: “Microsatellites by varieties” and “Microsatellites by profiles”. The implementation assists the management of grape- vine genetic resources, e.g. trueness to type assessment in grapevine collections and serves research and breeding.

  18. Combined use of high-resolution α-glucosidase inhibition profiling and HPLC-HRMS-SPE-NMR for investigation of antidiabetic principles in crude plant extracts

    DEFF Research Database (Denmark)

    Kongstad, Kenneth Thermann; Özdemir, Ceylan; Barzak, Asmah

    2015-01-01

    Type 2 diabetes is a metabolic disorder affecting millions of people worldwide, and new drug leads or functional foods containing selective α-glucosidase inhibitors are needed. Crude extract of 24 plants were assessed for α-glucosidase inhibitory activity. Methanol extracts of Cinnamomum zeylanicum...... bark, Rheum rhabarbarum peel, and Rheum palmatum root and ethyl acetate extracts of C. zeylanicum bark, Allium ascalonicum peel, and R. palmatum root showed IC50 values below 20 μg/mL. Subsequently, high-resolution α-glucosidase profiling was used in combination with high-performance liquid...... chromatography–high-resolution mass spectrometry–solid-phase extraction–nuclear magnetic resonance spectroscopy for identification of metabolites responsible for the α-glucosidase inhibitory activity. Quercetin (1) and its dimer (2), trimer (3), and tetramer (4) were identified as main α-glucosidase inhibitors...

  19. Glucosinolate profiles by HPLC-DAD, phenolic compositions and antioxidant activity of Eruca vesicaria longirostris: Impact of plant part and origin

    Directory of Open Access Journals (Sweden)

    Saoussen Bouacida

    2016-06-01

    Full Text Available The glucosinolate profiles, phenol and flavonoid contents and the antioxidant activity of Eruca vesicaria longirostris were studied for different organs and origins. Eleven desulpho-glucosinolates (DS-GLSs were isolated and quantified by lipid chromatography- DAD. Similarity between profiles was obtained. Total DS-GLS content, expressed as sinigrin equivalents (SE revealed a certain variabilily ranging between (76.07-45.61, (27.01-13.53, (4.52 -18.01, (9.39-3.37 and (1.16-13.99 µmol /g DW for seeds, flowers, leaves, roots and stems, respectively. Results showed that seeds are rich in phenolics as they contain highest amounts of phenolics ranging from 27.6±0.5 to 33.47±0.5 mg GAE/g extract as compared to all other parts. Leaves and flowers had a significantly higher total phenolic content than stems and roots in all samples (p < 0.05. According to statistical analysis, the investigated seed extracts with values between (16.20±0.10-18.50±0.10 mg QE/g exhibited the highest total flavonoids content, followed by leaves (13.00±0.40-15.80±0.30mg QE/g, flowers (10.40±0.40-12.90±0.90 mg QE/g and stems (7.80±0.20- 9.80±0.70 mg QE/g. Antioxidant activity tested by DPPH, ABTS and FRAP assays, was higher for seeds, leaves and flowers than the other studied organs. These organs were characterized by a significantly high content in glucoerucin, nasturtin and epiprogroitrin, respectively.

  20. Sensitive detectors in HPLC

    International Nuclear Information System (INIS)

    Anon.

    1992-01-01

    Detection of sample components in HPLC is difficult for many reasons; the key difficulty is the mobile phase which usually has properties similar to the solute. A variety of detectors have been developed for use in HPLC based on one of the above approaches; however, the search is still continuing for an ideal or universal detector. A universal detector should have the following characteristics: (1) responds to all solutes or has predictable specificity; (2) high detectability and the same predictable response; (3) fast response; (4) wide range of linearity; (5) unaffected by changes in temperature and mobile-phase flow; (6) responds independently of the mobile phase; (7) makes no contribution to extracolumn band broadening; (8) reliable and convenient to use; (9) nondestructive to the solute; (10) provides qualitative information on the detected peak. Unfortunately, no available HPLC detector possesses all these properties. 145 refs

  1. The role of substrate morphology for the cytokine release profile of immature human primary macrophages

    Energy Technology Data Exchange (ETDEWEB)

    Bartneck, Matthias [Department of Medicine III, Medical Faculty, RWTH Aachen, Pauwelsstr. 30, 52074 Aachen (Germany); Heffels, Karl-Heinz [Department and Chair of Functional Materials in Medicine and Dentistry, University of Würzburg, Pleicherwall 2, 97070 Würzburg (Germany); Bovi, Manfred [Electron Microscopic Facility, Medical Faculty, RWTH Aachen (Germany); Groll, Jürgen [Department and Chair of Functional Materials in Medicine and Dentistry, University of Würzburg, Pleicherwall 2, 97070 Würzburg (Germany); Zwadlo-Klarwasser, Gabriele [Interdisciplinary Center for Clinical Research and Dept. of Dermatology, Medical Faculty, RWTH Aachen, Pauwelsstr. 30, 52056 Aachen (Germany)

    2013-12-01

    There is increasing evidence that the physicochemical nature of any given material is a dominant factor for the release of cytokines by innate immune cells, specifically of macrophages, and thus majorly influences their interaction with other cell types. Recently, we could show that the 3D structure of star shaped polytheylene oxide–polypropylene oxide co-polymers (sP(EO-stat-PO))-hydrogel coated substrates has a stronger influence on the release pattern of cytokines after 7 days of culture than surface chemistry. Here, we focused on the analysis of cytokine release over time and a more detailed analysis of cell morphology by scanning electron microscopy (SEM). Therefore, we compared different strategies for SEM sample preparation and found that using osmium tetroxide combined with aqua bidest led to best preparation results. For cytokine release we show significant changes from day 3 to day 7 of cell culture. After 3 days, the sP(EO-stat-PO)-coated substrates led to an induction of pro-angiogenic CCL3 and CCL4, and of low amounts of the anti-inflammatory IL10, which declined at day 7. In contrast, pleiotropic IL6 and the pro-inflammatory TNFα and IL1β were expressed stronger at day 7 than at day 3. - Highlights: • Strategies for the preparation of macrophages on hydrogel materials (Fig. 1) • Cytokine release of immature macrophages on the substrates (Fig. 2 and Table 1) • Changes in cytokine release during macrophage maturation (Table 2)

  2. Morphology of the bipolar planetary nebula NGC 2346 from emission line profile studies

    Energy Technology Data Exchange (ETDEWEB)

    Anandarao, B G; Banerjee, D P.K.; Desai, J N; Jain, S K; Mallik, D C.V.

    1988-11-01

    High resolution observations of H..cap alpha.. 6563 A, (O III) 5007 A and (N II) 6583 A emission lines in the bipolar planetary nebula NGC 2346 are presented. Expansion velocities (V/sub exp/) of 8 +- 1 km s/sup -1/ in the :O III: line and 11 +- 1 km s/sup -1/ in the :N II: line are observed in the central region. An expansion velocity of 7.5 +- 1.0 km s/sup -1/ in the (O III) line is observed in a position 10 arcsec away from the centre, in the NE lobe of the nebula. From the widths of the H..cap alpha.. and (N II) lines, an ion temperature of T=10 650 +- 2950 K and a turbulent velocity V/sub T/ = 16 +- 2 km s/sup -1/ are derived. Using the detailed radial velocity mapping done by a previous author, a morphological model for the nebula is presented.

  3. Analysis of protein profile and pollen morphology of guaiacum officinale linn

    International Nuclear Information System (INIS)

    Zeb, S.

    2017-01-01

    Asthma and allergic rhinitis is triggered by the pollen of trees, grasses and weeds. Guaiacum officinale L. tree is widely cultivated along with the road side. This species was selected to check its allergenic role.Pollen morphology of Guaiacum officinale was examined by Light microsco4pe (LM) and Scanning electron microscope (SEM). Pollen grains of Guaiacum officinale were prolate shape, having tricolpate aperture, and rugulate tectum. Pollen protein concentration of G. officinale was determined by Bradford's assay and qualitative protein analysis of pollen was done by SDS-PAGE(Sodium Dodecyl Sulphate Polyacrylamide Gel Electrophoresis).Total protein content in the pollen extract was 24.28mg/g of pollen. The SDS-PAGE pollen grains protein analysis showed 07 different protein bands. The molecular weight of separated proteins ranged from 25 to 65kDa. Biochemical analysis of G. officinale pollen grains revealed the presence of low molecular weight proteins therefore it is strongly suggested that this species must be considered as a potent allergy causing species. This research would help for the proper diagnosis and treatment of the bronchial allergy suffering patients. (author)

  4. The role of substrate morphology for the cytokine release profile of immature human primary macrophages

    International Nuclear Information System (INIS)

    Bartneck, Matthias; Heffels, Karl-Heinz; Bovi, Manfred; Groll, Jürgen; Zwadlo-Klarwasser, Gabriele

    2013-01-01

    There is increasing evidence that the physicochemical nature of any given material is a dominant factor for the release of cytokines by innate immune cells, specifically of macrophages, and thus majorly influences their interaction with other cell types. Recently, we could show that the 3D structure of star shaped polytheylene oxide–polypropylene oxide co-polymers (sP(EO-stat-PO))-hydrogel coated substrates has a stronger influence on the release pattern of cytokines after 7 days of culture than surface chemistry. Here, we focused on the analysis of cytokine release over time and a more detailed analysis of cell morphology by scanning electron microscopy (SEM). Therefore, we compared different strategies for SEM sample preparation and found that using osmium tetroxide combined with aqua bidest led to best preparation results. For cytokine release we show significant changes from day 3 to day 7 of cell culture. After 3 days, the sP(EO-stat-PO)-coated substrates led to an induction of pro-angiogenic CCL3 and CCL4, and of low amounts of the anti-inflammatory IL10, which declined at day 7. In contrast, pleiotropic IL6 and the pro-inflammatory TNFα and IL1β were expressed stronger at day 7 than at day 3. - Highlights: • Strategies for the preparation of macrophages on hydrogel materials (Fig. 1) • Cytokine release of immature macrophages on the substrates (Fig. 2 and Table 1) • Changes in cytokine release during macrophage maturation (Table 2)

  5. Early steps of adventitious rooting: morphology, hormonal profiling and carbohydrate turnover in carnation stem cuttings.

    Science.gov (United States)

    Agulló-Antón, María Ángeles; Ferrández-Ayela, Almudena; Fernández-García, Nieves; Nicolás, Carlos; Albacete, Alfonso; Pérez-Alfocea, Francisco; Sánchez-Bravo, José; Pérez-Pérez, José Manuel; Acosta, Manuel

    2014-03-01

    The rooting of stem cuttings is a common vegetative propagation practice in many ornamental species. A detailed analysis of the morphological changes occurring in the basal region of cultivated carnation cuttings during the early stages of adventitious rooting was carried out and the physiological modifications induced by exogenous auxin application were studied. To this end, the endogenous concentrations of five major classes of plant hormones [auxin, cytokinin (CK), abscisic acid, salicylic acid (SA) and jasmonic acid] and the ethylene precursor 1-aminocyclopropane-1-carboxylic acid were analyzed at the base of stem cuttings and at different stages of adventitious root formation. We found that the stimulus triggering the initiation of adventitious root formation occurred during the first hours after their excision from the donor plant, due to the breakdown of the vascular continuum that induces auxin accumulation near the wounding. Although this stimulus was independent of exogenously applied auxin, it was observed that the auxin treatment accelerated cell division in the cambium and increased the sucrolytic activities at the base of the stem, both of which contributed to the establishment of the new root primordia at the stem base. Further, several genes involved in auxin transport were upregulated in the stem base either with or without auxin application, while endogenous CK and SA concentrations were specially affected by exogenous auxin application. Taken together our results indicate significant crosstalk between auxin levels, stress hormone homeostasis and sugar availability in the base of the stem cuttings in carnation during the initial steps of adventitious rooting. © 2013 Scandinavian Plant Physiology Society.

  6. Morphological, maturational, functional and technical profile of young Brazilian soccer players

    Directory of Open Access Journals (Sweden)

    Marcelo de Oliveira Matta

    2014-03-01

    The objectives of this study were to describe and compare the anthropometric profile, physical fitness and soccer-specific skills between under-15 and under-17 Brazilian soccer players, as well as to evaluate possible differences in these variables according to biological maturation in the age categories. The sample consisted of 245 male soccer players (under-15: n=161; under-17: n=84. Anthropometric measures included weight, height and skinfolds. Biological maturation was assessed based on pubic hair development. The following tests were used for functional assessment: static and countermovement jump, Yo-Yo intermittent endurance test (level 2, RAST, 5- and 30-meter running speed, and agility T-test. Soccer-specific skills were assessed using three tests: ball control, dribbling, and kick accuracy. Descriptive statistics, t-test and analysis of variance (ANOVA were used for statistical analysis. The results showed a larger body size (stature and body mass, longer sports experience (years of formal training and better performance in most of the functional tests for under-17 soccer players compared to under-15 players. There were no significant differences in adiposity or soccer-specific skills between levels of competition. Significant differences as a function of maturation stage were observed in anthropometric and functional variables only in the under-15 category. In conclusion, the under-17 category differs from the under-15 category in terms of anthropometric and physical fitness characteristics. However, no difference was observed in two of the three soccer-specific skills. Physical fitness components and soccer-specific skills were associated with maturity only in the under-15 category.

  7. An Investigation of Amphitheater-Headed Canyon Distribution, Morphology Variation, and Longitudinal Profile Controls in Escalante and Tarantula Mesa, Utah.

    Science.gov (United States)

    Ryan, A. J.; Whipple, K. X.

    2014-12-01

    Amphitheater-headed canyons are primarily distinguished from typical fluvial channels by their abrupt headwall terminations. A key goal in the study of river canyons is to establish a reliable link between form and formation processes. This is of particular significance for Mars, where, if such links can be established, amphitheater-headed canyons could be used to determine ancient erosion mechanisms and, by inference, climate conditions. Type examples in arid regions on Earth, such as in Escalante River, Utah, previously have been interpreted as products of groundwater seepage erosion. We investigate amphitheater-headed canyons in Escalante and Tarantula Mesa where variations in canyon head morphology may hold clues for the relative roles of rock properties and fluvial and groundwater processes. In lower Escalante, amphitheaters are only present where canyons have breached the Navajo Sandstone - Kayenta Formation contact. In some canyons, amphitheater development appears to have been inhibited by an abundance of coarse bedload. In Tarantula Mesa, canyons have a variety of headwalls, from amphitheaters to stepped knickzones. Headwall morphology distribution is directly related to the spatially variable presence of knickpoint-forming, fine-grained interbeds within cliff-forming sandstones. Amphitheaters only form where the sandstone unit is undisrupted by these interbeds. Finally, most canyons in Escalante and Tarantula Mesa, regardless of substrate lithology, amphitheater presence, or groundwater spring intensity, are well described by a slope-area power law relationship with regionally constant concavity and normalized steepness indices. This suggests that all channels here are subject to the same erosion rates, independent of groundwater weathering intensity. Thus: 1) variations in canyon headwall form do not necessary relate to differences in fluvial history, 2) stratigraphic variations are clearly of importance in sedimentary canyon systems, and 3) although

  8. Methods and applications of HPLC-AMS

    International Nuclear Information System (INIS)

    Buchholz, Bruce A.; Dueker, Stephen R.; Lin, Yumei; Clifford, Andrew J.; Vogel, John S.

    2000-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a 14 C-labeled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the 14 C content above the control predose tissue and converting to equivalents of the parent compound. High performance liquid chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are tentatively identified by co-elution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the 14 C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of 14 C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected 14 C activity <0.17 Bq (4.5 pCi) on the HPLC column

  9. Non-invasive metabolomic profiling of embryo culture media and morphology grading to predict implantation outcome in frozen-thawed embryo transfer cycles.

    Science.gov (United States)

    Li, Xiong; Xu, Yan; Fu, Jing; Zhang, Wen-Bi; Liu, Su-Ying; Sun, Xiao-Xi

    2015-11-01

    Assessment of embryo viability is a crucial component of in vitro fertilization and currently relies largely on embryo morphology and cleavage rate. Because morphological assessment remains highly subjective, it can be unreliable in predicting embryo viability. This study investigated the metabolomic profiling of embryo culture media using near-infrared (NIR) spectroscopy for predicting the implantation potential of human embryos in frozen-thawed embryo transfer (FET) cycles. Spent embryo culture media was collected on day 4 after thawed embryo transfer (n = 621) and analysed using NIR spectroscopy. Viability scores were calculated using a predictive multivariate algorithm of fresh embryos with known pregnancy outcomes. The mean viability indices of embryos resulting in clinical pregnancy following FET were significantly higher than those of non-implanted embryos and differed between the 0, 50, and 100 % implantation groups. Notably, the 0 % group index was significantly lower than the 100 % implantation group index (-0.787 ± 0.382 vs. 1.064 ± 0.331, P  0.05). NIR metabolomic profiling of thawed embryo culture media is independent of morphology and correlates with embryo implantation potential in FET cycles. The viability score alone or in conjunction with morphologic grading is a more objective marker for implantation outcome in FET cycles than morphology alone.

  10. HPLC: Early and Recent Perspectives.

    Science.gov (United States)

    Karger, Barry L.

    1997-01-01

    Provides a perspective on what it was like in the early days of high-performance liquid chromatography (HPLC) and several of the key developments. Focuses on the advances in HPLC generally, and more specifically for the biological sciences, that were necessary for the method to reach the preeminent stage of today. Contains 20 references. (JRH)

  11. Profiles

    International Nuclear Information System (INIS)

    2004-01-01

    Profiles is a synthetic overview of more than 100 national energy markets in the world, providing insightful facts and key energy statistics. A Profile is structured around 6 main items and completed by key statistics: Ministries, public agencies, energy policy are concerned; main companies in the oil, gas, electricity and coal sectors, status, shareholders; reserve, production, imports and exports, electricity and refining capacities; deregulation of prices, subsidies, taxes; consumption trends by sector, energy market shares; main energy projects, production and consumption prospects. Statistical Profiles are present in about 3 pages the main data and indicators on oil, gas, coal and electricity. (A.L.B.)

  12. The value of whole lesion ADC histogram profiling to differentiate between morphologically indistinguishable ring enhancing lesions–comparison of glioblastomas and brain abscesses

    Science.gov (United States)

    Hoffmann, Karl-Titus; Garnov, Nikita; Vörkel, Cathrin; Kohlhof-Meinecke, Patricia; Ganslandt, Oliver; Bäzner, Hansjörg; Gihr, Georg Alexander; Kalman, Marcell; Henkes, Elina; Henkes, Hans; Schob, Stefan

    2018-01-01

    Background Morphologically similar appearing ring enhancing lesions in the brain parenchyma can be caused by a number of distinct pathologies, however, they consistently represent life-threatening conditions. The two most frequently encountered diseases manifesting as such are glioblastoma multiforme (GBM) and brain abscess (BA), each requiring disparate therapeutical approaches. As a result of their morphological resemblance, essential treatment might be significantly delayed or even ommited, in case results of conventional imaging remain inconclusive. Therefore, our study aimed to investigate, whether ADC histogram profiling reliably can distinguish between both entities, thus enhancing the differential diagnostic process and preventing treatment failure in this highly critical context. Methods 103 patients (51 BA, 52 GBM) with histopathologically confirmed diagnosis were enrolled. Pretreatment diffusion weighted imaging (DWI) was obtained in a 1.5T system using b values of 0, 500, and 1000 s/mm2. Whole lesion ADC volumes were analyzed using a histogram-based approach. Statistical analysis was performed using SPSS version 23. Results All investigated parameters were statistically different in comparison of both groups. Most importantly, ADCp10 was able to differentiate reliably between BA and GBM with excellent accuracy (0.948) using a cutpoint value of 70 × 10−5 mm2 × s−1. Conclusions ADC whole lesion histogram profiling provides a valuable tool to differentiate between morphologically indistinguishable mass lesions. Among the investigated parameters, the 10th percentile of the ADC volume distinguished best between GBM and BA. PMID:29719596

  13. The value of whole lesion ADC histogram profiling to differentiate between morphologically indistinguishable ring enhancing lesions-comparison of glioblastomas and brain abscesses.

    Science.gov (United States)

    Horvath-Rizea, Diana; Surov, Alexey; Hoffmann, Karl-Titus; Garnov, Nikita; Vörkel, Cathrin; Kohlhof-Meinecke, Patricia; Ganslandt, Oliver; Bäzner, Hansjörg; Gihr, Georg Alexander; Kalman, Marcell; Henkes, Elina; Henkes, Hans; Schob, Stefan

    2018-04-06

    Morphologically similar appearing ring enhancing lesions in the brain parenchyma can be caused by a number of distinct pathologies, however, they consistently represent life-threatening conditions. The two most frequently encountered diseases manifesting as such are glioblastoma multiforme (GBM) and brain abscess (BA), each requiring disparate therapeutical approaches. As a result of their morphological resemblance, essential treatment might be significantly delayed or even ommited, in case results of conventional imaging remain inconclusive. Therefore, our study aimed to investigate, whether ADC histogram profiling reliably can distinguish between both entities, thus enhancing the differential diagnostic process and preventing treatment failure in this highly critical context. 103 patients (51 BA, 52 GBM) with histopathologically confirmed diagnosis were enrolled. Pretreatment diffusion weighted imaging (DWI) was obtained in a 1.5T system using b values of 0, 500, and 1000 s/mm 2 . Whole lesion ADC volumes were analyzed using a histogram-based approach. Statistical analysis was performed using SPSS version 23. All investigated parameters were statistically different in comparison of both groups. Most importantly, ADCp10 was able to differentiate reliably between BA and GBM with excellent accuracy (0.948) using a cutpoint value of 70 × 10 -5 mm 2 × s -1 . ADC whole lesion histogram profiling provides a valuable tool to differentiate between morphologically indistinguishable mass lesions. Among the investigated parameters, the 10th percentile of the ADC volume distinguished best between GBM and BA.

  14. Noninvasive metabolomic profiling as an adjunct to morphology for noninvasive embryo assessment in women undergoing single embryo transfer

    NARCIS (Netherlands)

    Seli, E.; Vergouw, C.G.; Morita, H.; Botros, L.; Roos, P.; Lambalk, C.B.; Yamashita, N.; Kato, O.; Sakkas, D.

    2010-01-01

    Objective: To determine whether metabolomic profiling of spent embryo culture media correlates with reproductive potential of human embryos. Design: Retrospective study. Setting: Academic and a private assisted reproductive technology (ART) programs. Patient(s): Women undergoing single embryo

  15. Noninvasive Metabolomic Profiling of Human Embryo Culture Media Using a Simple Spectroscopy Adjunct to Morphology for Embryo Assessment in in Vitro Fertilization (IVF

    Directory of Open Access Journals (Sweden)

    Jiming Hu

    2013-03-01

    Full Text Available Embryo quality is crucial to the outcome of in vitro fertilization (IVF; however, the ability to precisely distinguish the embryos with higher reproductive potential from others is poor. Morphologic evaluation used to play an important role in assessing embryo quality, but it is somewhat subjective. The culture medium is the immediate environment of the embryos in vitro, and a change of the substances in the culture medium is possibly related to the embryo quality. Thus, the present study aims to determine whether metabolomic profiling of the culture medium using Raman spectroscopy adjunct to morphology correlates with the reproductive potential of embryos in IVF and, thus, to look for a new method of assessing embryo quality. Fifty seven spent media samples were detected by Raman spectroscopy. Combined with embryo morphology scores, we found that embryos in culture media with less than 0.012 of sodium pyruvate and more than −0.00085 phenylalanine have a high reproductive potential, with up to 85.7% accuracy compared with clinical pregnancy. So, sodium pyruvate and phenylalanine in culture medium play an important role in the development of the embryo. Raman spectroscopy is an important tool that provides a new and accurate assessment of higher quality embryos.

  16. Application of Pattern Recognition Method for Color Assessment of Oriental Tobacco based on HPLC of Polyphenols

    Directory of Open Access Journals (Sweden)

    Dagnon S

    2014-12-01

    Full Text Available The color of Oriental tobaccos was organoleptically assayed, and high performance liquid chromatography (HPLC of polyphenols was performed. The major tobacco polyphenols (chlorogenic acid, its isomers, and rutin, as well as scopoletin and kaempferol-3-rutinoside were quantified. HPLC polyphenol profiles were processed by pattern recognition method (PRM, and the values of indexes of similarity (Is,% between the cultivars studied were determined. It was shown that data from organoleptic color assessment and from PRM based on HPLC profiles of polyphenols of the cultivars studied are largely compatible. Hence, PRM can be suggested as an additional tool for objective color evaluation and classification of Oriental tobacco.

  17. Morphological, physico-chemical and geochemical characterization of two weathering profiles developed on limestone from the Mintom Formation in the tropical humid zone of Cameroon

    Science.gov (United States)

    Engon, Thierry Constant; Abane, Monique Abessolo-Angue; Zo'o Zame, Philémon; Ekomane, Emile; Bekoa, Etienne; Mvogo, Kisito; Bitom, Dieudonné

    2017-07-01

    The purpose of this work was to study the morphology, physico-chemistry and geochemistry of two weathering profiles developed on limestone using observations area, basic analysis, and X-ray Fluorescence. The results showed that these soils have three main sets from the bottom to the top: the alteritic set (isalteritic and alloteritic horizons), the glaebular set (exclusively on profile TCR) with a more or less hardened duricrust, and the loose set (loose clayey and humiferous horizons). The soils were acid, with moderate cation exchange capacity, low to moderate sum of bases (0.96-8.24 meq/100 g). The base saturation, organic carbon and C/N ratio (˂15) were low. The geochemical signatures of the bedrock along the whole profile are not preserved, with SiO2 (∼45.26 wt%) being the dominant oxide followed by Al2O3 (∼13.37 wt%) and Fe2O3 (∼09.36 wt%). Also, the Si/Al ratio is always higher than 1 (2.17-4.43). The other major oxides such as MgO, K2O and Na2O show negligible contents in the profiles, while CaO is well represented at the top of the isalteritic horizon reaching 14.25 wt%. Weathering indices show that CaO, MgO, Na2O, and K2O are rapidly lost during chemical weathering and the amount of these elements lost is proportional to the degree of weathering. Humid tropical soils show pedological evolution mainly dominated by the behaviour of silicon and aluminium, with an intensive release of carbonates during the early stage of weathering. However, contrary to soils in temperate climates, in which bisiallitisation is the predominant process, soils of the humid tropical zone, characterized by high evacuation of silica concomitantly to notable accumulations of aluminium, allitisation and monosiallitisation predominate.

  18. Profiling and sorting Mangifera Indica morphology for quality attributes and grade standards using integrated image processing algorithms

    Science.gov (United States)

    Balbin, Jessie R.; Fausto, Janette C.; Janabajab, John Michael M.; Malicdem, Daryl James L.; Marcelo, Reginald N.; Santos, Jan Jeffrey Z.

    2017-06-01

    Mango production is highly vital in the Philippines. It is very essential in the food industry as it is being used in markets and restaurants daily. The quality of mangoes can affect the income of a mango farmer, thus incorrect time of harvesting will result to loss of quality mangoes and income. Scientific farming is much needed nowadays together with new gadgets because wastage of mangoes increase annually due to uncouth quality. This research paper focuses on profiling and sorting of Mangifera Indica using image processing techniques and pattern recognition. The image of a mango is captured on a weekly basis from its early stage. In this study, the researchers monitor the growth and color transition of a mango for profiling purposes. Actual dimensions of the mango are determined through image conversion and determination of pixel and RGB values covered through MATLAB. A program is developed to determine the range of the maximum size of a standard ripe mango. Hue, light, saturation (HSL) correction is used in the filtering process to assure the exactness of RGB values of a mango subject. By pattern recognition technique, the program can determine if a mango is standard and ready to be exported.

  19. Literatuuronderzoek HPLC-methoden voor vitamine E

    OpenAIRE

    Altena, A.; Hollman, P.C.H.

    1985-01-01

    Doel van dit onderzoek is: het inventariseren van HPLC-methoden voor vitamine E, eventueel in combinatie met vitamine A, in levensmiddelen. Een overzicht van de in de literatuur beschreven HPLC-methoden vanaf ca. 1977 wordt gegeven.

  20. Distinguishing commercially grown Ganoderma lucidum from Ganoderma lingzhi from Europe and East Asia on the basis of morphology, molecular phylogeny, and triterpenic acid profiles.

    Science.gov (United States)

    Hennicke, Florian; Cheikh-Ali, Zakaria; Liebisch, Tim; Maciá-Vicente, Jose G; Bode, Helge B; Piepenbring, Meike

    2016-07-01

    In China and other countries of East Asia, so-called Ling-zhi or Reishi mushrooms are used in traditional medicine since several centuries. Although the common practice to apply the originally European name 'Ganoderma lucidum' to these fungi has been questioned by several taxonomists, this is still generally done in recent publications and with commercially cultivated strains. In the present study, two commercially sold strains of 'G. lucidum', M9720 and M9724 from the company Mycelia bvba (Belgium), are compared for their fruiting body (basidiocarp) morphology combined with molecular phylogenetic analyses, and for their secondary metabolite profile employing an ultra-performance liquid chromatography-electrospray ionization mass spectrometry (UPLC-ESIMS) in combination with a high resolution electrospray ionization mass spectrometry (HR-ESI-MS). According to basidiocarp morphology, the strain M9720 was identified as G. lucidum s.str. whereas M9724 was determined as Ganoderma lingzhi. In molecular phylogenetic analyses, the M9720 ITS and beta-tubulin sequences grouped with sequences of G. lucidum s.str. from Europe whereas those from M9724 clustered with sequences of G. lingzhi from East Asia. We show that an ethanol extract of ground basidiocarps from G. lucidum (M9720) contains much less triterpenic acids than found in the extract of G. lingzhi (M9724). The high amount of triterpenic acids accounts for the bitter taste of the basidiocarps of G. lingzhi (M9724) and of its ethanol extract. Apparently, triterpenic acids of G. lucidum s.str. are analyzed here for the first time. These results demonstrate the importance of taxonomy for commercial use of fungi. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

  1. Methods and applications of HPLC-AMS (WBio 5)

    International Nuclear Information System (INIS)

    Bucholz, B A; Clifford, A J; Duecker, S R; Lin, Y; Vogel, J S

    1999-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a(sup 14)C-labelled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the(sup 14)C content above the control predose tissue and converting to equivalents of the parent compound. High Performance Liquid Chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are identified by coelution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the(sup 14)C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of(sup 14)C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected(sup 14)C activity and lt;0.17 Bq (4.5 pCi) on the HPLC column

  2. Determination of taxonomic status of chinese species of the genus clematis by using high performance liquid chromatography-mass spectrometry (HPLC-MS) technique

    International Nuclear Information System (INIS)

    Ishtiaq, M.; Ahmed, H.

    2010-01-01

    A comparative taxonomic study using chemometric and numerical taxonomic approaches on 15 populations of 12 species of major taxa of the genus Clematis, belonging to sections, Rectae, Clematis, Meclatis, Tubulosae and Viorna were analyzed by HPLC coupled with diode array detector and ESI-MS. The chemo diversity profile of saponins proved to be useful taxonomic markers for the genus and results are presented in pheno grams. The compound 'Huzhangoside D' was the most abundant in analyzed species of the genus. Numerical taxonomic study was also conducted based on phylogenetically informative characters which corroborated with chemical fingerprinting findings. The significance of chemical markers in taxonomic study as well as their correlation between morphology and chemical compound profile is also debated with its significant role in botanic drugs identification. (author)

  3. Effects of β-Glucans Ingestion on Alveolar Bone Loss, Intestinal Morphology, Systemic Inflammatory Profile, and Pancreatic β-Cell Function in Rats with Periodontitis and Diabetes

    Science.gov (United States)

    Silva, Viviam de O.; Lobato, Raquel V.; Orlando, Débora R.; Borges, Bruno D.B.; de Sousa, Raimundo V.

    2017-01-01

    This study aimed to evaluate the effects of β-glucan ingestion (Saccharomyces cerevisiae) on the plasmatic levels of tumor necrosis factor-α (TNF-α) and interleukin-10 (IL-10), alveolar bone loss, and pancreatic β-cell function (HOMA-BF) in diabetic rats with periodontal disease (PD). Besides, intestinal morphology was determined by the villus/crypt ratio. A total of 48 Wistar rats weighing 203 ± 18 g were used. Diabetes was induced by the intraperitoneal injection of streptozotocin (80 mg/kg) and periodontal inflammation, by ligature. The design was completely randomized in a factorial scheme 2 × 2 × 2 (diabetic or not, with or without periodontitis, and ingesting β-glucan or not). The animals received β-glucan by gavage for 28 days. Alveolar bone loss was determined by scanning electron microscopy (distance between the cementoenamel junction and alveolar bone crest) and histometric analysis (bone area between tooth roots). β-glucan reduced plasmatic levels of TNF-α in diabetic animals with PD and of IL-10 in animals with PD (p < 0.05). β-glucan reduced bone loss in animals with PD (p < 0.05). In diabetic animals, β-glucan improved β-cell function (p < 0.05). Diabetic animals had a higher villus/crypt ratio (p < 0.05). In conclusion, β-glucan ingestion reduced the systemic inflammatory profile, prevented alveolar bone loss, and improved β-cell function in diabetic animals with PD. PMID:28906456

  4. Edible seaweed as future functional food: Identification of α-glucosidase inhibitors by combined use of high-resolution α-glucosidase inhibition profiling and HPLC-HRMS-SPE-NMR

    DEFF Research Database (Denmark)

    Liu, Bingrui; Kongstad, Kenneth Thermann; Wiese, Stefanie

    2016-01-01

    -glucosidase inhibition profiling combined with high-performance liquid chromatography–high-resolution mass spectrometry–solid-phase extraction–nuclear magnetic resonance spectroscopy (HR-bioassay/HPLC–HRMS–SPE–NMR). The results showed Ascophyllum nodosum and Fucus vesicolosus to be rich in antioxidants, equaling...... as fatty acids – with oleic acid, linoleic acid and eicosapentaenoic acid being the most potent with IC50 values of 0.069, 0.075 and 0.10 mM, respectively, and showing a mixed-type inhibition mode....

  5. The genus Pyrenomyxa and its affinities to other cleistocarpous Hypoxyloideae as inferred from morphological and chemical traits

    DEFF Research Database (Denmark)

    Stadler, M.; Læssøe, Thomas; Vassilyeva, L.

    2005-01-01

    Types and authentic specimens of Hypoxylon piceum, Pulveria porrecta, and Pyrenomyxa invocans were studied for morphological traits and extrolite (= secondary metabolite) profiles generated by analytical HPLC with UV-visual and mass spectrometric detection. The orange stromatal pigments of P....... invocans are rubiginosin A and mitorubrinol. It lacks three different types of extrolites (BNT, macrocarpone and hypomiltin) that are known from Hypoxylon taxa and occur in H. piceum and P. porrecta. In agreement with morphological traits, the latter two names are regarded as synonymous and transferred...

  6. Plasma hormonal profiles and dendritic spine density and morphology in the hippocampal CA1 stratum radiatum, evidenced by light microscopy, of virgin and postpartum female rats.

    Science.gov (United States)

    Brusco, Janaína; Wittmann, Raul; de Azevedo, Márcia S; Lucion, Aldo B; Franci, Celso R; Giovenardi, Márcia; Rasia-Filho, Alberto A

    2008-06-27

    Successful reproduction requires that changes in plasma follicle-stimulating hormone (FSH), luteinizing hormone (LH), prolactin (PRL), oxytocin (OT), estrogen (E(2)) and progesterone (P(4)) occur together with the display of maternal behaviors. Ovarian steroids and environmental stimuli can affect the dendritic spines in the rat hippocampus. Here, studying Wistar rats, it is described: (a) the sequential and concomitant changes in the hormonal profile of females at postpartum days (PP) 4, 8, 12, 16, 20 and 24, comparing to estrous cycle referential values; (b) the dendritic spine density in the stratum radiatum of CA1 (CA1-SR) Golgi-impregnated neurons in virgin females across the estrous cycle and in multiparous age-matched ones; and (c) the proportion of different types of spines in the CA1-SR of virgin and postpartum females, both in diestrus. Plasma levels of gonadotrophins and ovarian hormones remained low along PP while LH increased and PRL decreased near the end of the lactating period. The lowest dendritic spine density was found in virgin females in estrus when compared to diestrus and proestrus phases or to postpartum females in diestrus (p0.4). There were no differences in the proportions of the different spine types in nulliparous and postpartum females (p>0.2). Results suggest that medium layer CA1-SR spines undergo rapid modifications in Wistar females across the estrous cycle (not quite comparable to Sprague-Dawley data or to hormonal substitutive therapy following ovariectomy), but persistent effects of motherhood on dendritic spine density and morphology were not found in this area.

  7. Arsenic-containing fatty acids and hydrocarbons in marine oils - Determination using reversed-phase HPLC-ICP-MS and HPLC-qTOF-MS

    DEFF Research Database (Denmark)

    Sele, Veronika; Sloth, Jens Jørgen; Holmelid, Bjarte

    2014-01-01

    ; dimethylarsinate (DMA), triphenylarsinoxide (Ph3AsO) and a synthesized arsenic-containing hydrocarbon (AsHC) (dimethylarsinoyl nonadecane; C21H43AsO). The observed variation in signal intensity for arsenic during the gradient elution profile in reversed-phase HPLC was compensated for by determining the time...

  8. Acquisition of HPLC-Mass Spectrometer

    Science.gov (United States)

    2015-08-18

    31-Jan-2015 Approved for Public Release; Distribution Unlimited Final Report: Acquisition of HPLC -Mass Spectrometer The views, opinions and/or findings...published in peer-reviewed journals: Final Report: Acquisition of HPLC -Mass Spectrometer Report Title The acquisition of the mass spectrometer has been a

  9. HPLC ‘Multi-Analyte’ Detection Method

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    The application of multi-analyte methods for pesticides carrying chromophoric structures by HPLC is described. Details are given on the materials and methods used. Recorded UV spectra of active substances are presented for allowing the verification of purity and the confirmation of substances eluting from the HPLC column. (author)

  10. Quality Control of Selected Pesticides with HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasali, H. [Benaki Phytopathological Institute Laboratory of Physical and Chemical Analysis of Pesticides, Ekalis (Greece)

    2009-07-15

    Laboratory data obtained on two different HPLC separation columns and detection by UV and DAD under repeatability conditions are presented and discussed. The behaviour of pesticides on different HPLC columns under gradient and isocratic conditions is evaluated concerning the applicability of respective methodologies. Representative chromatograms of real formulations and “empty” formlants are given for illustration. (author)

  11. Morphology and controlling mechanisms of shallow water pockmarks in the Yellow Sea Basin of China: employing multibeam bathymetry, backscatter data and subbottom profile

    Science.gov (United States)

    Liu, X.

    2017-12-01

    The presence of fluid escape features like seafloor pockmarks are observed in continental margin basins and ocean floors worldwide. While most of the reported depressions developed at deep water, this study provides a description of shallow pockmark field in shallow water that no deep than 55m in continent of the Yellow Sea. Combined with the multi-beam bathymetry data, terrain slope and the back- scattering intensity data, this study calculated the morphological parameters of the seabed pockmarks and carried out quantitative analysis. The outline of the seabed pockmarks were accurately defined, and 282 pockmarks with circle, elliptic, or elongated shape in the plan view were analyzed in ArcGIS. The average diameter of the pockmarks was 0.94 km, average area and circumference were 0.88 km2 and 3.82 km, the pockmarks also have the aspect ratio of 1.83, and relief from 0.5m to 2.5 m. The profile of the pockmarks shaped like W1, W2 and V, respectively distributed in the north, south, and west of the pockmark group. The large plane size but small vertical scale may be associated with the low concentration of the fluid. The orientation of the major axis of the pockmarks has 3 major directions, pockmarks aligned around ENE - WSW, NNE SSW consistent with the main direction of the bottom current in the study area, while pockmarks aligned around NNW-SSE direction mainly controlled by submarine topography. Some pockmark clustered as pockmark chain, which shows that the pockmark shape controlled by the ancient river or lagoon of the sedimentary strata. The acoustic backscatter strength of the pockmark area is of -71dB to -60dB, the average strength data inside the pockmark is significantly higher than the outside, with a difference of 5dB. The high backscatter strength may attribute to the coarse sediments that left inside the pockmark due to winnowing of fine-grained sediments, or result of the precipitation of diagenitic or authigenic minerals associated with fluid venting.

  12. HPLC for quality control of polyimides

    Science.gov (United States)

    Young, P. R.; Sykes, G. F.

    1979-01-01

    High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

  13. Expermental Studies of quantitative evaluation using HPLC

    Directory of Open Access Journals (Sweden)

    Ki Rok Kwon

    2005-06-01

    Full Text Available Methods : This study was conducted to carry out quantitative evaluation using HPLC Content analysis was done using HPLC Results : According to HPLC analysis, each BVA-1 contained approximately 0.36㎍ melittin, and BVA-2 contained approximately 0.54㎍ melittin. But the volume of coating was so minute, slight difference exists between each needle. Conclusion : Above results indicate that the bee venom acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

  14. 72 - 80_Aminu_HPLC1

    African Journals Online (AJOL)

    pc

    HPLC, Gymnema sylvestre, carbohydrate hydrolyzing enzymes, lipid a chronic .... Method. Test for Tannins and Flavonoids was by. Trease and Evans (2002). Soluble Starch ... Fenton reaction was quantified using 2- deoxyribose oxidative ...

  15. Principal Component and Cluster Analysis for determining diversification of bottom morphology based on bathymetric profiles from Brepollen (Hornsund, Spitsbergen* The project was partly supported by The Polish Ministry of Sciences and Higher Education Grant No. N N525 350038.

    Directory of Open Access Journals (Sweden)

    Mateusz Moskalik

    2014-01-01

    Full Text Available Navigation charts of the post-glacial regions of Arctic fjords tend not to cover regions from which glaciers have retreated. Whilst research vessels can make detailed bathymetric models using multibeam echosounders, they are often too large to enter such areas. To map these regions therefore requires smaller boats carrying single beam echosounders. To obtain morphology models of equivalent quality to those generated using multibeam echosounders, new ways of processing data from single beam echosounders have to be found. The results and comprehensive analysis of such measurements conducted in Brepollen (Hornsund, Spitsbergen are presented in this article. The morphological differentiation of the seafloor was determined by calculating statistical, spectral and wavelet transformation, fractal and median filtration parameters of segments of bathymetric profiles. This set of parameters constituted the input for Principal Component Analysis and then in the form of Principal Components for the Cluster Analysis. As a result of this procedure, three morphological classes are proposed for Brepollen: (i steep slopes (southern Brepollen, (ii flat bottoms (central Brepollen and gentle slopes (the Storebreen glacier valley and the southern part of the Hornbreen glacier valley, (iii the morphologically most diverse region (the central Storebreen valley, the northern part of the Hornbreen glacier valley and the north-eastern part of central Brepollen.

  16. Profile of red blood cell morphologies and causes of anaemia among pregnant women at first clinic visit in the mount Cameroon area: a prospective cross sectional study

    OpenAIRE

    Anchang-Kimbi, Judith K.; Nkweti, Vera Ngenwie; Ntonifor, Helen Ngum; Apinjoh, Tobias O.; Chi, Hanesh Fru; Tata, Rolland Bantar; Achidi, Eric Akum

    2017-01-01

    Objective Anaemia is a serious problem in pregnancy in malaria-endemic countries. This study investigated red cell morphologies and possible causes of anaemia among pregnant women at first clinic visit. Venous blood samples from consented women were used to determine haemoglobin (Hb) levels, mean corpuscular volume (MCV) and mean corpuscular haemoglobin (MCH) using an automated haematology analyzer. Malaria parasitaemia was diagnosed by microscopy. Definitions were as follows: anaemia (Hb 

  17. Environmentally evaluated HPLC-ELSD method to monitor enzymatic synthesis of a non-ionic surfactant.

    Science.gov (United States)

    Gaber, Yasser; Akerman, Cecilia Orellana; Hatti-Kaul, Rajni

    2014-01-01

    N-Lauroyl-N-methylglucamide is a biodegradable surfactant derived from renewable resources. In an earlier study, we presented an enzymatic solvent-free method for synthesis of this compound. In the present report, the HPLC method developed to follow the reaction between lauric acid/methyl laurate and N-methyl glucamine (MEG) and its environmental assessment are described. Use of ultraviolet (UV) absorption or refractive index (RI) detectors did not allow the detection of N-methyl glucamine (MEG). With Evaporative light scattering detector ELSD, it was possible to apply a gradient elution, and detect MEG with a limit of detection, LOD = 0.12 μg. A good separation of the peaks: MEG, lauric acid, product (amide) and by-product (amide-ester) was achieved with the gradient program with a run time of 40 min. The setting of ELSD detector was optimized using methyl laurate as the analyte. LC-MS/MS was used to confirm the amide and amide-ester peaks. We evaluated the greenness of the developed method using the freely available software HPLC-Environmental Assessment Tool (HPLC-EAT) and the method got a scoring of 73 HPLC-EAT units, implying that the analytical procedure was more environmentally benign compared to some other methods reported in literature whose HPLC-EAT values scored up to 182. Use of ELSD detector allowed the detection and quantification of the substrates and the reaction products of enzymatic synthesis of the surfactant, N-lauroyl-N-methylglucamide. The developed HPLC method has acceptable environmental profile based on HPLC-EAT evaluation.

  18. On-line radioactivity detector for HPLC

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1986-01-01

    Over the last ten years the technique of high performance liquid chromotography (HPLC) has become extensively employed for the separation and quantitation of various biological, organic, and inorganic substances. The use of HPLC for the separation of various metabolic compounds has become routine. The major problem of analyzing the metabolism process is that the quantitation is accomplished by the use of radioactive substrates. Until recently the only method to quantitate these radioactive compounds eluting from the HPLC was by collecting fractions at preset times, removing aliquots and quantitating in a liquid scintillation counter. Once the radioactivity present in each fraction was determined, the results were plotted on a graph and the area of each of the radioactive peaks was determined. This entire process required from 3-20 hours. The introduction of the flow through radioactivity detector enable the investigator to directly quantitate the radioactive peaks as they elute from the HPLC in real time and at about one-tenth the original cost of the previous methods. The detection limits of this technique are dependent on the residence time of the sample in the flow cell and the type of flow cell used for the analysis. Using a 2.5 ml liquid flow cell, (mixing with liquid scintillation solution), base line resolution can be obtained for peaks 1.5 minutes apart, and a sensitivity of 70 dpm for tritium and 30 dpm for carbon-14 can be achieved

  19. An Inexpensive Digital Gradient Controller for HPLC.

    Science.gov (United States)

    Brady, James E.; Carr, Peter W.

    1983-01-01

    Use of gradient elution techniques in high performance liquid chromatography (HPLC) is often essential for direct separation of complex mixtures. Since most commercial controllers have features that are of marginal value for instructional purposes, a low-cost controller capable of illustrating essential features of gradient elution was developed.…

  20. Determination of anthocyanins from camu-camu (Myrciaria dubia) by HPLC-PDA, HPLC-MS, and NMR.

    Science.gov (United States)

    Zanatta, Cinthia Fernanda; Cuevas, Elyana; Bobbio, Florinda O; Winterhalter, Peter; Mercadante, Adriana Z

    2005-11-30

    Camu-camu [Myrciaria dubia (HBK) McVaugh] is a small fruit native to the Amazonian rain forest. Its anthocyanin profile has now been investigated for the first time. Fruits from two different regions of the São Paulo state, Brazil, were analyzed. The major anthocyanins were isolated by high-speed countercurrent chromatography. HPLC-PDA, HPLC-MS/MS, and 1H NMR were used to confirm the identity of the main anthocyanins of camu-camu. Cyanidin-3-glucoside was identified as the major pigment in the fruits from both regions, representing 89.5% in the fruits produced in Iguape and 88.0% in those from Mirandópolis, followed by the delphinidin-3-glucoside, ranging between 4.2 and 5.1%, respectively. Higher total anthocyanin contents were detected in the fruits from Iguape (54.0 +/- 25.9 mg/100 g) compared to those from Mirandópolis (30.3 +/- 6.8 mg/100 g), most likely because of the lower temperatures in the Iguape region.

  1. Adenoid cystic carcinomas of the salivary gland, lacrimal gland, and breast are morphologically and genetically similar but have distinct microRNA expression profiles

    DEFF Research Database (Denmark)

    Andreasen, Simon; Tan, Qihua; Agander, Tina Klitmøller

    2018-01-01

    Adenoid cystic carcinoma is among the most frequent malignancies in the salivary and lacrimal glands and has a grave prognosis characterized by frequent local recurrences, distant metastases, and tumor-related mortality. Conversely, adenoid cystic carcinoma of the breast is a rare type of triple......-negative (estrogen and progesterone receptor, HER2) and basal-like carcinoma, which in contrast to other triple-negative and basal-like breast carcinomas has a very favorable prognosis. Irrespective of site, adenoid cystic carcinoma is characterized by gene fusions involving MYB, MYBL1, and NFIB, and the reason...... for the different clinical outcomes is unknown. In order to identify the molecular mechanisms underlying the discrepancy in clinical outcome, we characterized the phenotypic profiles, pattern of gene rearrangements, and global microRNA expression profiles of 64 salivary gland, 9 lacrimal gland, and 11 breast...

  2. Adenoid cystic carcinomas of the salivary gland, lacrimal gland, and breast are morphologically and genetically similar but have distinct microRNA expression profiles.

    Science.gov (United States)

    Andreasen, Simon; Tan, Qihua; Agander, Tina Klitmøller; Steiner, Petr; Bjørndal, Kristine; Høgdall, Estrid; Larsen, Stine Rosenkilde; Erentaite, Daiva; Olsen, Caroline Holkmann; Ulhøi, Benedicte Parm; von Holstein, Sarah Linéa; Wessel, Irene; Heegaard, Steffen; Homøe, Preben

    2018-02-21

    Adenoid cystic carcinoma is among the most frequent malignancies in the salivary and lacrimal glands and has a grave prognosis characterized by frequent local recurrences, distant metastases, and tumor-related mortality. Conversely, adenoid cystic carcinoma of the breast is a rare type of triple-negative (estrogen and progesterone receptor, HER2) and basal-like carcinoma, which in contrast to other triple-negative and basal-like breast carcinomas has a very favorable prognosis. Irrespective of site, adenoid cystic carcinoma is characterized by gene fusions involving MYB, MYBL1, and NFIB, and the reason for the different clinical outcomes is unknown. In order to identify the molecular mechanisms underlying the discrepancy in clinical outcome, we characterized the phenotypic profiles, pattern of gene rearrangements, and global microRNA expression profiles of 64 salivary gland, 9 lacrimal gland, and 11 breast adenoid cystic carcinomas. All breast and lacrimal gland adenoid cystic carcinomas had triple-negative and basal-like phenotypes, while salivary gland tumors were indeterminate in 13% of cases. Aberrations in MYB and/or NFIB were found in the majority of cases in all three locations, whereas MYBL1 involvement was restricted to tumors in the salivary gland. Global microRNA expression profiling separated salivary and lacrimal gland adenoid cystic carcinoma from their respective normal glands but could not distinguish normal breast adenoid cystic carcinoma from normal breast tissue. Hierarchical clustering separated adenoid cystic carcinomas of salivary gland origin from those of the breast and placed lacrimal gland carcinomas in between these. Functional annotation of the microRNAs differentially expressed between salivary gland and breast adenoid cystic carcinoma showed these as regulating genes involved in metabolism, signal transduction, and genes involved in other cancers. In conclusion, microRNA dysregulation is the first class of molecules separating adenoid

  3. The impact of mild hypercholesterolemia on glycemic and hormonal profiles, menstrual characteristics and the ovarian morphology of women with polycystic ovarian syndrome.

    Science.gov (United States)

    Pergialiotis, Vasilios; Trakakis, Eftihios; Chrelias, Charalampos; Papantoniou, Nikolaos; Hatziagelaki, Erifili

    2018-03-29

    Background The severity of polycystic ovarian syndrome (PCOS) has been clearly associated with insulin resistance, obesity and metabolic syndrome. The purpose of the present cross-sectional study is to investigate whether mild hypercholesterolemia alters the biochemical and clinical profile of PCOS patients. Methods Our study is based on a prospectively collected population of women of reproductive age who were diagnosed with PCOS according to the definition of the Rotterdam European Society of Human Reproduction and Embryology/American Society for Reproductive Medicine (ASRM/ESHRE) criteria. For the correlation analysis we used the non-parametric Spearman's rank correlation coefficient. Partial correlation was also performed to control for potential confounders observed in the univariate analysis. Results Overall, 235 patients were included. Their mean age ranged between 14 and 45 years old and the body mass index (BMI) between 17 and 54. Women with mild hypercholesterolemia had a higher BMI and their fasting insulin was increased as well as indices of insulin resistance [Homeostatic model assessment (HOMA), quantitative insulin sensitivity check index (QUICKI), Matsuda index] compared to women with PCOS with normal cholesterol levels. Correlation statistics suggested that the effect of serum lipids on the hormonal profile of patients was weak. Both low-density lipoprotein (LDL) and high-density lipoprotein (HDL) exerted a significant mild negative correlation to glucose and insulin. However, after controlling the results for BMI and age (the two variables that were found significantly different in the univariate analysis) we observed that this effect was non-significant. Conclusion Mild hypercholesterolemia does not affect the hormonal profile of patients with PCOS; hence, to date, there is no evidence to suggest its treatment for the correction of menstrual and hormonal abnormalities in PCOS women.

  4. Re-purification of labelled ferritin antigen with HPLC

    International Nuclear Information System (INIS)

    Zhang Haoyi; Jin Lichun

    2002-01-01

    Objective: To improve the quality of long-term stored labelled ferritin antigen with HPLC. Methods: The antigen was analyzed and purified with HPLC and again analyzed with RIA afterwards. Results: Ferritin antigen underwent significant polymerization after long-term (aggregation) storage. After re-purification with HPLC, its immuno-activity and labelled specific radioactivity were both significantly improved. Conclusion: Quality of stored ferritin RIA kit could be greatly improved after re-purification with HPLC

  5. Constraining dark matter halo profiles and galaxy formation models using spiral arm morphology. II. Dark and stellar mass concentrations for 13 nearby face-on galaxies

    International Nuclear Information System (INIS)

    Seigar, Marc S.; Davis, Benjamin L.; Berrier, Joel; Kennefick, Daniel

    2014-01-01

    We investigate the use of spiral arm pitch angles as a probe of disk galaxy mass profiles. We confirm our previous result that spiral arm pitch angles (P) are well correlated with the rate of shear (S) in disk galaxy rotation curves. We use this correlation to argue that imaging data alone can provide a powerful probe of galactic mass distributions out to large look-back times. We then use a sample of 13 galaxies, with Spitzer 3.6 μm imaging data and observed Hα rotation curves, to demonstrate how an inferred shear rate coupled with a bulge-disk decomposition model and a Tully-Fisher-derived velocity normalization can be used to place constraints on a galaxy's baryon fraction and dark matter halo profile. Finally, we show that there appears to be a trend (albeit a weak correlation) between spiral arm pitch angle and halo concentration. We discuss implications for the suggested link between supermassive black hole (SMBH) mass and dark halo concentration, using pitch angle as a proxy for SMBH mass.

  6. Measurement of menadione in urine by HPLC.

    Science.gov (United States)

    Al Rajabi, Ala; Peterson, James; Choi, Sang-Woon; Suttie, John; Barakat, Susan; Booth, Sarah L

    2010-09-15

    Menadione is a metabolite of vitamin K that is excreted in urine. A high performance liquid chromatography (HPLC) method using a C(30) column, post-column zinc reduction and fluorescence detection was developed to measure urinary menadione. The mobile phase was composed of 95% methanol with 0.55% aqueous solution and 5% DI H(2)O. Menaquinone-2 (MK-2) was used as an internal standard. The standard calibration curve was linear with a correlation coefficient (R(2)) of 0.999 for both menadione and MK-2. The lower limit of quantification (LLOQ) was 0.3pmole menadione/mL urine. Sample preparation involved hydrolysis of menadiol conjugates and oxidizing the released menadiol to menadione. Using this method, urinary menadione was shown to increase in response to 3 years of phylloquinone supplementation. This HPLC method is a sensitive and reproducible way to detect menadione in urine. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  7. [Spectrophotometric and HPLC evaluation of ceftazidime stability].

    Science.gov (United States)

    Palade, B; Cioroiu, B; Lazăr, Doina; Corciovă, Andreia; Lazăr, M I

    2010-01-01

    In this paper we followed up the stability of ceftazidime, raw material used in drug industry. Matherials and methods: We used three spectrophotometric methods based on ceftazidime property to form complexes with p-chloranilic acid (ac. p-CA), 3-methylbenzothiazolin-2-on hydrazone (MBTH) and N-(1-naphtil) etilendiamine (NEDA) and a chromatographic method (HPLC). Our results revealed that the substances analyzed maintained minimum content allowable.

  8. Retinoid quantification by HPLC/MS(n)

    Science.gov (United States)

    McCaffery, Peter; Evans, James; Koul, Omanand; Volpert, Amy; Reid, Kevin; Ullman, M. David

    2002-01-01

    Retinoic acid (RA) mediates most of the biological effects of vitamin A that are essential for vertebrate survival. It acts through binding to receptors that belong to the nuclear receptor transcription factor superfamily (Mangelsdorf et al. 1994). It is also a highly potent vertebrate teratogen. To determine the function and effects of endogenous and exogenous RA, it is important to have a highly specific, sensitive, accurate, and precise analytical procedure. Current analyses of RA and other retinoids are labor intensive, of poor sensitivity, have limited specificity, or require compatibility with RA reporter cell lines (Chen et al. 1995. BIOCHEM: Pharmacol. 50: 1257-1264; Creech Kraft et al. 1994. BIOCHEM: J. 301: 111-119; Lanvers et al. 1996. J. Chromatogr. B Biomed. Appl. 685: 233-240; Maden et al. 1998. DEVELOPMENT: 125: 4133-4144; Wagner et al. 1992. DEVELOPMENT: 116: 55-66). This paper describes an HPLC/mass spectrometry/mass spectrometry product ion scan (HPLC/MS(n)) procedure for the analysis of retinoids that employs atmospheric pressure chemical ionization MS. The retinoids are separated by normal-phase column chromatography with a linear hexane-isopropanol-dioxane gradient. Each retinoid is detected by a unique series of MS(n) functions set at optimal collision-induced dissociation energy (30% to 32%) for all MS(n) steps. The scan events are divided into three segments, based on HPLC elution order, to maximize the mass spectrometer duty cycle. The all-trans, 9-cis, and 13-cis RA isomers are separated, if desired, by an isocratic hexane-dioxane-isopropanol mobile phase. This paper describes an HPLC/MS(n) procedure possessing high sensitivity and specificity for retinoids.

  9. Abnormal morphology of the penis in male rats exposed neonatally to diethylstilbestrol is associated with altered profile of estrogen receptor-alpha protein, but not of androgen receptor protein: a developmental and immunocytochemical study.

    Science.gov (United States)

    Goyal, H O; Braden, T D; Williams, C S; Dalvi, P; Mansour, M M; Mansour, M; Williams, J W; Bartol, F F; Wiley, A A; Birch, L; Prins, G S

    2004-05-01

    Objectives of the study were to determine developmental changes in morphology and expression of androgen receptor (AR) and estrogen receptor (ER)alpha in the body of the rat penis exposed neonatally to diethylstilbestrol (DES). Male pups received DES at a dose of 10 microg per rat on alternate days from Postnatal Day 2 to Postnatal Day 12. Controls received olive oil vehicle only. Tissue samples were collected on Days 18 (prepuberty), 41 (puberty), and 120 (adult) of age. DES-induced abnormalities were evident at 18 days of age and included smaller, lighter, and thinner penis, loss of cavernous spaces and associated smooth muscle cells, and increased deposition of fat cells in the corpora cavernosa penis. Fat cells virtually filled the entire area of the corpora cavernosa at puberty and adulthood. Plasma testosterone (T) was reduced to an undetectable level, while LH was unaltered in all treated groups. AR-positive cells were ubiquitous and their profile (incidence and staining intensity) did not differ between control and treated rats of the respective age groups. Conversely, ERalpha-positive cells were limited to the stroma of corpus spongiosus in all age groups of both control and treated rats, but the expression in treated rats at 18 days was up-regulated in stromal cells of corpora cavernosa, coincident with the presence of morphological abnormalities. Hence, this study reports for the first time DES-induced developmental, morphological abnormalities in the body of the penis and suggests that these abnormalities may have resulted from decreased T and/or overexpression of ERalpha.

  10. An Investigation Into HPLC Data Quality Problems

    Science.gov (United States)

    Hooker, Stanford B.; VanHeukelem, Laurie

    2011-01-01

    This report summarizes the analyses and results produced by a five-member investigative team of Government, university, and industry experts, established by NASA HQ. The team examined data quality problems associated with high performance liquid chromatography (HPLC) analyses of pigment concentrations in seawater samples produced by the San Diego State University (SDSU) Center for Hydro-Optics and Remote Sensing (CHORS). This report shows CHORS did not validate the methods used before placing them into service to analyze field samples for NASA principal investigators (PIs), even though the HPLC literature contained easily accessible method validation procedures, and the importance of implementing them, more than a decade ago. In addition, there were so many sources of significant variance in the CHORS methodologies, that the HPLC system rarely operated within performance criteria capable of producing the requisite data quality. It is the recommendation of the investigative team to a) not correct the data, b) make all the data that was temporarily sequestered available for scientific use, and c) label the affected data with an appropriate warning, e.g., "These data are not validated and should not be used as the sole basis for a scientific result, conclusion, or hypothesis--independent corroborating evidence is required."

  11. Morphological demosaicking

    Science.gov (United States)

    Quan, Shuxue

    2009-02-01

    Bayer patterns, in which a single value of red, green or blue is available for each pixel, are widely used in digital color cameras. The reconstruction of the full color image is often referred to as demosaicking. This paper introduced a new approach - morphological demosaicking. The approach is based on strong edge directionality selection and interpolation, followed by morphological operations to refine edge directionality selection and reduce color aliasing. Finally performance evaluation and examples of color artifacts reduction are shown.

  12. The Probiotic Mixture VSL#3 Alters the Morphology and Secretion Profile of Both Polarized and Unpolarized Human Macrophages in a Polarization-Dependent Manner

    Science.gov (United States)

    Isidro, Raymond A.; Bonilla, Fernando J.; Pagan, Hendrick; Cruz, Myrella L.; Lopez, Pablo; Godoy, Lenin; Hernandez, Siomara; Loucil-Alicea, Raisa Y.; Rivera-Amill, Vanessa; Yamamura, Yasuhiro; Isidro, Angel A.; Appleyard, Caroline B.

    2014-01-01

    Background Patients with Inflammatory Bowel Disease (IBD), most commonly Crohn’s disease (CD) or ulcerative colitis (UC), suffer from chronic intestinal inflammation of unknown etiology. Increased proinflammatory macrophages (M1) have been documented in tissue from patients with CD. Anti-inflammatory macrophages (M2) may play a role in UC given the preponderance of Th2 cytokines in this variant of IBD. Animal and clinical studies have shown that the probiotic VSL#3 can ameliorate signs and symptoms of IBD. Although animal data suggests a modulatory effect on macrophage phenotype, the effect of VSL#3 on human macrophages remains unknown. Objective To determine the effect of the probiotic VSL#3 on the phenotype of polarized (M1/M2) and unpolarized (MΦ) human macrophages. Methods Human monocyte-derived macrophages, generated by culturing monocytes with M-CSF, were left unpolarized or were polarized towards an M1 or an M2 phenotype by culture with LPS and IFN-γ or IL-4, respectively, and were then cultured in the presence or absence of VSL#3 for 3 days. Changes in macrophage morphology were assessed. Cytokine and chemokine levels in supernatants were determined by multiplex assay. Results VSL#3 decreased the granuloma-like aggregates of M1 macrophages, increased fibroblast-like M2 macrophages, and decreased fibroblast-like MΦ macrophages. VSL#3 increased the secretion of IL-1β, IL-6, IL-10, and G-CSF by M1, M2, and MΦ macrophages. VSL#3 exposure maintained the proinflammatory phenotype of M1 macrophages, sustaining IL-12 secretion, increasing IL-23 secretion, and decreasing MDC secretion. Both VSL#3-treated M2 and MΦ macrophages secreted higher levels of anti-inflammatory and pro-healing factors such as IL-1Ra, IL-13, EGF, FGF-2, TGF-α, and VEGF, as well as proinflammatory cytokines, including IL-12 and TNF-α. Conclusion Under our experimental conditions VSL#3 induced a mixed proinflammatory and anti-inflammatory phenotype in polarized and unpolarized

  13. Morphological observation, RNA-Seq quantification, and expression profiling: novel insight into grafting-responsive carotenoid biosynthesis in watermelon grafted onto pumpkin rootstock.

    Science.gov (United States)

    Liu, Guang; Yang, Xingping; Xu, Jinhua; Zhang, Man; Hou, Qian; Zhu, Lingli; Huang, Ying; Xiong, Aisheng

    2017-03-01

    Watermelon is an important and economical horticultural crop in China, where ~20% of the plants are grafted. The development of grafted watermelon fruit involves a diverse range of gene interactions that results in dynamic changes in fruit. However, the molecular mechanisms underlying grafting-induced fruit quality change are unclear. In the present study, we measured the lycopene content by high-performance liquid chromatography and used RNA-Seq (quantification) to perform a genome-wide transcript analysis of fruits from watermelon grafted onto pumpkin rootstock (pumpkin-grafted watermelon, PGW), self-grafted watermelon (SGW), and non-grafted watermelon (NGW). The results showed variation in the lycopene content in the flesh of PGW fruits, first increasing and then decreasing in the four stages, which was different from the trend in the flesh of NGW and SGW fruits. The transcriptome profiling data provided new information on the grafting-induced gene regulation of lycopene biosynthesis during fruit growth and development. The expression levels of 33 genes from 8 gene families (GGPS, PSY, PDS, ZDS, CRTISO, LCYb, LCYe, and CHY) related to lycopene biosynthesis, which play critical roles in fruit coloration and contribute significantly to fruit phytonutrient values, were monitored during the four periods of fruit development in watermelon. Compared with those of NGW and SGW, 14 genes were differentially expressed in PGW during fruit development, suggesting that these genes possibly help to mediate lycopene biosynthesis in grafted watermelon fruit. Our work provides some novel insights into grafting-responsive carotenoid metabolism and its potential roles during PGW fruit development and ripening. © The Author 2016. Published by Oxford University Press on behalf of the Institute of Biochemistry and Cell Biology, Shanghai Institutes for Biological Sciences, Chinese Academy of Sciences. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  14. Ionisation constants of radiopharmaceuticals by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Stylli, C.G.; Theobald, A.E.

    It has long been recognised that the pKsub(a) of drugs and radiopharmaceuticals is an important determinant of their biological distribution. In this study an HPLC method for pKa measurement has been developed for radiotracers. It has been validated with several amines and used to estimate the pKsub(a) values of some Tc-99m PnAO complexes by observing the change in chromatographic retention with change in mobile phase pH. The pKsub(a) values were estimated from the data by three methods: derivative analysis, quadratic regression, and the Henderson - Hasselbalch equation.

  15. Ionisation constants of radiopharmaceuticals by HPLC

    International Nuclear Information System (INIS)

    Stylli, C.G.; Theobald, A.E.

    1986-01-01

    It has long been recognised that the pKsub(a) of drugs and radiopharmaceuticals is an important determinant of their biological distribution. In this study an HPLC method for pKa measurement has been developed for radiotracers. It has been validated with several amines and used to estimate the pKsub(a) values of some Tc-99m PnAO complexes by observing the change in chromatographic retention with change in mobile phase pH. The pKsub(a) values were estimated from the data by three methods: derivative analysis, quadratic regression, and the Henderson - Hasselbalch equation. (author)

  16. The metabolism of 4-bromoaniline in the bile-cannulated rat: application of ICPMS (79/81Br), HPLC-ICPMS & HPLC-oaTOFMS

    OpenAIRE

    Duckett, Catherine; McCullagh, Michael; Smith, Christopher; Wilson, Ian D

    2015-01-01

    ? 2015 The Author(s). Published by Taylor & Francis.1. An excretion balance study was performed following i.p. administration of 4-bromoaniline (50 mg kg-1) to bile-cannulated rats, using bromine-detected (79/81Br) ICPMS for quantification. Approximately 90% of the dose was recovered in urine (68.9 ? 3.6%) and bile (21.4 ? 1.4%) by 48 h post-administration.2. HPLC-ICPMS (79/81Br) was used to selectively detect and profile the major urinary and biliary-excreted metabolites and determined that ...

  17. HPLC determination of caffeine in coffee beverage

    Science.gov (United States)

    Fajara, B. E. P.; Susanti, H.

    2017-11-01

    Coffee is the second largest beverage which is consumed by people in the world, besides the water. One of the compounds which contained in coffee is caffeine. Caffeine has the pharmacological effect such as stimulating the central nervous system. The purpose of this study is to determine the level of caffeine in coffee beverages with HPLC method. Three branded coffee beverages which include in 3 of Top Brand Index 2016 Phase 2 were used as samples. Qualitative analysis was performed by Parry method, Dragendorff reagent, and comparing the retention time between sample and caffeine standard. Quantitative analysis was done by HPLC method with methanol-water (95:5v/v) as mobile phase and ODS as stationary phasewith flow rate 1 mL/min and UV 272 nm as the detector. The level of caffeine data was statistically analyzed using Anova at 95% confidence level. The Qualitative analysis showed that the three samples contained caffeine. The average of caffeine level in coffee bottles of X, Y, and Z were 138.048 mg/bottle, 109.699 mg/bottle, and 147.669 mg/bottle, respectively. The caffeine content of the three coffee beverage samples are statistically different (pcoffee beverage samples were not meet the requirements set by the Indonesian Standard Agency of 50 mg/serving.

  18. Radio-activity detectors in HPLC

    International Nuclear Information System (INIS)

    Kremers, H.D.

    1984-01-01

    Two different approaches were adopted to put the eluate from the HPLC into contact with the scintillator, i.e. a homogeneous and a heterogeneous system. In the heterogeneous system, the eluate runs directly through a cell filled with a fine-grain solid scintillator. In the homogeneous system, a liquid scintillator is admixed to the eluate or to a proportion of the eluate before flowing through the measurement cell. Both systems are contrasted with the fractionation method according to the criterias of handling, rapidity of analysis and facility cost. On-line detection of radio-activity will be easily settled for when comparing its investment cost with those of materials consumed in fractionation. A device prepared for scintillator admixture contains an integrated scintillator pump and a mixer but is suitable for application of solid scintillator cells, too. Such a system features a wider range of practical applications than a device exclusively designed for the heterogeneous system. A further asset of the detectors in the fact that they are adapted in their performance to up-to-date HPLC facilities in terms of speed and resolution. (orig./HP) [de

  19. [Determination of the profiles of secondary metabolites characteristic of Alternaria strains isolated from tomato].

    Science.gov (United States)

    Benavidez Rozo, Martha Elizabeth; Patriarca, Andrea; Cabrera, Gabriela; Fernández Pinto, Virginia E

    2014-01-01

    Many Alternaria species have been studied for their ability to produce bioactive secondary metabolites, such as tentoxin (TEN), some of which have toxic properties. The main food contaminant toxins are tenuazonic acid, alternariol (AOH), alternariol monomethyl ether (AME), altenuene, and altertoxins i, ii and iii. To determine the profiles of secondary metabolites characteristic of Alternaria strains isolated from tomato for their chemotaxonomic classification. The profiles of secondary metabolites were determined by HPLC MS. The Alternaria isolates obtained from spoiled tomatoes belong, according to their morphological characteristics, to the species groups Alternaria alternata, Alternaria tenuissima and Alternaria arborescens, with A. tenuissima being the most frequent. The most frequent profiles of secondary metabolites belonging to the species groups A. alternata (AOH, AME, TEN), A. tenuissima (AOH, AME, TEN, tenuazonic acid) and A. arborescens (AOH, AME, TEN, tenuazonic acid) were determined, with some isolates of the latter being able to synthesize AAL toxins. Secondary metabolite profiles are a useful tool for the differentiation of small spored Alternaria isolates not easily identifiable by their morphological characteristics. Copyright © 2013 Revista Iberoamericana de Micología. Published by Elsevier Espana. All rights reserved.

  20. Computer-aided method for identification of major flavone/flavonol glycosides by high-performance liquid chromatography-diode array detection-tandem mass spectrometry (HPLC-DAD-MS/MS).

    Science.gov (United States)

    Wang, Zhengfang; Lin, Longze; Harnly, James M; Harrington, Peter de B; Chen, Pei

    2014-11-01

    A new computational tool is proposed here for tentatively identifying major (UV quantifiable) flavone/flavonol glycoside peaks of high performance liquid chromatogram (HPLC)-diode array detection (DAD)-tandem mass spectrometry (MS/MS) profiles based on a MATLAB-based script implementing an in-house algorithm. The HPLC-DAD-MS/MS profiles of red onion, Chinese lettuce, carrot leaf, and celery seed extracts were analyzed by the proposed computer-aided screening method for identifying possible flavone/flavonol glycoside peaks from the HPLC-UV and MS total ion current (TIC) chromatograms. The number of identified flavone/flavonol glycoside peaks of the HPLC-UV chromatograms is four, four, six, and nine for red onion, Chinese lettuce, carrot leaf, and celery seed, respectively. These results have been validated by human(s) experts. For the batch processing of nine HPLC-DAD-MS/MS profiles of celery seed extract, the entire script execution time was within 15 s while manual calculation of only one HPLC-DAD-MS/MS profile by a flavonoid expert could take hours. Therefore, this MATLAB-based screening method is able to facilitate the HPLC-DAD-MS/MS analysis of flavone/flavonol glycosides in plants to a large extent.

  1. Electrochemical Detectors in HPLC and Ion Chromatography.

    Science.gov (United States)

    Horvai, George; Pungor, ErnÕ

    1989-01-01

    Back in 1952, the renowned Polish electrochemist Wiktor Kemula introduced chromato-polarography, 1 i.e., polaro-graphic detection for liquid chromatography. This technique continued to develop slowly until the early 1970s (for a review see Reference 2) when modem high-performance liquid chromatography (HPLC) emerged. This new, highly efficient chromatographc method could only be. used with detectors ensuring low dispersion. It was not easy to modify the dropping mercury electrode cells to satisfy this requirement. However, at the same time, electroanalytical chemists, who already had much experience in using carbon-based electrodes for oxidative detection in flow analysis, put forward the idea of oxidative amperometric detection in liquid chromatography. 3,4 In this technique, solid or quasi-solid (paste) electrodes were used and this made possible the construction of miniaturized cells with just a few microliter volume.

  2. Analysis of xanthophylls in corn by HPLC.

    Science.gov (United States)

    Moros, E E; Darnoko, D; Cheryan, M; Perkins, E G; Jerrell, J

    2002-10-09

    An HPLC method was developed using the C-30 carotenoid column to separate and identify the major xanthophylls in corn (lutein, zeaxanthin, and beta-cryptoxanthin). A photodiode array detector and a mobile phase consisting of methyl tert-butyl ether/methanol/water was used. All three xanthophylls eluted in less than 25 min. Yellow dent corn had a total xanthophyll content of 21.97 microg/g with lutein content of 15.7 microg/g, zeaxanthin content of 5.7 microg/g, and beta-cryptoxanthin of 0.57 microg/g. Commercial corn gluten meal had a 7 times higher concentration of xanthophylls (145 microg/g), and deoiled corn contained 18 microg/g, indicating that the xanthophylls are probably bound to the zein fraction of corn proteins.

  3. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    Science.gov (United States)

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  4. A novel approach for the quantitation of carbohydrates in mash, wort, and beer with RP-HPLC using 1-naphthylamine for precolumn derivatization.

    Science.gov (United States)

    Rakete, Stefan; Glomb, Marcus A

    2013-04-24

    A novel universal method for the determination of reducing mono-, di-, and oligosaccharides in complex matrices on RP-HPLC using 1-naphthylamine for precolumn derivatization with sodium cyanoborhydride was established to study changes in the carbohydrate profile during beer brewing. Fluorescence and mass spectrometric detection enabled very sensitive analyses of beer-relevant carbohydrates. Mass spectrometry additionally allowed the identification of the molecular weight and thereby the degree of polymerization of unknown carbohydrates. Thus, carbohydrates with up to 16 glucose units were detected. Comparison demonstrated that the novel method was superior to fluorophore-assisted carbohydrate electrophoresis (FACE). The results proved the HPLC method clearly to be more powerful in regard to sensitivity and resolution. Analogous to FACE, this method was designated fluorophore-assisted carbohydrate HPLC (FAC-HPLC).

  5. HPLC-ESR techniques for detection of complex trapped radicals

    International Nuclear Information System (INIS)

    Tu Tiecheng; Dong Jirong; Lin Nianyun; Xie Leidong; Liu Rengzhong

    1992-01-01

    High performance liquid chromatography (HPLC) and ESR combined examination of radical species is an advanced techniques for separation and identification of complex radical species. At SRCL, Waters 990 HPLC has been used to separate the complex trapped radicals and Varian E-112 ESR spectrometer to record the spectra of single trapped radicals after HPLC separation. The advantages of the combined techniques are described as bellow: HPLC is used to separate the long-lived complex trapped radicals derived from reaction of short-lived radicals with spin trap. ESR spectra from single trapped radicals, obtained following HPLC separation of complex trapped radicals, are recorded one by one and well resolved. The structures of short-lived radicals can be inferred from the ESR spectra of the long-lived trapped radicals

  6. Fast algorithm for Morphological Filters

    International Nuclear Information System (INIS)

    Lou Shan; Jiang Xiangqian; Scott, Paul J

    2011-01-01

    In surface metrology, morphological filters, which evolved from the envelope filtering system (E-system) work well for functional prediction of surface finish in the analysis of surfaces in contact. The naive algorithms are time consuming, especially for areal data, and not generally adopted in real practice. A fast algorithm is proposed based on the alpha shape. The hull obtained by rolling the alpha ball is equivalent to the morphological opening/closing in theory. The algorithm depends on Delaunay triangulation with time complexity O(nlogn). In comparison to the naive algorithms it generates the opening and closing envelope without combining dilation and erosion. Edge distortion is corrected by reflective padding for open profiles/surfaces. Spikes in the sample data are detected and points interpolated to prevent singularities. The proposed algorithm works well both for morphological profile and area filters. Examples are presented to demonstrate the validity and superiority on efficiency of this algorithm over the naive algorithm.

  7. Development and Application of Multidimensional HPLC Mapping Method for O-linked Oligosaccharides

    Directory of Open Access Journals (Sweden)

    Koichi Kato

    2011-12-01

    Full Text Available Glycosylation improves the solubility and stability of proteins, contributes to the structural integrity of protein functional sites, and mediates biomolecular recognition events involved in cell-cell communications and viral infections. The first step toward understanding the molecular mechanisms underlying these carbohydrate functionalities is a detailed characterization of glycan structures. Recently developed glycomic approaches have enabled comprehensive analyses of N-glycosylation profiles in a quantitative manner. However, there are only a few reports describing detailed O-glycosylation profiles primarily because of the lack of a widespread standard method to identify O-glycan structures. Here, we developed an HPLC mapping method for detailed identification of O-glycans including neutral, sialylated, and sulfated oligosaccharides. Furthermore, using this method, we were able to quantitatively identify isomeric products from an in vitro reaction catalyzed by N-acetylglucosamine-6O-sulfotransferases and obtain O-glycosylation profiles of serum IgA as a model glycoprotein.

  8. A study of the red clover extract trinovin by ESR HPLC/MS and UVS

    International Nuclear Information System (INIS)

    Troup, G.; Hutton, D.; Hunter, C.; Hewitt, D.; Mulinacci, N.; Romani, A.; Pinelli, P.; Mancini, P.

    1999-01-01

    Full text: Trinovin is an extract of red clover, recently released on the dietary supplement market. It is recommended for 'Men's Health', because it contains the phenolics (isoflavones) genistein, biochanin, daidzein and formononetin, said to act as 'phytoestrogens', and is therefore a possible help in prostate gland problems. An Electron Spin Resonance (ESR) study (∼9.1Ghz, room temperature) revealed at least 3 different free radical lines, one with hyperfine structure, consistent with the listed molecules. Accordingly, HPLC/DAD (High Performance Liquid Chromatography/Diode Array Detector) and HPLC/Mass Spectroscopy analyses were performed in order to evaluate the quali-quantitative contents of flavonoidic compounds. The HPLC profile shows two main isoflavones and another three compounds, one of them being a quercetin glycoside. The quercetin glycosides are flavonoidic derivatives abundant in plant materials and present in wine. We can therefore say: even if the phytoestrogen properties claimed for Trinovin turn out to be less than hoped for, the antioxidants contained are very powerful, and so possibly helpful in protection against many diseases, including cancers, atherosclerosis, diabetic retinal bleeding, and non-alcoholic dementia

  9. [Development of Tianma HPLC fingerprint and discriminant analysis].

    Science.gov (United States)

    Xiao, Jia-Jia; Huang, Hong; Lei, You-Cheng; Lin, Ting-Wen; Ma, Yue; Zhang, Jing; Zhang, Xing-Guo; Zhang, Da-Quan; Lv, Guang-Hua

    2017-07-01

    Tianma(the tuber of Gastrodia eleta) is a widely used and pricy Chinese herb. Its counterfeits are often found in herbal markets, which are the plant materials with similar macroscopic characteristics of Tianma. Moreover, the prices of Winter Tianma(cultivated Tianma) and Spring Tianma(mostly wild Tianma) have significant difference. However, it is difficult to identify the true or false, good or bad quality of Tianma samples. Thus, a total of 48 Tianma samples with different characteristics(including Winter Tianma, Spring Tianma, slice, powder, etc.) and 9 plant species 10 samples of Tianma counterfeits were collected and analyzed by HPLC-DAD-MS techniques. After optimizing the procedure of sample preparation, chromatographic and mass-spectral conditions, the HPLC chromatograms of all those samples were collected and compared. The similarities and Fisher discriminant analysis were further conducted between the HPLC chromatograms of Tianma and counterfeit, Winter Tianma and Spring Tianma. The results showed the HPLC chromatograms of 48 Tianma samples were similar at the correlation coefficient more than 0.848(n=48). Their mean chromatogram was simulated and used as Tianma HPLC fingerprint. There were 11 common peaks on the HPLC chromatograms of Tianma, in which 6 main peaks were chosen as characteristic peaks and identified as gastrodin, p-hydroxybenzyl alcohol, parishin A, parishin B, parishin C, parishin E, respectively by comparison of the retention time, UV and MS data with those of standard chemical compounds. All the six chemical compounds are bioactive in Tianma. However, the HPLC chromatograms of the 10 counterfeit samples were significantly different from Tianma fingerprint. The correlation coefficients between HPLC fingerprints of Tianma with the HPLC chromatograms of counterfeits were less than 0.042 and the characteristic peaks were not observed on the HPLC chromatograms of these counterfeit samples. It indicated the true or false Tianma can be

  10. HPLC assay for ethiofos in plasma: Application to pharmacokinetics in the beagle dog

    International Nuclear Information System (INIS)

    Swynnerton, N.F.; Mangold, D.J.; Ludden, T.M.

    1985-01-01

    An HPLC assay for ethiofos [S-2-(3-amino-propylamino)ethyl phosphorothioate, WR 2727] in plasma is presented. Its application to the development of pharmacokinetic parameters following IV administration of the drug to beagle dogs is demonstrated and preliminary pharmacokinetics of four dosings will be presented. Following a dose of 150 mg kg -1 , the plasma concentration versus time profile was best described by a two-compartment pharmacokinetics model. Mean pharmacokinetic parameters were: terminal elimination half-life = 16.0 minutes, volume of central compartment = 129 mL kg -1 , and clearance = 11.0 mL min -1 kg -1

  11. Direct 13C NMR Detection in HPLC Hyphenation Mode

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils

    2012-01-01

    Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments...... application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings...

  12. DETERMINATION AND VALIDATION OF MEBHYDROLINE NAPADISYLATE IN TABLETS BY HPLC

    Directory of Open Access Journals (Sweden)

    Lestyo Wulandari

    2010-06-01

    Full Text Available An accurate and sensitive HPLC method has been developed for the determination of mebhydroline napadisylate in the tablet. The Chromatography was performed on a reversed phase C-18 column, using a mobile phase of acetonitrile : ammonia 25% (80 : 20 v/v at ambient temperature 25±5 °C and UV detection operates at 320 nm in an overall analysis time of about 15 min, based on peak area. This HPLC method is selective, precise, and accurate and can be used for routine analysis of pharmaceutical preparation in industrial quality-control laboratories.   Keywords : HPLC, mebhydroline napadisylate, validation

  13. Determination of carbonyl compounds in air by HPLC; Determinacion de compuestos carbonilicos en aire por HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S; Perez, R M; Campos, A; Gonzalez, D

    1995-07-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs.

  14. The metabolism of 4-bromoaniline in the bile-cannulated rat: application of ICPMS (79/81Br), HPLC-ICPMS & HPLC-oaTOFMS

    Science.gov (United States)

    Duckett, Catherine; McCullagh, Michael; Smith, Christopher; Wilson, Ian D

    2015-01-01

    Abstract 1. An excretion balance study was performed following i.p. administration of 4-bromoaniline (50 mg kg−1) to bile-cannulated rats, using bromine-detected (79/81Br) ICPMS for quantification. Approximately 90% of the dose was recovered in urine (68.9 ± 3.6%) and bile (21.4 ± 1.4%) by 48 h post-administration. 2. HPLC-ICPMS (79/81Br) was used to selectively detect and profile the major urinary and biliary-excreted metabolites and determined that the 0–12 h urine contained at least 21 brominated metabolites with 19 bromine-containing peaks observed in the 6–12 h bile samples. 3. The urinary and biliary metabolites were subsequently profiled using HPLC-oaTOFMS. By exploiting the distinctive bromine isotope pattern ca. 60 brominated metabolites were detected in the urine in negative electrospray ionisation (ESI) mode while bile contained ca. 21. 4. While a large number of bromine-containing metabolites were detected, the profiles were dominated by a few major components with the bulk of the 4-bromoaniline-related material in urine accounted for by 4-bromoanaline O-sulfate (∼75% of the total by ICPMS, 84% by TOFMS). In bile a hydroxylated N-acetyl compound was the major metabolite detected, forming some ∼65% of the 4-bromoaniline-related material by ICPMS (37% by TOFMS). PMID:25837688

  15. The metabolism of 4-bromoaniline in the bile-cannulated rat: application of ICPMS ((79/81)Br), HPLC-ICPMS & HPLC-oaTOFMS.

    Science.gov (United States)

    Duckett, Catherine; McCullagh, Michael; Smith, Christopher; Wilson, Ian D

    2015-01-01

    1. An excretion balance study was performed following i.p. administration of 4-bromoaniline (50 mg kg(-1)) to bile-cannulated rats, using bromine-detected ((79/81)Br) ICPMS for quantification. Approximately 90% of the dose was recovered in urine (68.9 ± 3.6%) and bile (21.4 ± 1.4%) by 48 h post-administration. 2. HPLC-ICPMS ((79/81)Br) was used to selectively detect and profile the major urinary and biliary-excreted metabolites and determined that the 0-12 h urine contained at least 21 brominated metabolites with 19 bromine-containing peaks observed in the 6-12 h bile samples. 3. The urinary and biliary metabolites were subsequently profiled using HPLC-oaTOFMS. By exploiting the distinctive bromine isotope pattern ca. 60 brominated metabolites were detected in the urine in negative electrospray ionisation (ESI) mode while bile contained ca. 21. 4. While a large number of bromine-containing metabolites were detected, the profiles were dominated by a few major components with the bulk of the 4-bromoaniline-related material in urine accounted for by 4-bromoanaline O-sulfate (∼75% of the total by ICPMS, 84% by TOFMS). In bile a hydroxylated N-acetyl compound was the major metabolite detected, forming some ∼65% of the 4-bromoaniline-related material by ICPMS (37% by TOFMS).

  16. Auroral morphology

    International Nuclear Information System (INIS)

    Deehr, C.S.; Romick, G.J.; Sivjee, G.G.

    1981-01-01

    The aurora is a radiant manifestation of solar particle emissions and their control by intervening electromagnetic fields. The analogy with a television system was first made, we believe, by Elvey, (1958). The latest concepts of solar-terrestrial control are included in description by Akasofu (1979) showing the phosphor screen as the upper atmosphere with an auroral image produced by particles from a source on the sun, modulated by electric and magnetic fields with the magnetohydrodynamic (MDH) generator formed by electrons and protons from the solar wind across the geomagnetic tail as the power supply. Thus, the size and shape of the aurora must reflect all the forces acting in the auroral particles on their way from the sun to the earth. Auroral morphology, therefore, is the study of the occurence of aurora in space and time for the purpose of describing the origin of solar particels and the forces acting upon them between the time of their production on the sun and their loss in the atmosphere. The advantage of using the aurora as a television monitor of this process over any conceivable system of in situ measurements is obvious when one considers the large number of space vehicles which would be necessary to record the information concentrated in the auroral oval which differs in scale with the magnetosphere by perhaps 10 6 . (orig.)

  17. A comparative study for PSP toxins quantification by using MBA and HPLC official methods in shellfish.

    Science.gov (United States)

    Ben-Gigirey, B; Rodríguez-Velasco, M L; Otero, A; Vieites, J M; Cabado, A G

    2012-10-01

    Commission Regulation (EC) N° 2074/2005 recognises the biological method as the reference method for Paralytic Shellfish Poisoning (PSP) toxins detection in molluscs. It was amended by Commission Regulation (EC) N° 1664/2006 that accepted the so-called Lawrence method as an alternative to the reference method. The goal of this study was to compare AOAC Official Methods of Analysis 959.08 (Biological method) and 2005.06 (Prechromatographic Oxidation and Liquid Chromatography with fluorescence detection) in samples with different toxin profiles. The influence of extraction solvent in the total samples toxicity was also evaluated. A total of 40 samples including mussels, clams, scallops, razor-clams, cockles, oysters and barnacles were analysed by both official methods. Samples were selected with Alexandrium and Gymnodinium toxic profiles, from different origin and including several presentations: fresh, frozen, canned and boiled. Acetic and hydrochloric acid extractions were performed in all samples and the extracts were simultaneously analysed by both methods. Most samples were naturally contaminated and two samples were spiked. Comparison of both official methods, mouse bioassay (MBA) with HCl extraction and Liquid Chromatography with fluorescence detection (HPLC-FLD) with acetic acid extraction, led to an 85% of consistent results regarding compliance with legal limit, including samples below and above it. The linear correlation coefficient was r² = 0.69 and the paired t test (two tails, α = 0.05) indicated that there were not significant differences among both sets of data. Nevertheless, toxicity differences were found in several samples. In 15 out of 18 shellfish with a Gymnodinium toxic profile, higher toxicity levels were obtained by MBA. This fact was more evident in 7 samples, partially related to the lack of standards and the impossibility of analysing dc-NEO, C1, 2 and GTX6 at the beginning of the study. However, other factors concerning the extraction

  18. Ciclosporine A asxay: RIA or HPLC, plasma or total blood

    International Nuclear Information System (INIS)

    Lapalus, P.; Garraffo, R.; Krebs, B.; Lapalus, F.

    1985-01-01

    The two methods now in force for ciclosporine A assay are radioimmunoassay (RIA) and high pressure liquid chromatography (HPLC) in various biological media (plasma, serum, total blood). The advantages and disadvantages of the two methods are presented [fr

  19. [HPLC characteristic fingerprints of sedi linearis herba and sedi herba].

    Science.gov (United States)

    Lu, Lan-Qing; Mei, Qing; Wan, Ding-Rong; Yang, Xin-Zhou; Qiao, Shu; Zhao, Yu-Dan

    2014-04-01

    To study HPLC characteristic fingerprint of Sedum lineare from different harvest periods, and to compare with its related species Sedum sarmentosum. The HPLC fingerprints of Sedum lineare from different collecting periods were established and compared with Sedum sarmentosum by the same detection method. Hyperin, isoquercitrin and astragaloside were identified from the HPLC fingerprint of Sedum lineare. The fingerprint of Sedum lineare growing in the same area but different environment were basically identical; while there were remarkable differences of Sedum lineare growing in the same place but from different harvest periods, with the area of most common peaks changing from little to great, and slightly different peak number. The HPLC fingerprint of the two Sedum species had four common peaks, but could be distinguished from each other. The optimal harvest period of these two species should be full-bloom stage. The established method can provide reference for identification and quality analysis of Sedum lineare.

  20. Development of Reverse-Phase HPLC Method for Simultaneous ...

    African Journals Online (AJOL)

    Erah

    Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

  1. Standardization of RP-HPLC methods for the detection of the major peanut allergens Ara h 1, Ara h 2 and Ara h 3

    Science.gov (United States)

    Crude peanut extract (CPE) was analyzed for three major allergens (Ara h 1, h 2, and h 3) using a C12 and a C18 column at two wavelengths (280 and 220 nm) and under different solvent conditions. HPLC profiles were compared for retention time, resolution, and peak heights. CPE samples were spiked wit...

  2. Magnetic ligand fishing as a targeting tool for HPLC-HRMS-SPE-NMR: α-glucosidase inhibitory ligands and alkylresorcinol glycosides from Eugenia catharinae

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Brighente, Inês M. C.; Moaddel, Ruin

    2015-01-01

    A bioanalytical platform combining magnetic ligand fishing for α-glucosidase inhibition profiling and HPLC-HRMS-SPE-NMR for structural identification of α-glucosidase inhibitory ligands, both directly from crude plant extracts, is presented. Magnetic beads with N-terminus-coupled α-glucosidase we...

  3. HPLC analysis of vitamin B6 in foods

    Directory of Open Access Journals (Sweden)

    V.-M. OLLILAINEN

    2008-12-01

    Full Text Available The objective of this work was to evaluate the methods for determination of vitamin B6 in foods. To achieve this, the literature review focused on sample treatment and liquid chromatographic analysis of vitamin B6 related compounds. In the experimental part, the chosen sample pretreatment and the high-performance liquid chromatographic (HPLC method were validated, and used to produce vitamin B6 data on various food items commonly consumed in Finland. The main emphasis of the sample treatment was on the extraction efficiency and the maintenance of the original concentration profile of the vitamers. Several acid extraction procedures were tested for this purpose. Perchloric acid was chosen as the extraction agent. Routine food analysis was then performed using dilute ice-cold perchloric acid extraction followed by an internally standardized ion-paired reversed-phase liquid chromatography. Food samples were hydrolyzed with takadiastase and alkaline phosphatase enzymes, phosphorylated and glycosylated vitamers were quantitated before and after the enzymatic digestion. This procedure enabled the extraction of vitamin B6 compounds in their intact forms, and the measurement of free, phosphorylated and glycosylated forms. The maintenance of the concentration profile of the vitamers was verified by using 14C -labeled pyridoxal 5'-phosphate in the examination of the extraction procedure. The extraction efficiency and laboratory performance were confirmed by interlaboratory studies. Up-to-date data on vitamin B6 content of about fifty common food items was produced. The data includes the results from meat and poultry, fish and fish product, dairy product, cereal and vegetable, and ready-to-eat food samples. Free and phosphorylated vitamin B6 compounds were measured in all food groups, and the glycosylated vitamer fraction was analyzed in all plant-derived foods. The results obtained in this work showed that vitamin B6 content of nearly all foods of plant

  4. GlycoExtractor: a web-based interface for high throughput processing of HPLC-glycan data.

    Science.gov (United States)

    Artemenko, Natalia V; Campbell, Matthew P; Rudd, Pauline M

    2010-04-05

    Recently, an automated high-throughput HPLC platform has been developed that can be used to fully sequence and quantify low concentrations of N-linked sugars released from glycoproteins, supported by an experimental database (GlycoBase) and analytical tools (autoGU). However, commercial packages that support the operation of HPLC instruments and data storage lack platforms for the extraction of large volumes of data. The lack of resources and agreed formats in glycomics is now a major limiting factor that restricts the development of bioinformatic tools and automated workflows for high-throughput HPLC data analysis. GlycoExtractor is a web-based tool that interfaces with a commercial HPLC database/software solution to facilitate the extraction of large volumes of processed glycan profile data (peak number, peak areas, and glucose unit values). The tool allows the user to export a series of sample sets to a set of file formats (XML, JSON, and CSV) rather than a collection of disconnected files. This approach not only reduces the amount of manual refinement required to export data into a suitable format for data analysis but also opens the field to new approaches for high-throughput data interpretation and storage, including biomarker discovery and validation and monitoring of online bioprocessing conditions for next generation biotherapeutics.

  5. Two-dimensional fingerprinting approach for comparison of complex substances analysed by HPLC-UV and fluorescence detection.

    Science.gov (United States)

    Ni, Yongnian; Liu, Ying; Kokot, Serge

    2011-02-07

    This work is concerned with the research and development of methodology for analysis of complex mixtures such as pharmaceutical or food samples, which contain many analytes. Variously treated samples (swill washed, fried and scorched) of the Rhizoma atractylodis macrocephalae (RAM) traditional Chinese medicine (TCM) as well as the common substitute, Rhizoma atractylodis (RA) TCM were chosen as examples for analysis. A combined data matrix of chromatographic 2-D HPLC-DAD-FLD (two-dimensional high performance liquid chromatography with diode array and fluorescence detectors) fingerprint profiles was constructed with the use of the HPLC-DAD and HPLC-FLD individual data matrices; the purpose was to collect maximum information and to interpret this complex data with the use of various chemometrics methods e.g. the rank-ordering multi-criteria decision making (MCDM) PROMETHEE and GAIA, K-nearest neighbours (KNN), partial least squares (PLS), back propagation-artificial neural networks (BP-ANN) methods. The chemometrics analysis demonstrated that the combined 2-D HPLC-DAD-FLD data matrix does indeed provide more information and facilitates better performing classification/prediction models for the analysis of such complex samples as the RAM and RA ones noted above. It is suggested that this fingerprint approach is suitable for analysis of other complex, multi-analyte substances.

  6. Analysis of protein profiles using fuzzy clustering methods

    DEFF Research Database (Denmark)

    Karemore, Gopal Raghunath; Ukendt, Sujatha; Rai, Lavanya

    The tissue protein profiles of healthy volunteers and volunteers with cervical cancer were recorded using High Performance Liquid Chromatography combined with Laser Induced Fluorescence  technique  (HPLC-LIF)  developed  in  our  lab.      We analyzed      the protein profile data using different...

  7. Comparison of Peak-area Ratios and Percentage Peak Area Derived from HPLC-evaporative Light Scattering and Refractive Index Detectors for Palm Oil and its Fractions.

    Science.gov (United States)

    Ping, Bonnie Tay Yen; Aziz, Haliza Abdul; Idris, Zainab

    2018-01-01

    High-Performance Liquid Chromatography (HPLC) methods via evaporative light scattering (ELS) and refractive index (RI) detectors are used by the local palm oil industry to monitor the TAG profiles of palm oil and its fractions. The quantitation method used is based on area normalization of the TAG components and expressed as percentage area. Although not frequently used, peak-area ratios based on TAG profiles are a possible qualitative method for characterizing the TAG of palm oil and its fractions. This paper aims to compare these two detectors in terms of peak-area ratio, percentage peak area composition, and TAG elution profiles. The triacylglycerol (TAG) composition for palm oil and its fractions were analysed under similar HPLC conditions i.e. mobile phase and column. However, different sample concentrations were used for the detectors while remaining within the linearity limits of the detectors. These concentrations also gave a good baseline resolved separation for all the TAGs components. The results of the ELSD method's percentage area composition for the TAGs of palm oil and its fractions differed from those of RID. This indicates an unequal response of TAGs for palm oil and its fractions using the ELSD, also affecting the peak area ratios. They were found not to be equivalent to those obtained using the HPLC-RID. The ELSD method showed a better baseline separation for the TAGs components, with a more stable baseline as compared with the corresponding HPLC-RID. In conclusion, the percentage area compositions and peak-area ratios for palm oil and its fractions as derived from HPLC-ELSD and RID were not equivalent due to different responses of TAG components to the ELSD detector. The HPLC-RID has a better accuracy for percentage area composition and peak-area ratio because the TAG components response equally to the detector.

  8. HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication

    DEFF Research Database (Denmark)

    Johansen, Kenneth; Wubshet, Sileshi Gizachew; Nyberg, Nils

    2013-01-01

    Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC......–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts......, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin...

  9. Comparative study of fourteen alkaloids from Uncaria rhynchophylla hooks and leaves using HPLC-diode array detection-atmospheric pressure chemical ionization/MS method.

    Science.gov (United States)

    Qu, Jialin; Gong, Tianxing; Ma, Bin; Zhang, Lin; Kano, Yoshihiro; Yuan, Dan

    2012-01-01

    The purpose of the study is to compare alkaloid profile of Uncaria rhynchophylla hooks and leaves. Ten oxindole alkaloids and four glycosidic indole alkaloids were identified using HPLC-diode array detection (DAD) or LC-atmospheric pressure chemical ionization (APCI)-MS method, and a HPLC-UV method for simultaneous quantification of major alkaloids was validated. The hooks are characterized by high levels of four oxindole alkaloids rhynchophylline (R), isorhynchophylline (IR), corynoxeine (C) and isocorynoxeine (IC), while the leaves contained high level of two glycosidic indole alkaloids vincoside lactam (VL) and strictosidine (S). The presented methods have proven its usefulness in chemical characterization of U. rhynchophylla hooks and leaves.

  10. Efecto del proceso de secado de la lombriz de tierra (Eisenia andrei sobre el perfil aminoacídico de la harina determinado por cromatografía (CLAE | Effect of drying process of the earthworm (Eisenia andrei on amino acidic profile of the meal determined by chromatography (HPLC

    Directory of Open Access Journals (Sweden)

    José Ovalles

    2017-11-01

    Full Text Available The possible effect of the drying temperature of the earthworm, Eisenia andrei, biomass on the amino acid profile of the resulting flour was evaluated. A tray dryer with air recirculation was used as a drying technique. The tested drying temperature were relatively low, T1 = 30, T2 = 40, T3 = 45 (°C, until obtaining a relative humidity below 10%. The differences in protein content of meal among treatments were not significant and resulted in average 63 ± 2% on a dry basis, and practically did not affect the proximate analysis in terms of total fat (7.2 ± 0.7% and ash content (5.3 ± 0.6%. Differences in the amino acid profile of the earthworm meal were not significant (p = 0.05 among treatments, except for asparagine (as Asp and glutamine (as Glu. Although, under the experimental conditions of the proposed approach, the results in terms of nutritional values were expected and satisfactory, they were not convenient in terms of microbiological quality. The results allow to infer that the use of low temperature drying is not a recommended approach to obtain earthworm meal, unless experimental conditions also ensure the microbiological quality without compromising the cost-benefit of the proposed drying process.

  11. Sensitive measurement of positron emitters eluted from HPLC

    International Nuclear Information System (INIS)

    Takei, Makoto; Kida, Takayo; Suzuki, Kazutoshi

    2001-01-01

    For sensitive analysis of the radioactive-metabolite in human PET, a radio-HPLC system coupled to a newly designed positron detector was constructed. The detector had the advantages of low noise level (1.7±1.0 cpm) and high sensitivity (32±1%) due to coincidence counting and large BGO crystals. Furthermore, the detector was easy to move, since a pair of the BGO housings coupled to photomultipliers was effectively arranged in parallel and a HPLC cell with different volume could be inserted between the BGO housing. This radio-HPLC system was useful for analyzing samples with low radioactivity. It was applied to the measurement of [ 11 C]FLB457 in plasma, having high affinity and high selectivity with dopamine D2 receptors. Extremely low radioactivity of [ 11 C]FLB457 (2500 dpm) could be analyzed by using the radio-HPLC system. The performance of this detector was compared with those of commercially available systems that had been used as sensitive detectors for HPLC

  12. [Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC].

    Science.gov (United States)

    Yang, Xiu-Juan; Hong, Yan-Long; Wu, Fei; Ruan, Ke-Feng; Feng, Yi

    2013-03-01

    To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhnchophylla. An HPLC method has been developed for determination of rhnchophylline and isorhnchophylline. The transformation of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS. Good linearities of rhynchophylline and isorhynchophylline were 0.064-5.100, 0.064-5.110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynchophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 12.60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic extraction procedure, the average recoveries of rhynchophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59%, resepectively. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 47.08% and 51.03%, respectively. The unqualified recovery could be elucidated by HPLC-ESI-MS analysis, indicating that trhynchophylline could be transformed mostly into isorhynchophylline and a little amount of unkown composition, while isorhynchophylline could be transformed into rhynchophylline isocorynoxeine, corynoxeine and 22-O-beta-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure. Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynchophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.

  13. Characterization of nonstarch polysaccharides content from different edible organs of some vegetables, determined by GC and HPLC: comparative study.

    Science.gov (United States)

    Villanueva-Suárez, M J; Redondo-Cuenca, A; Rodríguez-Sevilla, M D; de las Heras Martínez, M

    2003-09-24

    Content and composition of dietary fiber as nonstarch polysaccharides (NSP) was determined in vegetables belonging to different types of edible organs, using GC and HPLC. Samples analyzed were subterranean organs (radish and leek), leaves (celery, swiss chard, and lettuce), stalks (celery, swiss chard, and asparagus), inflorescence (broccoli), and fruits (tomato, green pepper, and marrow). The results indicate that though the monomeric profile is similar in all these samples quantitative differences were found for neutral sugars and uronic acids among samples of the same type of vegetal organ. The NSP values determined using CG method were in good agreement with HPLC method (R(2) = 0.9005). However, arabinose, mannose, and galactose plus rhamnose are more influenced by the analytical method used than the rest of the monomers in nearly all the samples analyzed. Final values of NSP depend on the method used in celery stalks, broccoli, and green pepper.

  14. Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

    Directory of Open Access Journals (Sweden)

    Andrea N. de L. Batista

    2011-06-01

    Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

  15. Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

    Directory of Open Access Journals (Sweden)

    Andrea N. de L. Batista

    2011-04-01

    Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

  16. Quantitation of radiolabeled compounds eluting from the HPLC system

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1982-01-01

    Three techniques are compared for the quantitation of various radiolabeled compounds eluting in the high performance liquid chromatography system. The first technique requires fraction-collecting the effluent from the HPLC, removing an aliquot to scintillation vials, and counting each fraction in a liquid scintillation counter. The second uses direct interface of the HPLC effluent to a flow-through radioactivity detector. The third involves quantitation of various radiolabeled compounds (proteins, steroids, and nucleotides) by splitting the effluent from the HPLC with an electronic steam splitter, thus diverting a present portion to the fraction collector for further chemical characterization and the remainder to the radioactivity flow detector for direct quantitation. A direct comparison of the chromatograms and the radioactivity counting efficiencies of these three techniques is presented

  17. [Study and comparison on HPLC fingerprints of flavonoids of frequently used Chinese materia medica in citrus].

    Science.gov (United States)

    Chen, Yonggang; Lin, Li

    2011-10-01

    To establish the HPLC fingerprint of flavonoids of the six clinical frequently used Chinese materia medica for regulating Qi flow,such as Citri grandis, C. grands, Citri Reticulatae Pericarpium, Citri Reticulatae Pericarpium Viride, Aurantii Fructus, and Aurantii Fructus Immaturus from Citrus, and analysis differences in the fingerprints to provide scientific basis for profile-effect research and clinical reasonable use. HPLC was performed on a C18 column with methanol-water (with acetic acid), to establish HPLC fingerprints of the six kinds of medicinal herbs on the same chromatograph condition. The six frequently used Chinese materia medica were divided into naringin type and hesperidin type according to the method of phytochemotaxonomy. Based on the retention time of chromatograph peaks, C. grandis and C. grands had fifteen common peaks; Citri Reticulatae Pericarpium, Citri Reticulatae Pericarpium Viride, Aurantii Fructus and Aurantii Fructus Immaturus had ten common peaks. All herbs had five common peaks. Compared with mutual model, the holistic similarity of chromatograms of C. grandis and C. grands was in the range of 0.9285 - 0.9962. The degree of similarity was high. For Citri Reticulatae Pericarpium, Citri Reticulatae Pericarpium Viride and Aurantii Fructus Immaturus, it was in the range of 0.9221 - 0.9973 and high. But the similarity of Aurantii Fructus was only in 0.4547 - 0.7733 with the mutual model. The established fingerprints of flavonoids of the six common traditional Chinese medicines can be used to compare the differences intuitively. Meanwhile, the peak height and peak areas of characteristic peaks are different remarkably, but whether it is connected with the different function of regulating Qi flow of the six medical materials in clinical use, is still needed to be studied.

  18. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    Adcock, Jacqui L.; Francis, Paul S.; Agg, Kent M.; Marshall, Graham D.; Barnett, Neil W.

    2007-01-01

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  19. Chemical fingerprinting and quantitative analysis of a Panax notoginseng preparation using HPLC-UV and HPLC-MS

    Directory of Open Access Journals (Sweden)

    Shao Qing

    2011-02-01

    Full Text Available Abstract Background Xuesaitong (XST injection, consisting of total saponins from Panax notoginseng, was widely used for the treatment of cardio- and cerebro-vascular diseases in China. This study develops a simple and global quality evaluation method for the quality control of XST. Methods High performance liquid chromatography-ultraviolet detection (HPLC-UV was used to identify and quantify the chromatographic fingerprints of the XST injection. Characteristic common peaks were identified using HPLC with photo diode array detection/electrospray ionization tandem mass spectrometry (HPLC-PDA/ESI-MSn. Results Representative fingerprints from ten batches of samples showed 27 'common saponins' all of which were identified and quantified using ten reference saponins. Conclusion Chemical fingerprinting and quantitative analysis identified most of the common saponins for the quality control of P. notoginseng products such as the XST injection.

  20. Immunoassay screening of lysergic acid diethylamide (LSD) and its confirmation by HPLC and fluorescence detection following LSD ImmunElute extraction.

    Science.gov (United States)

    Grobosch, T; Lemm-Ahlers, U

    2002-04-01

    In all, 3872 urine specimens were screened for lysergic acid diethylamide (LSD) using the CEDIA DAU LSD assay. Forty-eight samples, mainly from psychiatric patients or drug abusers, were found to be LSD positive, but only 13 (27%) of these could be confirmed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) following immunoaffinity extraction (IAE). Additional analysis for LSD using the DPC Coat-a-Count RIA was performed to compare the two immunoassay screening methods. Complete agreement between the DPC RIA assay and HPLC-FLD results was observed at concentrations below a cutoff concentration of 500 pg/mL. Samples that were LSD positive in the CEDIA DAU assay but not confirmed by HPLC-FLD were also investigated for interfering compounds using REMEDI HS drug-profiling system. REMEDI HS analysis identified 15 compounds (parent drugs and metabolites) that are believed to cross-react in the CEDIA DAU LSD assay: ambroxol, prilocaine, pipamperone, diphenhydramine, metoclopramide, amitriptyline, doxepine, atracurium, bupivacaine, doxylamine, lidocaine, mepivacaine, promethazine, ranitidine, and tramadole. The IAE/HPLC-FLD combination is rapid, easy to perform and reliable. It can reduce costs when standard, rather than more advanced, HPLC equipment is used, especially for labs that perform analyses for LSD infrequently. The chromatographic analysis of LSD, nor-LSD, and iso-LSD is not influenced by any of the tested cross-reacting compounds even at a concentration of 100 ng/mL.

  1. [Evaluation of Brodifacoum-induced Toxicity by Metabonomics Approach Based on HPLC-TOF-MS].

    Science.gov (United States)

    Yan, H; Zhuo, X Y; Shen, B H; Xiang, P; Shen, M

    2017-06-01

    To analyse the metabolic changes in urine of rats with brodifacoum intoxication, and to reveal the molecular mechanism of brodifacoum-induced toxicity on rats. By establishing a brodifacoum poisoning rats model, the urine metabolic profiling data of rats were acquired using high performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF-MS). The orthogonal partial least squares analysis-discrimination analysis (OPLS-DA) was applied for the multivariate statistics and the discovery of differential metabolites closely related to toxicity of brodifacoum. OPLS-DA score plot showed that the urinary metabolic at different time points before and after drug administration had good similarity within time period and presented clustering phenomenon. Comparing the urine samples of rats before drug administration with which after drug administration, twenty-two metabolites related to brodifacoum-induced toxicity were selected. The toxic effect of brodifacoum worked by disturbing the metabolic pathways in rats such as tricarboxylic cycle, glycolysis, sphingolipid metabolism and tryptophan metabolism, and the toxicity of brodifacoum is characterized of accumulation effect. The metabonomic method based on urine HPLC-TOF-MS can provide a novel insight into the study on molecular mechanism of brodifacoum-induced toxicity. Copyright© by the Editorial Department of Journal of Forensic Medicine

  2. Fingerprint analysis of polysaccharides from different Ganoderma by HPLC combined with chemometrics methods.

    Science.gov (United States)

    Sun, Xiaomei; Wang, Haohao; Han, Xiaofeng; Chen, Shangwei; Zhu, Song; Dai, Jun

    2014-12-19

    A fingerprint analysis method has been developed for characterization and discrimination of polysaccharides from different Ganoderma by high performance liquid chromatography (HPLC) coupled with chemometrics means. The polysaccharides were extracted under ultrasonic-assisted condition, and then partly hydrolyzed with trifluoroacetic acid. Monosaccharides and oligosaccharides in the hydrolyzates were subjected to pre-column derivatization with 1-phenyl-3-methyl-5-pyrazolone and HPLC analysis, which will generate unique fingerprint information related to chemical composition and structure of polysaccharides. The peak data were imported to professional software in order to obtain standard fingerprint profiles and evaluate similarity of different samples. Meanwhile, the data were further processed by hierarchical cluster analysis and principal component analysis. Polysaccharides from different parts or species of Ganoderma or polysaccharides from the same parts of Ganoderma but from different geographical regions or different strains could be differentiated clearly. This fingerprint analysis method can be applied to identification and quality control of different Ganoderma and their products. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. A validated bioanalytical HPLC method for pharmacokinetic evaluation of 2-deoxyglucose in human plasma.

    Science.gov (United States)

    Gounder, Murugesan K; Lin, Hongxia; Stein, Mark; Goodin, Susan; Bertino, Joseph R; Kong, Ah-Ng Tony; DiPaola, Robert S

    2012-05-01

    2-Deoxyglucose (2-DG), an analog of glucose, is widely used to interfere with glycolysis in tumor cells and studied as a therapeutic approach in clinical trials. To evaluate the pharmacokinetics of 2-DG, we describe the development and validation of a sensitive HPLC fluorescent method for the quantitation of 2-DG in plasma. Plasma samples were deproteinized with methanol and the supernatant was dried at 45°C. The residues were dissolved in methanolic sodium acetate-boric acid solution. 2-DG and other monosaccharides were derivatized to 2-aminobenzoic acid derivatives in a single step in the presence of sodium cyanoborohydride at 80°C for 45 min. The analytes were separated on a YMC ODS C₁₈ reversed-phase column using gradient elution. The excitation and emission wavelengths were set at 360 and 425 nm. The 2-DG calibration curves were linear over the range of 0.63-300 µg/mL with a limit of detection of 0.5 µg/mL. The assay provided satisfactory intra-day and inter-day precision with RSD less than 9.8%, and the accuracy ranged from 86.8 to 110.0%. The HPLC method is reproducible and suitable for the quantitation of 2-DG in plasma. The method was successfully applied to characterize the pharmacokinetics profile of 2-DG in patients with advanced solid tumors. Copyright © 2011 John Wiley & Sons, Ltd.

  4. Quantitative analysis of the major constituents of St John's wort with HPLC-ESI-MS.

    Science.gov (United States)

    Chandrasekera, Dhammitha H; Welham, Kevin J; Ashton, David; Middleton, Richard; Heinrich, Michael

    2005-12-01

    A method was developed to profile the major constituents of St John's wort extracts using high-performance liquid chromatography-electrospray mass spectrometry (HPLC-ESI-MS). The objective was to simultaneously separate, identify and quantify hyperforin, hypericin, pseudohypericin, rutin, hyperoside, isoquercetrin, quercitrin and chlorogenic acid using HPLC-MS. Quantification was performed using an external standardisation method with reference standards. The method consisted of two protocols: one for the analysis of flavonoids and glycosides and the other for the analysis of the more lipophilic hypericins and hyperforin. Both protocols used a reverse phase Luna phenyl hexyl column. The separation of the flavonoids and glycosides was achieved within 35 min and that of the hypericins and hyperforin within 9 min. The linear response range in ESI-MS was established for each compound and all had linear regression coefficient values greater than 0.97. Both protocols proved to be very specific for the constituents analysed. MS analysis showed no other signals within the analyte peaks. The method was robust and applicable to alcoholic tinctures, tablet/capsule extracts in various solvents and herb extracts. The method was applied to evaluate the phytopharmaceutical quality of St John's wort preparations available in the UK in order to test the method and investigate if they contain at least the main constituents and at what concentrations.

  5. Arsenic-containing fatty acids and hydrocarbons in marine oils - determination using reversed-phase HPLC-ICP-MS and HPLC-qTOF-MS.

    Science.gov (United States)

    Sele, Veronika; Sloth, Jens J; Holmelid, Bjarte; Valdersnes, Stig; Skov, Kasper; Amlund, Heidi

    2014-04-01

    Arsenolipids are the major arsenic species present in marine oils. Several structures of arsenolipids have been elucidated the last 5 years, demonstrating the chemical complexity of this trace element in the marine environment. Several commercial fish oils and marine oils, ranging in total arsenic concentrations from 1.6 to 12.5 mg kg(-1) oil, were analyzed for arsenolipids using reversed-phase high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The arsenolipids were quantified using three different arsenic-containing calibration standards; dimethylarsinate (DMA), triphenylarsinoxide (Ph₃AsO) and a synthesized arsenic-containing hydrocarbon (AsHC) (dimethylarsinoyl nonadecane; C₂₁H₄₃AsO). The observed variation in signal intensity for arsenic during the gradient elution profile in reversed-phase HPLC was compensated for by determining the time-resolved response factors for the arsenolipids. Isotopes of germanium ((74)Ge) and indium ((115)In) were suited as internal standards for arsenic, and were used for verification of the arsenic signal response factors during the gradient elution. Dimethylarsinate was the most suitable calibration standard for the quantification of arsenolipids, with recoveries between 91% and 104% compared to total arsenic measurements in the same extracts. A range of marine oils was investigated, including oils of several fish species, cod liver and seal, as well as three commercial fish oils. The AsHCs - C₁₇H₃₈AsO, C₁₉H₄₂AsO and C₂₃H₃₈AsO - were identified as the major arsenolipids in the extracts of all oils by HPLC coupled with quadrupole time-of-flight mass spectrometry (qTOF-MS). Minor amounts of two arsenic-containing fatty acids (AsFAs) (C₂₃H₃₈AsO₃ and C₂₄H₃₈AsO₃) were also detected in the oils. The sum of the AsHCs and the AsFAs determined in the present study accounted for 17-42% of the total arsenic in the oils

  6. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  7. Exorphin Peptides in Urine with HPLC-MS/MS Detection

    OpenAIRE

    2015-01-01

    Exorphins have been found in urine from individuals diagnosed with autism spectrum disorders by HPLC techniques. However, several studies, using sophisticated analytical techniques , have reported negative findings. This made it necessary to improve our methods. The sample stability during transport and storage and the pre -analytical treatment of urines was improved by peptidase inhibition and solid ...

  8. Validated RP-HPLC Method for Quantification of Phenolic ...

    African Journals Online (AJOL)

    Purpose: To evaluate the total phenolic content and antioxidant potential of the methanol extracts of aerial parts and roots of Thymus sipyleus Boiss and also to determine some phenolic compounds using a newly developed and validated reversed phase high performance liquid chromatography (RP-HPLC) method.

  9. Rapid and Reliable HPLC Method for the Determination of Vitamin ...

    African Journals Online (AJOL)

    Purpose: To develop and validate an accurate, sensitive and reproducible high performance liquid chromatographic (HPLC) method for the quantitation of vitamin C in pharmaceutical samples. Method: The drug and the standard were eluted from Superspher RP-18 (250 mm x 4.6 mm, 10ìm particle size) at 20 0C.

  10. A Simple HPLC Bioanalytical Method for the Determination of ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, accurate, and precise high performance chromatography (HPLC) method with spectrophotometric detection for the determination of doxorubicin hydrochloride in rat plasma. Methods: Doxorubicin hydrochloride and daunorubicin hydrochloride (internal standard, IS) were separated on a C18 ...

  11. A Stability Indicating HPLC Method for the Determination of ...

    African Journals Online (AJOL)

    Erah

    stability indicating reverse phase HPLC method for estimating meloxicam (MLX) in bulk ... acetonitrile-water-glacial acetic acid [55:40:5 (% v/v)] at a flow rate of 1ml/min and detection wavelength .... pore and degassed before use. ... determined to assess the effect of small but ... deviation, the standard error of slope, and the.

  12. Separation of complex oligosaccharides from wort and beer using HPLC

    Czech Academy of Sciences Publication Activity Database

    Cabálková, Jana; Bobálová, Janette

    2008-01-01

    Roč. 102, č. 15 (2008), s608-s609 ISSN 1803-2389. [Meeting on Chemistry and Life /4./. Brno, 09.09.2008-11.09.2008] R&D Projects: GA MŠk 2B06037 Institutional research plan: CEZ:AV0Z40310501 Keywords : oligosacharides * beer * HPLC Subject RIV: CB - Analytical Chemistry, Separation

  13. SCREENING CORD BLOOD FOR HEMOGLOBINOPATHIES AND THALASSEMIA BY HPLC

    NARCIS (Netherlands)

    VANDERDIJS, FPL; VANDENBERG, GA; SCHERMER, JG; MUSKIET, FD; LANDMAN, H; MUSKIET, FAJ

    We evaluated the use of an HPLC method for screening hemoglobins in cord blood. We studied the genotype frequencies of the structural hemoglobin variants HbS and HbC and the synthesis variants alpha- and beta+-thalassemia in babies born on Curacao. During three months, 67.2% of all (748) newborns

  14. Chiral HPLC and physical characterisation of orthoconic antiferroelectric liquid crystals

    Czech Academy of Sciences Publication Activity Database

    Vojtylová, Terézia; Żurowska, M.; Milewska, K.; Hamplová, Věra; Sýkora, D.

    2016-01-01

    Roč. 43, č. 9 (2016), s. 1244-1250 ISSN 0267-8292 R&D Projects: GA MŠk(CZ) LD14007; GA ČR GA15-02843S Institutional support: RVO:68378271 Keywords : liquid crystals * chiral HPLC * orthoconic antiferroelectric LC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.661, year: 2016

  15. HPLC quantification of phenolic content and assessment of ...

    African Journals Online (AJOL)

    omotayo

    2016-03-02

    Mar 2, 2016 ... detection (HPLC-DAD) fingerprinting of phenolic content. Furthermore, the .... Briefly, deionised water (0.5 ml) and 125 μl of Folin–Colcalteu reagent were added to ..... to be organ-specific and can leak from a damaged or an.

  16. Reverse-phase HPLC analysis of human alpha crystallin.

    Science.gov (United States)

    Swamy, M S; Abraham, E C

    1991-03-01

    A rapid and highly sensitive reverse-phase HPLC (RP-HPLC) method was used to separate crystallin subunits from human alpha crystallin. Three distinct peaks were separated; by electrophoretic and immunological analyses the first and second peaks were identified as alpha B and alpha A respectively. On the other hand, peak 3 appeared to be a modified form of alpha crystallin. The ratio of alpha A and alpha B proteins was 3:1 in 1 day old lenses which gradually changed to 2:1 in 17 year old lenses and to 1:1 in the 50 and 82 year old whole lenses and 82 year old lens cortex, with a concomitant increase in the modified alpha, suggesting that alpha A subunits are relatively more involved in aggregation. Analysis of the 82 year old lens nucleus also supported this conclusion. The RP-HPLC analysis of the HMW aggregate fraction showed substantial enrichment of the modified alpha. The alpha A and alpha B subunits independently reassociated to form polymeric alpha crystallin whereas the modified alpha reassociated to form HMW aggregates as shown by molecular sieve HPLC. Hence it appears that the HMW aggregate peak was constituted by modified alpha crystallin. Only in the peak 3 material the 280 nm absorbance was about 2-fold higher than what was expected from the actual protein content. The data suggest that the changes induced by post-translational modifications may have some role in the formation of modified alpha. The present RP-HPLC method is useful in separating these modified alpha from the unmodified alpha A and alpha B subunits.

  17. Morphological, chemical and molecular differentiation of Fusarium equiseti isolated from Norwegian cereals.

    Science.gov (United States)

    Kosiak, Elzbieta Barbara; Holst-Jensen, Arne; Rundberget, Thomas; Gonzalez Jaen, Maria Teresa; Torp, Mona

    2005-03-15

    The morphological variation, secondary metabolite profiles and restriction fragment length polymorphisms (RFLPs) of PCR amplified intergenic spacer (IGS) ribosomal DNA (rDNA) were studied in 27 isolates of Fusarium equiseti, 25 isolated from Norwegian cereals and 2 from soil obtained from the IBT culture collection (BioCentrum, Technical University of Denmark). All 27 isolates were tested for production of fusarochromanone (FUSCHR), zearalenone (ZEA) and the trichothecenes: 15-monoacetoxy-scirpentriol (MAS), diacetoxy-scirpenol (DAS), T-2 and HT-2 toxins, T2-triol, neosolaniol (NEO), deoxynivalenol (DON), nivalenol (NIV) and 4-acetylnivalenol (Fus-X). The trichothecenes were analysed by GC-MS in a selected ion monitoring mode, while FUSCHR was determined by ion pair HPLC with fluorometric detection and production of ZEA by TLC. For amplification of IGS rDNA primers CNL12 and CNS1 were applied. IGS rDNA was digested with the four restriction enzymes: AvaII, CfoI, EcoRI and Sau3A. In addition, we sequenced the IGS rDNA region of three of the Norwegian isolates. There were two morphological types among the Norwegian strains of F. equiseti, type I with short apical cells (dominating) and type II with long apical cells, with four haplotypes identified based on the RFLP data. Variation in secondary metabolite profiles within and between the morphological groups was observed and the levels of produced toxins were: FUSCHR 3000-42,500 and 25-30 ng/g, NIV 20-2500 and 120-700 ng/g, FUS-X 20-15,000 and 0 ng/g, DAS 30-7500 and 0-600 ng/g, and MAS 10-600 and 0-500 ng/g, for strains with short and long apical cells, respectively. NEO was detected in 16/27 strains tested (all morphotype I). All but four strains of type I (these four lacked a restriction site for EcoRI) had identical RFLP profiles. The isolates of type II had two haplotypes. The IGS sequence similarity data indicated differences between these morphotypes corresponding to two separate lineages apparently at the

  18. Analysis of taxines in Taxus plant material and cell cultures by hplc photodiode array and hplc-electrospray mass spectrometry

    NARCIS (Netherlands)

    Theodoridis, G.; Laskaris, G.; Rozendaal, E.L.M.; Verpoorte, R.

    2001-01-01

    A semi-purified Taxus baccata needles extract was analysed by RP-HPLC. More than 18 taxines and cinnamates were detected by photodiode array detection and LC-MS, 10 of them being positively identified. Furthermore, 10-deacetyl baccatin III (paclitaxel's main precursor) and other taxanes were also

  19. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  20. Analysis of flavonoids from propolis by on-line HPLC-electrospray mass spectrometry.

    Science.gov (United States)

    Volpi, Nicola; Bergonzini, Gianluca

    2006-09-26

    In this paper, the qualitative and quantitative separation and determination of the polyphenolic component of propolis preparations in the form of ethanolic extract, usually used for commercial pharmaceutical preparations, has been investigated by means of on-line HPLC-ESI/MS technique. Propolis of different origin have been evaluated for their components and a specific fingerprint has been determined potentially useful for the quality control of extracts in pharmaceutical preparations. The ethanolic extracts of propolis from Argentina, Italy and Spain shows approximately the same total ion chromatogram (TIC) profile due to the presence of the same molecular species, identified by the negative ESI-MS. On the contrary, the samples from Azerbaijan, China, Ethiopia and Kenya show a very peculiar TIC profiles. By using many purified flavonoids and calibration curves over a wide concentration range, from 0.05 (5 microg/ml) to 5 microg (500 microg/ml), an accurate assessment of the contents of several bioactive compounds in extract samples was performed. The propolis from Argentina, Italy and Spain show a great amount of pinocembrin (approximately 49%, 48% and 39% of the total identified flavonoids, respectively) and variable but similar percentages of the other species. On the contrary, the propolis from China, Azerbaijan and Ethiopia have a great amount of pinocembrin (approximately 63%, 46% and 62%, respectively) but no presence of genistein, kaempferol, apigenin and chrysin for the sample from China, genistein, kaempferol, acacetin and chrysin for the propolis from Azerbaijan, and no kaempferol and acacetin for the sample from Ethiopia. The ethanolic extract from propolis of Kenya has no identified flavonoid species but just a peak possessing a m/z of 253.0. Finally, an evaluation of the presence of total flavonoids for the various propolis samples was performed, with extracts from Argentina, Italy and Spain more rich in polyphenols than those from Azerbaijan, China

  1. Authentication and Quantitation of Fraud in Extra Virgin Olive Oils Based on HPLC-UV Fingerprinting and Multivariate Calibration

    Science.gov (United States)

    Carranco, Núria; Farrés-Cebrián, Mireia; Saurina, Javier

    2018-01-01

    High performance liquid chromatography method with ultra-violet detection (HPLC-UV) fingerprinting was applied for the analysis and characterization of olive oils, and was performed using a Zorbax Eclipse XDB-C8 reversed-phase column under gradient elution, employing 0.1% formic acid aqueous solution and methanol as mobile phase. More than 130 edible oils, including monovarietal extra-virgin olive oils (EVOOs) and other vegetable oils, were analyzed. Principal component analysis results showed a noticeable discrimination between olive oils and other vegetable oils using raw HPLC-UV chromatographic profiles as data descriptors. However, selected HPLC-UV chromatographic time-window segments were necessary to achieve discrimination among monovarietal EVOOs. Partial least square (PLS) regression was employed to tackle olive oil authentication of Arbequina EVOO adulterated with Picual EVOO, a refined olive oil, and sunflower oil. Highly satisfactory results were obtained after PLS analysis, with overall errors in the quantitation of adulteration in the Arbequina EVOO (minimum 2.5% adulterant) below 2.9%. PMID:29561820

  2. Lack of evidence from HPLC 32P-post-labelling for tamoxifen-DNA adducts in the human endometrium.

    Science.gov (United States)

    Carmichael, P L; Sardar, S; Crooks, N; Neven, P; Van Hoof, I; Ugwumadu, A; Bourne, T; Tomas, E; Hellberg, P; Hewer, A J; Phillips, D H

    1999-02-01

    Tamoxifen is associated with an increased incidence of endometrial cancer in women. It is also a potent carcinogen in rat liver and forms covalent DNA adducts in this tissue. A previous study exploring DNA adducts in human endometria, utilizing thin layer chromatography 32P-postlabelling, found no evidence for adducts in tamoxifen-treated women [Carmichael,P.L., Ugwumadu,A.H.N., Neven,P., Hewer,A.J., Poon,G.K. and Phillips,D.H. (1996) Cancer Res., 56, 1475-1479]. However, subsequent work utilizing HPLC 32P-post-labelling [Hemminki,K., Ranjaniemi,H., Lindahl,B. and Moberger,B. (1996) Cancer Res., 56, 4374-4377] suggested that very low levels could be detected. We have sought to investigate this question further by reproducing the HPLC methodology at two centres, and analysing endometrial DNA from 20 patients treated with 20 mg/day tamoxifen for between 22 and 65 months. Liver DNA isolated from tamoxifen-treated rats was used as a positive control. We found no convincing evidence for tamoxifen-derived DNA adducts in human endometrium. HPLC elution profiles of post-labelled DNA from tamoxifen-treated women were indistinguishable from those obtained with DNA from 14 untreated women and from six women taking toremifene, an analogue of tamoxifen.

  3. Self-assembled highly ordered ethane-bridged periodic mesoporous organosilica and its application in HPLC.

    Science.gov (United States)

    Huang, Lili; Lu, Juan; Di, Bin; Feng, Fang; Su, Mengxiang; Yan, Fang

    2011-09-01

    Monodisperse spherical periodic mesoporous organosilicas (PMOs) with ethane integrated in the framework were synthesized and their application as stationary phase for chromatographic separation is demonstrated. The ethane-PMOs were prepared by condensation of 1,2-bis(triethoxysilyl)ethane (BTSE) in basic condition using octadecyltrimethylammonium chloride (C(18)TMACl) as template and ethanol as co-solvent. The morphology and mesoporous structure of ethane-PMOs were controlled under different concentrations of sodium hydroxide (NaOH) and EtOH. The results of scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), nitrogen sorption measurement, Fourier transform infrared spectroscopy (FT-IR) and elemental analysis showed that ethane-PMOs have spherical morphology, uniform particle distribution, highly ordered pore structure, high surface area and narrow pore-size distribution. The column packed with these materials exhibits good permeability, high chemical stability and good selectivity of mixtures of aromatic hydrocarbons in normal phase high-performance liquid chromatography (HPLC). Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Gross morphology betrays phylogeny

    DEFF Research Database (Denmark)

    Alström, Per; Fjeldså, Jon; Fregin, Silke

    2011-01-01

    .). Superficial morphological similarity to cisticolid warblers has previously clouded the species true relationship. Detailed morphology, such as facial bristles and claw and footpad structure, also supports a closer relationship to Cettiidae and some other non-cisticolid warblers....

  5. Equilibrium shoreface profiles

    DEFF Research Database (Denmark)

    Aagaard, Troels; Hughes, Michael G

    2017-01-01

    Large-scale coastal behaviour models use the shoreface profile of equilibrium as a fundamental morphological unit that is translated in space to simulate coastal response to, for example, sea level oscillations and variability in sediment supply. Despite a longstanding focus on the shoreface...... profile and its relevance to predicting coastal response to changing environmental conditions, the processes and dynamics involved in shoreface equilibrium are still not fully understood. Here, we apply a process-based empirical sediment transport model, combined with morphodynamic principles to provide......; there is no tuning or calibration and computation times are short. It is therefore easily implemented with repeated iterations to manage uncertainty....

  6. Vergelijking van HPLC-methoden voor de bepaling van pentachloorfenol in houtmonsters

    NARCIS (Netherlands)

    Goewie; C.E.; Berkhoff; C.J.

    1986-01-01

    Een vergelijkend onderzoek is verricht naar de bruikbaarheid van verschillende detectiemethoden in combinatie met HPLC voor de analyse van pentachloorfenol in hout. In het onderzoek wordt RP-HPLC met UK en amperometrische detectie beschreven, evenals NP-HPLC met elektroneninvangdetectie. In

  7. Morphological studies of some cultivated soils

    NARCIS (Netherlands)

    Slager, S.

    1966-01-01

    A study was made of those morphological and physical soil properties considered to govern root development.

    A deep and wide-branched root system was shown only to develop in a soil containing a permanent heterogeneous pore system, formed by biological activity in the profile. Therefore a

  8. [Neotropical plant morphology].

    Science.gov (United States)

    Pérez-García, Blanca; Mendoza, Aniceto

    2002-01-01

    An analysis on plant morphology and the sources that are important to the morphologic interpretations is done. An additional analysis is presented on all published papers in this subject by the Revista de Biología Tropical since its foundation, as well as its contribution to the plant morphology development in the neotropics.

  9. Measurements of urinary kinins by HPLC-radioimmunoassay

    International Nuclear Information System (INIS)

    Fejes-Toth, G.; Naray-Fejes-Toth, A.; Froelich, J.C.

    1984-01-01

    In this paper the authors describe a method for the individual determination of urinary kinins. Extraction from the urine is performed on an Amberlite CG-50 column and kinins are eluted with formic acid. The samples are further purified and kinins are separated by reversed phase HPLC. Bradykinin and lysylbradykinin are quantified by a sensitive radioimmunoassay capable of detecting 0.1 fmol of either peptide. Procedural losses are monitored by measuring the recovery of [ 3 H]bradykinin and [ 3 H]lysylbradykinin. Simple methods for labeling of bradykinin and lysylbradykinin with tritium are also presented. Recoveries of [ 3 H]bradykinin and [ 3 H]lysylbradykinin from biological material ranged between 77 and 91%. The combination of HPLC with radioimmunoassay makes it possible to determine kinin concentrations of biological samples with a higher sensitivity and greater specificity than previous methods. (Auth.)

  10. [Studies on fingerprinting of Flos Buddleja by RP-HPLC].

    Science.gov (United States)

    Han, Peng; Cui, Ya-jun; Guo, Hong-zhu; Guo, De-an

    2004-10-01

    To establish fingerprinting of Flos Buddleja by using RP-HPLC for the quality control. The HPLC condition was as follows: Inertsil ODS-3 C18 analytical column (4.6 mm x 250 mm, 5 microm), gredient eluation with MeCN (0.1% TFA)-H2O (0.1%TFA), flow rate 1.0 mL x min(-1), detection wavelength 254 nm. 10 commercial samples were analyzed to establish a fingerprinting. Among the obtained fingerprinting, most of the detected peaks were separated effectively. The accuracy, repeatability and stability of this method were satisfied. The RSDs of relative retention time and area of aimed peaks which existed in all samples wereless than 5%. Theresults were in accordance with the request of fingerprinting. The established fingerprinting can be used for the quality control of Flos Buddleja.

  11. HPLC-DAD determination of imidacloprid in onion

    OpenAIRE

    Mandić Aljoša; Lazić Sanja; Inđić Dušanka

    2003-01-01

    Imidacloprid is an insecticide most commonly used on vegetables, potato sugar beet, fruit, cereal, maize and rice. Imidacloprid residue has been determined in spiked onion and in onion samples. Sample preparation consisted of dichlormethane extraction of imidacloprid from onion, followed by purification of the obtained extract on a LC-Florisil disposable cartridge. The HPLC-DAD method bas been developed on reversed-phase for separation of imidacloprid with a mixture of 0.01 M phosphate buffer...

  12. Optimalizace HPLC metody pro separaci tetracyklinových antibiotik

    OpenAIRE

    Kučerová, Gabriela

    2011-01-01

    The aim of this work is to develop and to optimize HPLC method for separation of a set of four tetracycline antibiotics - tetracycline, chlortetracycline, oxytetracycline, and doxycycline. Four different reversed octadecyl-silica stationary phases in various mobile phase compositions were examined in isocratic elution. The baseline resolution of all the analytes was obtained by using two columns - Astec C18 and Atlantis C18 I. The optimized separation system consisted of Atlantis C18 I. colum...

  13. Gradient Scouting in Reversed-Phase HPLC Revisited

    Science.gov (United States)

    Alcazar, A.; Jurado, J. M.; Gonzalez, A. G.

    2011-01-01

    Gradient scouting is the best way to decide the most suitable elution mode in reversed-phase high-performance liquid chromatography (RP-HPLC). A simple rule for this decision involves the evaluation of the ratio [delta]t/t[subscript G] (where [delta]t is the difference in the retention time between the last and the first peak and t[subscript G] is…

  14. [Determination of genkwanin in flos Genkwa by HPLC].

    Science.gov (United States)

    Zhang, B; Yuan, S; Xia, K

    1996-04-01

    In this paper, the method for determining genkwanin in Flos Genkwa was established by HPLC. Detected at 332nm on a Lichrosorb 5 RP-18 column with a mobile phase of methanol-water-acetic acid (65:35:5), the content of genkwanin in Flos Genkwa was determined to be 0.16%. The recovery rate was 95.46% and RSD 1.15%.

  15. High performance liquid chromatography (HPLC fingerprints and primary structure identification of corn peptides by HPLC-diode array detection and HPLC-electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chi Wang

    2016-01-01

    Full Text Available Corn peptides (CPs are reported to have many biological functions, such as facilitating alcohol metabolism, antioxidation, antitumor, antihypertension, and hepatoprotection. To develop a method for quality control, the high-performance liquid chromatography (HPLC system was applied. Twenty-eight common peaks were found in all the CPs of corn samples from Enshi, China, based on which, a fingerprinting chromatogram was established for use in quality control in future research. Subsequently, the major chemical constituents of these common peaks were identified respectively using the HPLC-diode-array detection electrospray ionization tandem mass spectrometry (DAD-ESI-MS/MS system, and 48 peptide fractions were determined ultimately. This was the first time for the majority of these peptides to be reported, and many of them contained amino acids of glutamine (Q, L and A, which might play an important role in the exhibition of the bioactivities of CPs. Many peptides had a similar primary structure to the peptides which had been proven to be bioactive such as facilitating alcohol metabolism, scavenging free radicals, and inhibiting lipid peroxidation. This systematical analysis of the primary structure of CPs facilitated subsequent studies on the relationship between the structures and functions, and could accelerate holistic research on CPs.

  16. HPLC/MS analysis of glucose and fluorodeoxyglucose

    Energy Technology Data Exchange (ETDEWEB)

    Bruder, P; Macasek, F; Patakyova, A; Buriova, E [Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, 84215 Bratislava (Slovakia)

    2001-05-31

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  17. HPLC/MS analysis of glucose and fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Bruder, P.; Macasek, F.; Patakyova, A.; Buriova, E.

    2001-01-01

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  18. [Studies on HPLC-FPS of the saponins from Semen Ziziphi Spinosae].

    Science.gov (United States)

    Wu, He-zhen; Chen, Jing; Liu, Yan-wen

    2006-09-01

    To establish a method of HPLC-fingerprint spectrum (HPLC-FPS) for the active part in Semen Ziziphi Spinosae (SZS) in order to control the quality of SZS from different places. The gradient elution mode was applied in chromatographic separation, and data were analysed by" Similarity Evaluation software" to compare the HPLC-FPS of SZS from different places. The conditions for HPLC analysis of SZS were established and the FPS of samples from different habitats showed some differences. All components in the spectrum were separated well and the HPLC fingerprint method is repeatable. The method can be used in quality assessment of SZS.

  19. HPLC ANALYSIS FOR DETERMINATION OF CHARACTERISTICS OF FRUCTO-OLIGOSACCHARIDE SYRUPS EXTRACTED FROM JERUSALEM ARTICHOKE

    Directory of Open Access Journals (Sweden)

    Sibel (YİĞİTARSLAN YILDIZ

    2009-02-01

    Full Text Available Abstract: This study was aimed to assess the feasibility of extracting fructo-oligosaccharides (degree of polymerization of 3-6 from jerusalem artichoke tubers by solvent extraction. Together with harvest date, storage time, and peeling of the raw material it was also investigated the influence of some process parameters on final dry matter, degree of polymerization and product profile of the extracts: time (10-60 min, temperature (40-80 °C, amount of solvent (30-50 ml and citric acid concentration (0-39 mmol/L. HPLC analysis showed that the most functional extracts (2.33 were obtained with mid-February harvested, 20 day-stored whole jerusalem artichoke tubers extracted with 40 ml of water containing 26 mmol/L citric acid at 60 °C for 40 min. Under those conditions, syrups with 17g of dry matter and degree of polymerization of 6 were produced. The density, viscosity, darkness and color of the syrups were found as 0.98 g/ml, 1.1 mPa-s, 0.38, and 13.3, respectively. Keywords: Fructo-oligosaccharides, HPLC, inulin, extraction, jerusalem artichoke YER ELMASINDAN ÖZÜTLENEN FRÜKTO-OLİGOSAKKARİT ŞURUPLARININ KARAKTERİSTİK ÖZELLİKLERİNİN HPLC ANALİZİ İLE BELİRLENMESİ Özet: Bu çalışmada, yer elmasından, çözücü özütleme yöntemiyle frükto-oligosakkaritlerin (polimerizasyon derecesi 3-6 özütlenebilirliğinin fizibilitesinin tayini amaçlanmıştır. Hasat zamanı, depolama süresi ve ham maddenin soyulmasının etkilerinin yanı sıra diğer bazı proses parametrelerinin (zaman (10-60 dak, sıcaklık (40-80°C, çözücü miktarı (30-50 ml ve sitrik asit derişimi (0-39 mmol/L de sonuçtaki kuru madde, polimerizasyon derecesi ve özütteki ürün profili üzerindeki etkileri incelenmiştir. HPLC analizleri, en fonksiyonel özütün (2,33 Şubat ayı ortalarında hasat edilmiş, 20 gün depolanmış, soyulmamış yer elması yumrularının, 26 mmol/L sitrik asit içeren 40 ml suyla, 60 °C'de 40 dakika süreyle

  20. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    Energy Technology Data Exchange (ETDEWEB)

    Hong, L; Altorfer, H R [Institute of Pharmaceutical Science, Swiss Federal Institute of Technology (ETH), Zurich (Switzerland); Horni, A; Hesse, M [Institute of Organic Chemistry, University of Zurich, Zurich (Switzerland)

    2005-07-01

    The radiolysis products of chloramphenicol under {gamma}-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of {gamma}-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by {gamma}-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  1. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    International Nuclear Information System (INIS)

    Hong, L.; Altorfer, H.R.; Horni, A.; Hesse, M.

    2005-01-01

    The radiolysis products of chloramphenicol under γ-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of γ-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by γ-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  2. Lignan profile of Piper cubeba, an Indonesian medicinal plant

    NARCIS (Netherlands)

    Elfahmi, [No Value; Ruslan, Komar; Batterman, Sieb; Bos, Rein; Kayser, Oliver; Woerdenbag, Herman J.; Quax, Wim J.

    The lignan profile of the aerial part of Piper cubeba L. (Piperaceae) was determined using GC, GC-MS and HPLC. The number of lignans found in the leaves was 15, followed by berries and the stalks with respectively 13 and five lignans. This is the first investigation of lignans from the leaves and

  3. HPLC-UV ATMOSPHERIC-PRESSURE IONIZATION MASS-SPECTROMETRIC DETERMINATION OF THE DOPAMINE-D2 AGONIST N-0923 AND ITS MAJOR METABOLITES AFTER OXIDATIVE-METABOLISM BY RAT-LIVER, MONKEY LIVER, AND HUMAN LIVER-MICROSOMES

    NARCIS (Netherlands)

    SWART, PJ; BRONNER, GM; BRUINS, AP; ENSING, K; TEPPER, PG; DEZEEUW, RA

    1993-01-01

    An innovative custom-built atmospheric ionization source afforded an opportunity to perform on-line LC/MS analysis and to obtain identification of metabolites without need to rely on radioactive profiling. An HPLC with a UV detector coupled to a modified R 3010 triple quadrupole mass spectrometer

  4. HPLC FOR CONTROL STABILITY OF QUERCETIN INJECTABLE DOSAGE FORM

    Directory of Open Access Journals (Sweden)

    Martynov AV

    2016-12-01

    Full Text Available Introduction. Quercetin is a flavone derivatives which known like a substances with vitamin activity, high antioxidant, antimutagenic and anticarcinogenic activity and many other types of biological activity. Wide usage of quercetin prevents their polyphenolic nature structure which does not allow a high bioavailability of pure quercetin when administered orally. This is associated with a wide spectrum variety of chemical reactions for the phenolic groups: from interaction with amino acid residues in proteins to reactions with amine heterocyclic alkaloids and polysaccharides. In our days Corvitin – one from the number of quercetin based drugs with sufficiently low levels all types toxicity, allergenic and has no irritating action on intravenous administration. In the same time quercetin cannot be used in full measure because of the limited number of publications with analysis methods, especially HPLC. Determining the stability over time of concentrate quercetin solution, as well as determining the stability of the concentrate to the original autoclave sterilization conditions is a promising direction in creating new drugs. Materials and methods The objective was to research quercetin soluble formulation samples in different conditions: 1 fresh dilute concentrate (0.9% sodium chloride; 2 the original dilute concentrate, which was stored at room temperature for 14 days in light and 3 similar to the first sample dilute concentrate, which went before breeding in autoclaving at 120 0 C for 20 minutes. The objects used in the studies were industrial drug-substance quercetin (Sinkea manufactured (China, the original pharmaceutical composition as the soluble form of quercetin for injection and aerosol applications, glycerol (Sigma, Polysorbat 80 (Merk, ethanol 96 %. For the HPLC – analysis, chromatograph "Milichrom A-02" (SiChrom, Knauer (Econova, Novosibirsk, Russia was used. Results and discussion Quercetin was identified using information on its

  5. Chemical Differentiation of Dendrobium officinale and Dendrobium devonianum by Using HPLC Fingerprints, HPLC-ESI-MS, and HPTLC Analyses

    Science.gov (United States)

    Ye, Zi; Dai, Jia-Rong; Zhang, Cheng-Gang; Lu, Ye; Wu, Lei-Lei; Gong, Amy G. W.; Wang, Zheng-Tao

    2017-01-01

    The stems of Dendrobium officinale Kimura et Migo (Dendrobii Officinalis Caulis) have a high medicinal value as a traditional Chinese medicine (TCM). Because of the limited supply, D. officinale is a high priced TCM, and therefore adulterants are commonly found in the herbal market. The dried stems of a closely related Dendrobium species, Dendrobium devonianum Paxt., are commonly used as the substitute; however, there is no effective method to distinguish the two Dendrobium species. Here, a high performance liquid chromatography (HPLC) method was successfully developed and applied to differentiate D. officinale and D. devonianum by comparing the chromatograms according to the characteristic peaks. A HPLC coupled with electrospray ionization multistage mass spectrometry (HPLC-ESI-MS) method was further applied for structural elucidation of 15 flavonoids, 5 phenolic acids, and 1 lignan in D. officinale. Among these flavonoids, 4 flavonoid C-glycosides were firstly reported in D. officinale, and violanthin and isoviolanthin were identified to be specific for D. officinale compared with D. devonianum. Then, two representative components were used as chemical markers. A rapid and reliable high performance thin layer chromatography (HPTLC) method was applied in distinguishing D. officinale from D. devonianum. The results of this work have demonstrated that these developed analytical methods can be used to discriminate D. officinale and D. devonianum effectively and conveniently. PMID:28769988

  6. Qualitative and Quantitative Analysis of Lignan Constituents in Caulis Trachelospermi by HPLC-QTOF-MS and HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiao-Ting Liu

    2015-05-01

    Full Text Available A high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass (HPLC-QTOF-MS and ultraviolet spectrometry (HPLC-UV was established for simultaneous qualitative and quantitative analysis of the major chemical constituents in Caulis Trachelospermi, respectively. The analysis was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 5 μm using a binary gradient system of water and methanol, with ultraviolet absorption at 230 nm. Based on high-resolution ESI-MS/MS fragmentation behaviors of the reference standards, the characteristic cleavage patterns of lignano-9, 9'-lactones and lignano-8'-hydroxy-9, 9'-lactones were obtained. The results demonstrated that the characteristic fragmentation patterns are valuable for identifying and differentiating lignano-9,9'-lactones and lignano-8'-hydroxy-9,9'-lactones. As such, a total of 25 compounds in Caulis Trachelospermi were unambiguously or tentatively identified via comparisons with reference standards or literature. In addition, 14 dibenzylbutyrolatone lignans were simultaneously quantified in Caulis Trachelospermi by HPLC-UV method. The method is suitable for the qualitative and quantitative analyses of dibenzylbutyrolatone lignans in Caulis Trachelospermi.

  7. Development of a HPLC method for determination of four UV filters in sunscreen and its application to skin penetration studies.

    Science.gov (United States)

    Souza, Carla; Maia Campos, Patrícia M B G

    2017-12-01

    This study describes the development, validation and application of a high-performance liquid chromatography (HPLC) method for the simultaneous determination of the in vitro skin penetration profile of four UV filters on porcine skin. Experiments were carried out on a gel-cream formulation containing the following UV filters: diethylamino hydroxybenzoyl hexyl benzoate (DHHB), bis-ethylhexyloxyphenol methoxyphenyl triazine (BEMT), methylene bis-benzotriazolyl tetramethylbutylphenol (MBBT) and ethylhexyl triazone (EHT). The HPLC method demonstrated suitable selectivity, linearity (10.0-50.0 μg/mL), precision, accuracy and recovery from porcine skin and sunscreen formulation. The in vitro skin penetration profile was evaluated using Franz vertical diffusion cells for 24 h after application on porcine ear skin. None of the UV filters penetrated the porcine skin. Most of them stayed on the skin surface (>90%) and only BEMT, EHT and DHHB reached the dermis plus epidermis layer. These results are in agreement with previous results in the literature. Therefore, the analytical method was useful to evaluate the in vitro skin penetration of the UV filters and may help the development of safer and effective sunscreen products. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Biological variability dominates and influences analytical variance in HPLC-ECD studies of the human plasma metabolome

    Directory of Open Access Journals (Sweden)

    Willett Walter C

    2007-11-01

    Full Text Available Abstract Background Biomarker-based assessments of biological samples are widespread in clinical, pre-clinical, and epidemiological investigations. We previously developed serum metabolomic profiles assessed by HPLC-separations coupled with coulometric array detection that can accurately identify ad libitum fed and caloric-restricted rats. These profiles are being adapted for human epidemiology studies, given the importance of energy balance in human disease. Methods Human plasma samples were biochemically analyzed using HPLC separations coupled with coulometric electrode array detection. Results We identified these markers/metabolites in human plasma, and then used them to determine which human samples represent blinded duplicates with 100% accuracy (N = 30 of 30. At least 47 of 61 metabolites tested were sufficiently stable for use even after 48 hours of exposure to shipping conditions. Stability of some metabolites differed between individuals (N = 10 at 0, 24, and 48 hours, suggesting the influence of some biological factors on parameters normally considered as analytical. Conclusion Overall analytical precision (mean median CV, ~9% and total between-person variation (median CV, ~50–70% appear well suited to enable use of metabolomics markers in human clinical trials and epidemiological studies, including studies of the effect of caloric intake and balance on long-term cancer risk.

  9. Pink berry grape (Vitis vinifera L.) characterization: Reflectance spectroscopy, HPLC and molecular markers.

    Science.gov (United States)

    Rustioni, Laura; De Lorenzis, Gabriella; Hârţa, Monica; Failla, Osvaldo

    2016-01-01

    Color has a fundamental role for the qualitative evaluation and cultivar characterization of fruits. In grape, a normally functional pigment biosynthesis leads to the accumulation of a high quantity of anthocyanins. In this work, 28 Vitis vinifera L. cultivars accumulating low anthocyanins in berries were studied to characterize the biosynthetic dysfunctions in both a phenotypic and genotypic point of view. Reflectance spectroscopy, HPLC profiles and molecular markers related to VvMybA1 and VvMybA2 genes allowed a detailed description of the pigment-related characteristics of these cultivars. Data were consistent concerning the heterozygosity of the non-functional allele in both investigated genes, resulting in a low colored phenotype as described by reflectance. However, the variability in berry colour among our samples was not fully explained by MybA locus, probably due to specific interferences among the biosynthetic pathways, as suggested by the anthocyanin profile variations detected among our samples. The results presented in this work confirmed the importance of the genetic background: grapes accumulating high levels of cyanidin-3-O-glucosides (di-substituted anthocyanin) are generally originated by white cultivar retro-mutations and they seem to preserve the anomalies in the flavonoid hydroxylases enzymes which negatively affect the synthesis of tri-substituted anthocyanins. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

  10. Molecular characterization and bio-functional property determination using SDS-PAGE and RP-HPLC of protein fractions from two Nigella species.

    Science.gov (United States)

    Alu'datt, Muhammad H; Rababah, Taha; Alhamad, Mohammad N; Alodat, Moh'd; Al-Mahasneh, Majdi A; Gammoh, Sana; Ereifej, Khalil; Almajwal, Ali; Kubow, Stan

    2017-09-01

    This study aimed to investigate the molecular and bio-functional properties of protein fractions from Nigella damascena and Nigella arvensis, including the albumin, globulin, glutein-1, glutein-2 and prolamin fractions. Protein subunits were not observed in globulin and prolamin fractions. No peaks appeared in RP-HPLC chromatograms of globulin for either species. Two predominant peaks were observed in the RP-HPLC profiles of all protein fractions. Proteins separated by RP-HPLC have potential inhibitory and antioxidant activities in all fractions. Optimum ACE-inhibitory and antioxidant activities of proteins separated by RP-HPLC were observed in glutein-2 and albumin, respectively, for both species. For pepsin and combined pepsin-trypsin hydrolyses, the highest degree of hydrolysis (DH) was obtained in glutein-2 fraction of Nigella arvensis. Highest ACE-inhibitory activity of hydrolyzed protein fractions was found at 4h via pepsin hydrolysis in globulin fraction of Nigella damascena. Highest antioxidant activities of hydrolyzed protein fractions were found in glutelin-2 for both species. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Serum Protein Profile Study of Clinical Samples Using High Performance Liquid Chromatography-Laser Induced Fluorescence

    DEFF Research Database (Denmark)

    Karemore, Gopal Raghunath; Ukendt, Sujatha; Rai, Lavanya

    2009-01-01

    The serum protein profiles of normal subjects, patients diagnosed with cervical cancer, and oral cancer were recorded using High Performance Liquid Chromatography combined with Laser Induced Fluorescence detection (HPLC-LIF). Serum protein profiles of the above three classes were tested for estab...

  12. Protein Profile study of clinical samples using Laser Induced Fluorescence as the detection method

    DEFF Research Database (Denmark)

    Karemore, Gopal Raghunath; Raja, Sujatha N.; Rai, Lavanya

    2009-01-01

      Protein profiles of tissue homogenates were recorded using HPLC separation and LIF detection method. The samples were collected from volunteers with clinically normal or cervical cancer conditions. It is shown that the protein profile can be classified as belonging to malignant or normal state ...

  13. Data Profiling

    OpenAIRE

    Hladíková, Radka

    2010-01-01

    Title: Data Profiling Author: Radka Hladíková Department: Department of Software Engineering Supervisor: Ing. Vladimír Kyjonka Supervisor's e-mail address: Abstract: This thesis puts mind on problems with data quality and data profiling. This Work analyses and summarizes problems of data quality, data defects, process of data quality, data quality assessment and data profiling. The main topic is data profiling as a process of researching data available in existing...

  14. Determination of blood cyanide by HPLC-MS.

    Science.gov (United States)

    Tracqui, A; Raul, J S; Géraut, A; Berthelon, L; Ludes, B

    2002-04-01

    An original high-performance liquid chromatographic-mass spectrometric (HPLC-MS) procedure was developed for the determination of cyanide (CN) in whole blood. After the addition of K13C15N as internal standard, blood was placed in a microdiffusion device, the inner well of which was filled with a mixture of taurine (50mM in water)/naphthalene-2,3-dicarboxaldehyde (NDA, 10mM in methanol)/methanol/ concentrated (approximately 20%) ammonia solution (25:25:45:5, v/v). Concentrated H2SO4 was added to the blood sample, and the microdiffusion chamber was sealed. After 30 min of gentle agitation, 2 microL of the contents of the inner vial were pipetted and directly injected onto a NovaPak C18 HPLC column. Separation was performed by a gradient of acetonitrile in 2mM NH4COOH, pH 3.0 buffer (35-80% in 10 min). Detection was done with a Perkin-Elmer Sciex API-100 mass analyzer with an ionspray interface, operated in the negative ionization mode. MS data were collected as either TIC or SIM at m/z (299 + 191) and (301 + 193) for the derivatives formed with CN and 13C15N, respectively. Inspired by previous works dealing with the complexation of CN by NDA + taurine to form a 1-cyano [f] benzoisoindole derivative analyzed by HPLC-fluorimetry, this method appears simple, rapid, and extremely specific. Limits of detection and quantitation for blood CN are 5 and 15 ng/mL, respectively. The use of 13C15N as internal standard allows the quantitation of CN with elegance and accuracy in comparison with previously reported methods.

  15. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-09-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetone+acrolein. Three different types of samples (rural, urban, petrol emission) were successfully analyzed

  16. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-01-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs

  17. [Determination of 10-HDA in honeybee body by HPLC].

    Science.gov (United States)

    Fan, H; He, C; Han, H

    1999-05-01

    In the present work we found that in the honeybee body there exists an unsaturated fatty acid, trans-10-hydroxy-2-decenoic acid (10-HDA), which was known only to be present in royal jelly. We established the analytical method of 10-HDA in honeybee body by HPLC and simplified the extraction method of 10-HDA. In the optimum conditions the linear range of detection was 10-1,000 ng, the correlation coefficient was 0.9998, the recovery was 96.5%-99.2% and the detectable limit was 0.53 microgram/g.

  18. Generalized Morphology using Sponges

    NARCIS (Netherlands)

    van de Gronde, Jasper J.; Roerdink, Jos B.T.M.

    2016-01-01

    Mathematical morphology has traditionally been grounded in lattice theory. For non-scalar data lattices often prove too restrictive, however. In this paper we present a more general alternative, sponges, that still allows useful definitions of various properties and concepts from morphological

  19. Karolinske psychodynamic profile (KAPP)

    DEFF Research Database (Denmark)

    Mathiesen, Birgit Bork; Søgaard, Ulf

    2006-01-01

    psykologiske testmetoder, assesment, Karolinska psychodynamic profile (KAPP), psykodynamisk profil......psykologiske testmetoder, assesment, Karolinska psychodynamic profile (KAPP), psykodynamisk profil...

  20. Extrinsic morphology of graphene

    International Nuclear Information System (INIS)

    Li, Teng

    2011-01-01

    Graphene is intrinsically non-flat and corrugates randomly. Since the corrugating physics of atomically thin graphene is strongly tied to its electronics properties, randomly corrugating morphology of graphene poses a significant challenge to its application in nanoelectronic devices for which precise (digital) control is the key. Recent studies revealed that the morphology of substrate-supported graphene is regulated by the graphene–substrate interaction, thus is distinct from the random intrinsic morphology of freestanding graphene. The regulated extrinsic morphology of graphene sheds light on new pathways to fine tune the properties of graphene. To guide further research to explore these fertile opportunities, this paper reviews recent progress on modeling and experimental studies of the extrinsic morphology of graphene under a wide range of external regulation, including two-dimensional and one-dimensional substrate surface features and one-dimensional and zero-dimensional nanoscale scaffolds (e.g. nanowires and nanoparticles)

  1. Enrichment of steroid hormones in water with porous and hydrophobic polymer-based SPE followed by HPLC-UV determination.

    Science.gov (United States)

    Hu, Yinfen; Zhang, Man; Tong, Changlun; Wu, Jianmin; Liu, Weiping

    2013-10-01

    There have been great concerns about the persistence of steroid hormones in surface water. Since the concentrations of these compounds in water samples are usually at a trace level, the efficient enrichment of steroid hormones is vital for further analysis. In this work, a porous and hydrophobic polymer was synthesized and characterized. The composition of solvent used as porogen in the synthetic process was shown to have an effect on the morphology of the polymer, which was successfully used as an SPE sorbent for simultaneously enriching steroid hormones in surface water samples. The recoveries of the steroid hormones on the custom-made polymer ranged from 93.4 to 106.2%, whereas those on commercialized ENVI-18, LC-18, and Oasis HLB ranged from 54.8 to 104.9, 66 to 93.6, and 77.2 to 106%, respectively. Five types of steroid hormones were simultaneously measured using HPLC-UV after they were enriched by the custom-made sorbent. Based on these findings, the SPE-HPLC method was developed. The LODs of this method for estriol, estradiol, estrone, androstenedione, progesterone were 0.07, 0.43, 0.61, 0.27, and 0.42 μg/L, respectively, while precision and reproducibility RSDs were <6.40 and 7.49%, respectively. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. [Assay of Tetramethylpyrazine in Szechwan Lovage Rhizome and Cnidium Rhizome by HPLC-DAD-MS].

    Science.gov (United States)

    Hong, Yuan-lin; Jin, Yu-qing; Yao, Yi-xin; Lin, Mao-yi; Wei, Bo-ping; Jiang, Wei-dong; Lu, Guang-hua

    2015-01-01

    To quantity the amount of tetramethylpyrazine in Szechwan Lovage Rhizome (Chuanxiong, the rhizome of Ligusticum chuanxiong Hort., CX) and Cnidium Rhizome(Japanese Chuanxiong, the rhizome of Cnidium officinale Makino, JCX) for quality assessment. An HPLC-DAD-MS technique was employed to detect tetramethylpyrazine in 27 CX and 10 JCX samples. Tetramethylpyrazine was separated on a Waters Symmetry C,, column (250 mm x 4. 6 mm, 5 µm). The mobile phase was methanol-acetonitrile-water(27: 1: 72) at a flow rate of 1. 0 mL/min. The column temperature was 35 °C. DAD detection wavelength was 280 nm, while electrospray ionization detector was set at positive mode to collect MS spectrum. In the total of 37 herb samples, 11 samples were found to contain tetramethylpyrazine with the mean amount of 2. 19 µg/g(n = 11). 6 of 27 CX samples and 5 of 10 JCX sample were found the existence of tetramethylpyrazine with the amount of 0. 60 - 11. 75 µg and 0. 61 - 3. 05 µg/g,respectively. The correlation was not found between tetramethylpyrazine and the cultivation area, morphological character, processing or storage method for CX and JCX samples. It was possible that tetramethylpyrazine resulted from the microbes in soil. The developed method is accurate to quantify tetramethylpyrazine in CX and JCX herbs. Both the two herbs indeed contain tetramethylpyrazine, but it is not suitable to be a chemical marker to assess the quality of CX and JCX owing to low content.

  3. Quantification of furanoheliangolides by HPLC and GC Quantificação dos furanoeliangolidos por HPLC e CG

    Directory of Open Access Journals (Sweden)

    Pierre Alexandre dos Santos

    2003-09-01

    Full Text Available The development and comparison of two analytical methods (HPLC and GC for the quantification of the most common furanoheliangolides from Lychnophora is reported in this paper. Both methods are sensitive and suitable for quantification of these metabolites.Neste trabalho são descritos o desenvolvimento e comparação de dois métodos analíticos (CLAE e CG para quantificação dos furanoeliangolidos mais comuns em Lychnophora.Ambos os métodos são sensíveis e adequados para a quantificação desses metabólitos.

  4. Quantification of furanoheliangolides by HPLC and GC Quantificação dos furanoeliangolidos por HPLC e CG

    OpenAIRE

    Pierre Alexandre dos Santos; Izabel Cristina Casanova Turati; José Carlos Tomaz; Norberto Peporine Lopes

    2003-01-01

    The development and comparison of two analytical methods (HPLC and GC) for the quantification of the most common furanoheliangolides from Lychnophora is reported in this paper. Both methods are sensitive and suitable for quantification of these metabolites.Neste trabalho são descritos o desenvolvimento e comparação de dois métodos analíticos (CLAE e CG) para quantificação dos furanoeliangolidos mais comuns em Lychnophora.Ambos os métodos são sensíveis e adequados para a quantificação desses m...

  5. [Determination method of polysorbates in powdered soup by HPLC].

    Science.gov (United States)

    Takeda, Y; Abe, Y; Ishiwata, H; Yamada, T

    2001-04-01

    A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.

  6. Retinol analysis in dried blood spots by HPLC.

    Science.gov (United States)

    Craft, N E; Haitema, T; Brindle, L K; Yamini, S; Humphrey, J H; West, K P

    2000-04-01

    There are many advantages to measuring vitamin A in dried blood spots (DBS) from a finger prick as compared to plasma collected by venipuncture. The advantages include easier collection, transport and storage; accessibility to younger and more remote populations; and decreased risk of disease transmission. We describe a method for the extraction of retinol from DBS for analysis by HPLC and initial comparison to plasma retinol. The effects of various buffers, detergents, antioxidants and chelators were evaluated to establish the most effective approach to elute the retinol: retinol binding protein (holo-RBP) complex from the blood collection cards. The process involves ultrasonic agitation to elute holo-RBP into a phosphate buffer containing an antioxidant and metal chelator. The holo-RBP complex was denatured by the addition of ethanol containing additional antioxidants permitting the extraction of free retinol into hexane. Following solvent evaporation, the extract was dissolved in methanol for HPLC analysis. The initial measured retinol levels in freshly collected DBS declined for 6-10 d whether stored at 25, 4 or -20 degrees C, but remained consistent thereafter (homeostatic). By incorporating a "recovery/volume adjustment" factor, measured retinol values in homeostatic DBS were adjusted to the equivalent of plasma retinol. For 17 normal adults, the correlation coefficient was 0.90 between plasma retinol and adjusted DBS retinol in samples that had been stored at -70 degrees C for < 9 mo. The use of this new sample matrix for vitamin A assessment will allow access to previously unavailable populations.

  7. Pungency Quantitation of Hot Pepper Sauces Using HPLC

    Science.gov (United States)

    Betts, Thomas A.

    1999-02-01

    A class of compounds known as capsaicinoids are responsible for the "heat" of hot peppers. To determine the pungency of a particular pepper or pepper product, one may quantify the capsaicinoids and relate those concentrations to the perceived heat. The format of the laboratory described here allows students to collectively develop an HPLC method for the quantitation of the two predominant capsaicinoids (capsaicin and dihydrocapsaicin) in hot-pepper products. Each small group of students investigated one of the following aspects of the method: detector wavelength, mobile-phase composition, extraction of capsaicinoids, calibration, and quantitation. The format of the lab forced students to communicate and cooperate to develop this method. The resulting HPLC method involves extraction with acetonitrile followed by solid-phase extraction clean-up, an isocratic 80:20 methanol-water mobile phase, a 4.6 mm by 25 cm C-18 column, and UV absorbance detection at 284 nm. The method developed by the students was then applied to the quantitation of capsaicinoids in a variety of hot pepper sauces. Editor's Note on Hazards in our April 2000 issue addresses the above.

  8. HPLC assisted Raman spectroscopic studies on bladder cancer

    Science.gov (United States)

    Zha, W. L.; Cheng, Y.; Yu, W.; Zhang, X. B.; Shen, A. G.; Hu, J. M.

    2015-04-01

    We applied confocal Raman spectroscopy to investigate 12 normal bladder tissues and 30 tumor tissues, and then depicted the spectral differences between the normal and the tumor tissues and the potential canceration mechanism with the aid of the high-performance liquid chromatographic (HPLC) technique. Normal tissues were demonstrated to contain higher tryptophan, cholesterol and lipid content, while bladder tumor tissues were rich in nucleic acids, collagen and carotenoids. In particular, β-carotene, one of the major types of carotenoids, was found through HPLC analysis of the extract of bladder tissues. The statistical software SPSS was applied to classify the spectra of the two types of tissues according to their differences. The sensitivity and specificity of 96.7 and 66.7% were obtained, respectively. In addition, different layers of the bladder wall including mucosa (lumps), muscle and adipose bladder tissue were analyzed by Raman mapping technique in response to previous Raman studies of bladder tissues. All of these will play an important role as a directive tool for the future diagnosis of bladder cancer in vivo.

  9. Analysis of the radiochemical purity of 18F-FDG by HPLC

    International Nuclear Information System (INIS)

    Chen Liguang; Tang Anwu; He Shanzhen; Chen Yulong

    2001-01-01

    The radiochemical purity (RCP) of 18 F-FDG is analyzed by HPLC. Eighty-five percent acetonitrile is used as the eluting solution. Carbon hydrate column is used as separation column. The t R of 18 F - is 6.50 min and 18 F-FDG is 9.00 min. HPLC take less time and has higher sensitivity than TLC for the same sample at the same time. So HPLC excels TLC in analyzing RCP of 18 F-FDG

  10. Multi-Analyte Separation Methods for HPLC Determination of the Active Ingredients of Pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Virtics, I.; Korsós, I.; Homoki, E.; Lantos, J. [Plant Protection and Soil Conservation Service of Szabolcs-Szatmár-Bereg County, Nyíregyháza (Hungary)

    2009-07-15

    The practical quality control of selected pesticides, such as carbamates, organophosphorous compounds, phthalimides, pyrethroids, with HPLC is described. Detailed descriptions are given of materials and methods used, including sample preparation and HPLC operating conditions. The relationship between pH value of the HPLC eluent and the logP{sub ow} is discussed, illustrated by chromatograms, graphics and tables. The results are also compared with those elaborated by. E. Dudar and presented above. (author)

  11. Identification and quantification of flavonoids and chromes in Baeckea frutescens by using HPLC coupled with diode-array detection and quadruple time-of-flight mass spectrometry.

    Science.gov (United States)

    Jia, Bei-Xi; Huangfu, Qian-Qian; Ren, Feng-Xiao; Jia, Lu; Zhang, Yan-Bing; Liu, Hong-Min; Yang, Jie; Wang, Qiang

    2015-01-01

    This article marks the first report on high-performance liquid chromatography (HPLC) coupled with diode-array detection (DAD) and quadruple time-of-flight mass spectrometry (Q-TOF/MS) for the identification and quantification of main bioactive constituents in Baeckea frutescens. In total, 24 compounds were identified or tentatively characterised based on their retention behaviours, UV profiles and MS fragment information. Furthermore, a validated method with good linearity, sensitivity, precision, stability, repeatability and accuracy was successfully applied for simultaneous determination of five flavonoids and one chromone in different plant parts of B. frutescens collected at different harvest times, and their dynamic contents revealed the appropriate harvest times. The established HPLC-DAD-Q-TOF/MS using multi-bioactive markers was proved to be a validated strategy for the quality evaluation on both raw materials and related products of B. frutescens.

  12. Identification and determination of the major constituents in traditional Chinese medicine Longdan Xiegan Pill by HPLC-DAD-ESI-MS

    Directory of Open Access Journals (Sweden)

    Hui Liu

    2011-02-01

    Full Text Available A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill. The chemical profile of the twelve compounds, including geniposidic acid (1, geniposide(2, gentiopicroside(3, liquiritin(4, crocin(5, baicalin(6, wogonoside(7, baicalein(8, glycyrrhizic acid (9, wogonin (10, oroxylin A (11 and aristolochic acid A (12, was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS. The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4. 6 mm, 5 μm with a gradient solvent system of acetonitrile-0. 1% aqueous formic acid. The validation was carried out and the linearities (r > 0. 9996, repeatability (RSD<1. 8%, intra- and inter-day precision (RSD< 1. 3%, and recoveries (ranging from 96. 6% to 103. 4% were acceptable. The limits of detection (LOD of these compounds ranged from 0.29 to 4. 17 ng. Aristolochic acid A, which is the toxic ingredient, was not detected in all the batches of Longdan Xiegan Pill. Furthermore, hierarchical cluster analysis was used to evaluate the variation of the herbal prescription. The proposed method is simple, effective and suitable for the quality control of this traditional Chinese medicine (TCM. Keywords: Longdan Xiegan Pill, high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS, qualitative evaluation, aristolochic acid A, hierarchical cluster analysis

  13. Optimizing an online SPE-HPLC method for analysis of (R)-[11C]1-(2-chlorophenyl)-N-methyl-N-(1-methylpropyl)- 3-isoquinolinecarboxamide [(R)-[11C]PK11195] and its metabolites in humans

    International Nuclear Information System (INIS)

    Greuter, Henri N.J.M.; van Ophemert, Patricia L.B.; Luurtsema, Gert; van Berckel, Bart N.M.; Franssen, Eric J.F.; Windhorst, Bert D.; Lammertsma, Adriaan A.

    2005-01-01

    (R)-[ 11 C]PK11195 is used as a positron emission tomography tracer for activated microglia in several neurological disorders. Quantification of specific binding requires a metabolite-corrected plasma input function. In this study, a high-performance liquid chromatography (HPLC) procedure with online solid phase extraction was modified for analyzing (R)-[ 11 C]PK11195 plasma samples, yielding total sample recoveries of more than 98%. When applied to human studies, the use of two HPLC systems enabled analysis of up to seven plasma samples under regular conditions. Online radioactivity detection was compared with offline sample measurements of HPLC profiles. Offline measurements provided the most reliable results especially for late plasma samples. In 10 patients, an average decrease of parent compound from 94.6% at 2.5 min to 45.2% at 1 h after administration was observed

  14. Determination of cadmium and lead species and phytochelatins in pea (Pisum sativum) by HPLC-ICPMS and HPLC-ESIMSn

    International Nuclear Information System (INIS)

    Baralkiewicz, D.; Magorzata, K.; Piechalak, A.; Tomaszewska, B.

    2009-01-01

    Full text: Trace elements play an important role in the functioning of life on our planet. Some of them can be highly toxic, whereas others can be essential. These effects are very often related to particular form in which the element is present. Often these different chemical forms of a particular element or its compounds are referred to as 'species'. Cadmium and lead are widespread heavy metal pollutants released into the environment by human activities. The presence of Pb 2+ and Cd 2+ in the environment leads to a numerous disturbances in many metabolic processes in plants. Inhibition of growth is a major symptom. Hyphenated techniques, such as HPLC-ICPMS and HPLC-ESIMSn seem to be the best analytical instruments to study metal speciation in plants. In our study, we used hyphenated techniques to identify compounds engaged in Cd and Pb metabolism and to perform analysis of metal complexes induced in Pisum sativum exposed to cadmium and lead. These identified compounds might be valuable source of information to study metal accumulation mechanism for bioremediation processes. (author)

  15. Determination of some psychotropic drugs in serum and saliva samples by HPLC-DAD and HPLC MS.

    Science.gov (United States)

    Petruczynik, A; Wróblewski, K; Szultka-Młyńska, M; Buszewski, B; Karakuła-Juchnowicz, H; Gajewski, J; Morylowska-Topolska, J; Waksmundzka-Hajnos, M

    2016-08-05

    A simple, rapid and sensitive HPLC-DAD method has been developed and validated for the simultaneous determination of seven psychotropic drugs (risperidone, citalopram, clozapine,quetiapine, levomepromazine, perazine and aripiprazole) in human serum or saliva samples. The chromatographic analyses were performed on a XSELECT CSH Phenyl-Hexyl column with a mobile phase containing methanol, acetate buffer at pH 3.5 and 0.025mL(-1) diethylamine. The influence of concentration of methanol in injection samples and injection volume on peak symmetry and system efficiency was examined.The full separation of all investigated drugs, good peaks' symmetry and simultaneously high systems efficiency were obtained in applied chromatographic system. The method is suitable for the analysis of investigated drugs in human plasma or saliva for psychiatric patients for control of pharmacotherapy, particularly in combination therapy. HPLC-MS was applied for verification of the presence of drugs and their metabolites in serum and saliva samples from patients. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. HPLC-MS technique for radiopharmaceuticals research and control

    Energy Technology Data Exchange (ETDEWEB)

    Macasek, F; Bruder, P [Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Buriova, E [Cyclotron Centre of the Slovak Republic, Slovak Office of Standards, Metrology and Testing, Bratislava (Slovakia)

    2002-03-01

    A liquid chromatography/refractive index detector/radiometric detector/ mass spectrometric detector combination (Agilent 1100 HPLC/RAD/DAD/RID/MSD system) is used as a complex technique for quality assessment of radiopharmaceuticals such as 2-deoxy-2-[{sup 18}F]fluoro-D-glucose (FDG). Optimisation of HPLC/MS analysis was performed investigating the electrospray ionisation (ESI) analytical signal of the mass spectrometer as a function of solvent composition. The anion-exchange eluents applied as specified by the pharmacopoeia are not suitable for ESI detection due to high ion concentrations. Therefore, solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analysed by flow injection analysis (FIA) and chromatographically. The best analytical response was obtained with acetonitrile : 0.25% ammonium formate = 80:20 solutions. The most intense MSD signals of FDG in ammonium formate were obtained for the following complex ions: (i) positive ions: fdg.NH{sub 4}{sup +}, fdg.Na{sup +} and (fdg{sub 2}-CH{sub 3}O).Na{sup +} (m/z = 200, 205 and 344); (ii) negative ions: fdg.Cl{sup -} and fdg.HCOO{sup -} (m/z= 217 and 227). The HPLC-MS analysis with Zorbax C-18 and Asahipak-NH2P50 columns gave evidence of admixtures and radiolytic formation of deoxyglucose, deoxychloro-glucose, erythrose, erythritol, gluconic acid, lactose, raffinose, saccharic acid, sorbitol/[{sup 19}F]FDG, sorbitol/[{sup 19}F]FDG, xylitol, and other compounds. However, radiometric analysis of expired samples of [{sup 18}F]FDG gave evidence of a very high radiation stability of its water-ethanol solutions at the point of output of radioactive products. Remarkable is the exceedingly high complexity of the mass spectra of FDG as compared to glucose. Therefore, further research concerns the influence of sodium chloride, linearity of signal response, impurities (mannitol, mannose etc.) interference, and

  17. HPLC-MS technique for radiopharmaceuticals research and control

    International Nuclear Information System (INIS)

    Macasek, F.; Bruder, P.; Buriova, E.

    2002-01-01

    A liquid chromatography/refractive index detector/radiometric detector/ mass spectrometric detector combination (Agilent 1100 HPLC/RAD/DAD/RID/MSD system) is used as a complex technique for quality assessment of radiopharmaceuticals such as 2-deoxy-2-[ 18 F]fluoro-D-glucose (FDG). Optimisation of HPLC/MS analysis was performed investigating the electrospray ionisation (ESI) analytical signal of the mass spectrometer as a function of solvent composition. The anion-exchange eluents applied as specified by the pharmacopoeia are not suitable for ESI detection due to high ion concentrations. Therefore, solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analysed by flow injection analysis (FIA) and chromatographically. The best analytical response was obtained with acetonitrile : 0.25% ammonium formate = 80:20 solutions. The most intense MSD signals of FDG in ammonium formate were obtained for the following complex ions: (i) positive ions: fdg.NH 4 + , fdg.Na + and (fdg 2 -CH 3 O).Na + (m/z = 200, 205 and 344); (ii) negative ions: fdg.Cl - and fdg.HCOO - (m/z= 217 and 227). The HPLC-MS analysis with Zorbax C-18 and Asahipak-NH2P50 columns gave evidence of admixtures and radiolytic formation of deoxyglucose, deoxychloro-glucose, erythrose, erythritol, gluconic acid, lactose, raffinose, saccharic acid, sorbitol/[ 19 F]FDG, sorbitol/[ 19 F]FDG, xylitol, and other compounds. However, radiometric analysis of expired samples of [ 18 F]FDG gave evidence of a very high radiation stability of its water-ethanol solutions at the point of output of radioactive products. Remarkable is the exceedingly high complexity of the mass spectra of FDG as compared to glucose. Therefore, further research concerns the influence of sodium chloride, linearity of signal response, impurities (mannitol, mannose etc.) interference, and robustness of the MS analysis, with special attention

  18. Morphological neural networks

    Energy Technology Data Exchange (ETDEWEB)

    Ritter, G.X.; Sussner, P. [Univ. of Florida, Gainesville, FL (United States)

    1996-12-31

    The theory of artificial neural networks has been successfully applied to a wide variety of pattern recognition problems. In this theory, the first step in computing the next state of a neuron or in performing the next layer neural network computation involves the linear operation of multiplying neural values by their synaptic strengths and adding the results. Thresholding usually follows the linear operation in order to provide for nonlinearity of the network. In this paper we introduce a novel class of neural networks, called morphological neural networks, in which the operations of multiplication and addition are replaced by addition and maximum (or minimum), respectively. By taking the maximum (or minimum) of sums instead of the sum of products, morphological network computation is nonlinear before thresholding. As a consequence, the properties of morphological neural networks are drastically different than those of traditional neural network models. In this paper we consider some of these differences and provide some particular examples of morphological neural network.

  19. FABRICATION, MORPHOLOGICAL AND OPTOELECTRONIC ...

    African Journals Online (AJOL)

    2014-12-31

    Dec 31, 2014 ... porous silicon has better optoelectronic properties than bulk .... Measurement: The morphological properties of PS layer such as nanocrystalline size, the .... excess carrier removal by internal recombination and diffusion.

  20. HPLC Determination of Polyphenols from Calendula officinalis L. Flowers

    Directory of Open Access Journals (Sweden)

    Frum Adina

    2017-12-01

    Full Text Available Romanian spontaneous flora provides a lot of resources for the determination of different chemical compounds. This study uses flower samples from Calendula officinalis L. extracted through maceration. The chemical compounds determined were: (+-catechin, caffeic acid, chlorogenic acid, cinnamic acid, ferulic acid, gallic acid, rutin, resveratrol and quercetin. They were analyzed by using an optimized HPLC method. (+-Catechin, caffeic acid, chlorogenic acid and quercetin could not be identified in the analyzed samples. The greatest amount of phenolic compound found was rutin and the smallest quantity was determined for ferulic acid. The quantified compounds have proven to have benefits regarding human health, thus they can be used as functional compounds and can be included in food products and food supplements.

  1. Quantitative analysis of PMR-15 polyimide resin by HPLC

    Science.gov (United States)

    Roberts, Gary D.; Lauver, Richard W.

    1987-01-01

    The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

  2. HPLC identification of isoniazid residues in bovine milk

    Directory of Open Access Journals (Sweden)

    Leite R.M.H.

    2000-01-01

    Full Text Available The high pressure liquid chromatography (HPLC was used for the identification of isoniazid (isonicotinic acid hydrazide in the milk of cattle treated with a dose of 25 mg/kg/day in alternated days. The effect of milk pasteurization on the isoniazid residue concentration was also studied. The drug excretion presented a cyclic variation, with higher levels in the first day after administration (aa, a mean of 1104.48µg/l, and a decrease two days aa, with a mean of 104.12µg/l. Four days after the last administration of the drug it was not possible to identify residues of isoniazid in the milk of treated animals. Body weight and milk yield influenced the amount of the excreted drug, and pasteurization decreased (mean 47.07% the concentration of isoniazid residue in milk.

  3. Anthocyanins and antioxidant capacities of six Chilean berries by HPLC-HR-ESI-ToF-MS.

    Science.gov (United States)

    Ramirez, Javier E; Zambrano, Ricardo; Sepúlveda, Beatriz; Kennelly, Edward J; Simirgiotis, Mario J

    2015-06-01

    The HPLC profiles of six fruits endemic of the VIII region of Chile were investigated using high resolution mass analysis (HR-ToF-ESI-MS). The anthocyanin fingerprints generated for the fruits were compared and the antioxidant capacities measured by the scavenging of the DPPH radical, the ferric reducing antioxidant power (FRAP), the superoxide anion scavenging activity assay (SA), and correlated with the inhibition of lipid peroxidation in human erythrocytes (LP) and total content of phenolics, flavonoids and anthocyanins measured by spectroscopic methods. Several anthocyanins were identified, including 3-O-glycosides derivatives of delphinidin, cyanidin, petunidin, peonidin and malvidin. Three phenolic acids (feruloyl-quinic acid, chlorogenic acid, and neochlorogenic acid) and five flavonols (hyperoside, isoquercitrin, quercetin, rutin, myricetin and isorhamnetin) were also identified. Calafate fruits showed the highest antioxidant activity. However, the highest LP activity was found for Chilean blueberries (>95%) followed by calafate fruits (91.27%) and luma (83.4%). Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Ramalina capitata (Ach.) Nyl. acetone extract: HPLC analysis, genotoxicity, cholinesterase, antioxidant and antibacterial activity.

    Science.gov (United States)

    Zrnzevic, Ivana; Stankovic, Miroslava; Stankov Jovanovic, Vesna; Mitic, Violeta; Dordevic, Aleksandra; Zlatanovic, Ivana; Stojanovic, Gordana

    2017-01-01

    In the present investigation, effects of Ramalina capitata acetone extract on micronucleus distribution on human lymphocytes, on cholinesterase activity and antioxidant activity (by the CUPRAC method) were examined, for the first time as well as its HPLC profile. Additionally, total phenolic compounds (TPC), antioxidant properties (estimated via DPPH, ABTS and TRP assays) and antibacterial activity were determined. The predominant phenolic compounds in this extract were evernic, everninic and obtusatic acids. Acetone extract of R. capitata at concentration of 2 μg mL -1 decreased a frequency of micronuclei (MN) for 14.8 %. The extract reduces the concentration of DPPH and ABTS radicals for 21.2 and 36.1 % (respectively). Values for total reducing power (TRP) and cupric reducing capacity (CUPRAC) were 0.4624 ± 0.1064 μg ascorbic acid equivalents (AAE) per mg of dry extract, and 6.1176 ± 0.2964 μg Trolox equivalents (TE) per mg of dry extract, respectively. The total phenol content was 670.6376 ± 66.554 μg galic acid equivalents (GAE) per mg of dry extract. Tested extract at concentration of 2 mg mL -1 exhibited inhibition effect (5.2 %) on pooled human serum cholinesterase. The antimicrobial assay showed that acetone extract had inhibition effect towards Gram-positive strains. The results of manifested antioxidant activity, reducing the number of micronuclei in human lymphocytes, and antibacterial activity recommends R. capitata extract for further in vivo studies.

  5. Revealing metabolomic variations in Cortex Moutan from different root parts using HPLC-MS method.

    Science.gov (United States)

    Xiao, Chaoni; Wu, Man; Chen, Yongyong; Zhang, Yajun; Zhao, Xinfeng; Zheng, Xiaohui

    2015-01-01

    The distribution of metabolites in the different root parts of Cortex Moutan (the root bark of Paeonia suffruticosa Andrews) is not well understood, therefore, scientific evidence is not available for quality assessment of Cortex Moutan. To reveal metabolomic variations in Cortex Moutan in order to gain deeper insights to enable quality control. Metabolomic variations in the different root parts of Cortex Moutan were characterised using high-performance liquid chromatography combined with mass spectrometry (HPLC-MS) and multivariate data analysis. The discriminating metabolites in different root parts were evaluated by the one-way analysis of variance and a fold change parameter. The metabolite profiles of Cortex Moutan were largely dominated by five primary and 41 secondary metabolites . Higher levels of malic acid, gallic acid and mudanoside-B were mainly observed in the second lateral roots, whereas dihydroxyacetophenone, benzoyloxypaeoniflorin, suffruticoside-A, kaempferol dihexoside, mudanpioside E and mudanpioside J accumulated in the first lateral and axial roots. The highest contents of paeonol, galloyloxypaeoniflorin and procyanidin B were detected in the axial roots. Accordingly, metabolite compositions of Cortex Moutan were found to vary among different root parts. The axial roots have higher quality than the lateral roots in Cortex Moutan due to the accumulation of bioactive secondary metabolites associated with plant physiology. These findings provided important scientific evidence for grading Cortex Moutan on the general market. Copyright © 2014 John Wiley & Sons, Ltd.

  6. Simultaneous quantification of flavonoids and triterpenoids in licorice using HPLC.

    Science.gov (United States)

    Wang, Yuan-Chuen; Yang, Yi-Shan

    2007-05-01

    Numerous bioactive compounds are present in licorice (Glycyrrhizae Radix), including flavonoids and triterpenoids. In this study, a reversed-phase high-performance liquid chromatography (HPLC) method for simultaneous quantification of three flavonoids (liquiritin, liquiritigenin and isoliquiritigenin) and four triterpenoids (glycyrrhizin, 18alpha-glycyrrhetinic acid, 18beta-glycyrrhetinic acid and 18beta-glycyrrhetinic acid methyl ester) from licorice was developed, and further, to quantify these 7 compounds from 20 different licorice samples. Specifically, the reverse-phase HPLC was performed with a gradient mobile phase composed of 25 mM phosphate buffer (pH 2.5)-acetonitrile featuring gradient elution steps as follows: 0 min, 100:0; 10 min, 80:20; 50 min, 70:30; 73 min, 50:50; 110 min, 50:50; 125 min, 20:80; 140 min, 20:80, and peaks were detected at 254 nm. By using our technique, a rather good specificity was obtained regarding to the separation of these seven compounds. The regression coefficient for the linear equations for the seven compounds lay between 0.9978 and 0.9992. The limits of detection and quantification lay in the range of 0.044-0.084 and 0.13-0.25 microg/ml, respectively. The relative recovery rates for the seven compounds lay between 96.63+/-2.43 and 103.55+/-2.77%. Coefficient variation for intra-day and inter-day precisions lay in the range of 0.20-1.84 and 0.28-1.86%, respectively. Based upon our validation results, this analytical technique is a convenient method to simultaneous quantify numerous bioactive compounds derived from licorice, featuring good quantification parameters, accuracy and precision.

  7. An improved HPLC method for determination of colocynthin in colocynth

    Directory of Open Access Journals (Sweden)

    M. Shekarchi

    2015-10-01

    Full Text Available Background and objectives: Colocynthin is the major active secondary metabolite of colocynth, Citrullus colocynthis (L. Schrad, which has been used in traditional and ethno medicine of many countries.  It could be considered as an active marker for quality control of colocynth and its herbal products. Analysis and standardization of colocynth and its herbal preparations are a critical issue for their safe applications in phytotherapy and traditional medicine. In the present work, a simple and efficient sample preparation was developed and optimized through combination of matrix solid phase dispersion and ultrasonic assisted extraction. In addition, analytical reversed-phase HPLC method was optimized for analyzing the concentration of colocynthin in colocynth pulp. Methods: Powdered colocynth pulp was grinded with diatomaceous earth to obtain a homogenous mixture. The blend was mixed with methanol and extracted by sonication, followed by centrifugation and filtration. The analytical chromatographic separation was carried out using Luna C18 in isocratic elution with methanol: isopropanol: water: triflouroacetic acid (30:10:60:0.1 v/v. The method was validated as well.  Results: The validation parameters were determines as follows, linear range (r2 = 0.999, 75-500 μg/mL, precision (intra-day < 2.7%, inter-day = 4.4% and accuracy measured via determination of recovery (90-107%. The limit of detection and quantization were calculated 8.5 and 25.7 μg/mL, respectively. Conclusion: Regarding the relatively high content of colocynthin in colocynth pulp, the validated HPLC method could be applied for quality control of colocynth pulp used in Traditional Persian Medicine.

  8. Analysis of brominated and phosphate-based flame retardants in polymer samples by HPLC-UV/MS and online-GPC-HPLC-UV

    Energy Technology Data Exchange (ETDEWEB)

    Schlummer, M.; Brandl, F. [Fraunhofer-Institut fuer Verfahrenstechnik und Verpackung (IVV), Freising (Germany); Maeurer, A.

    2004-09-15

    Here we present two analytical approaches for the identification and quantification of brominated and phosphate-based flame retardants. The first is an HPLC-UV/MS approach, which allows the separation and unequivocal identification and quantification of at least 15 different technical flame retardants. The second approach was set-up as a screening tool, consisting of a GPC separation coupled to an HPLC-UV device.

  9. Comparative HPLC/ESI-MS and HPLC/DAD study of different populations of cultivated, wild and commercial Gentiana lutea L.

    Science.gov (United States)

    Mustafa, Ahmed M; Caprioli, Giovanni; Ricciutelli, Massimo; Maggi, Filippo; Marín, Rosa; Vittori, Sauro; Sagratini, Gianni

    2015-05-01

    The root of Gentiana lutea L., famous for its bitter properties, is often used in alcoholic bitter beverages, food products and traditional medicine to stimulate the appetite and improve digestion. This study presents a new, fast, and accurate HPLC method using HPLC/ESI-MS and HPLC/DAD for simultaneous analysis of iridoids (loganic acid), secoiridoids (gentiopicroside, sweroside, swertiamarin, amarogentin) and xanthones (isogentisin) in different populations of G.lutea L., cultivated in the Monti Sibillini National Park, obtained wild there, or purchased commercially. Comparison of HPLC/ESI-MS and HPLC/DAD indicated that HPLC/ESI-MS is more sensitive, reliable and selective. Analysis of twenty samples showed that gentiopicroside is the most dominant compound (1.85-3.97%), followed by loganic acid (0.11-1.30%), isogentisin (0.03-0.48%), sweroside (0.05-0.35%), swertiamarin (0.08-0.30%), and amarogentin (0.01-0.07%). The results confirmed the high quality of the G.lutea cultivated in the Monti Sibillini National Park. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Grosser, Katharina; van Dam, Nicole M

    2017-03-15

    Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil quality, food flavoring, and human health. The biological activity of glucosinolates is released upon tissue damage, when they are mixed with the enzyme myrosinase. This results in the formation of pungent and toxic breakdown products, such as isothiocyanates and nitriles. Currently, more than 130 structurally different glucosinolates have been identified. The chemical structure of the glucosinolate is an important determinant of the product that is formed, which in turn determines its biological activity. The latter may range from detrimental (e.g., progoitrin) to beneficial (e.g., glucoraphanin). Each glucosinolate-containing plant species has its own specific glucosinolate profile. For this reason, it is important to correctly identify and reliably quantify the different glucosinolates present in brassicaceous leaf, seed, and root crops or, for ecological studies, in their wild relatives. Here, we present a well-validated, targeted, and robust method to analyze glucosinolate profiles in a wide range of plant species and plant organs. Intact glucosinolates are extracted from ground plant materials with a methanol-water mixture at high temperatures to disable myrosinase activity. Thereafter, the resulting extract is brought onto an ion-exchange column for purification. After sulfatase treatment, the desulfoglucosinolates are eluted with water and the eluate is freeze-dried. The residue is taken up in an exact volume of water, which is analyzed by high-pressure liquid chromatography (HPLC) with a photodiode array (PDA) or ultraviolet (UV) detector. Detection and quantification are achieved by conducting comparisons of the retention times and UV spectra of commercial reference standards. The concentrations are calculated based on a sinigrin reference curve and well-established response factors. The advantages and

  11. Determination of 5-fluorouracil in plasma with HPLC-tandem mass spectrometry

    NARCIS (Netherlands)

    van Kuilenburg, A. B. P.; van Lenthe, H.; Maring, J. G.; van Gennip, A. H.

    2006-01-01

    In this article, we describe a fast and specific method to measure 5FU with HPLC tandem-mass spectrometry. Reversed-phase HPLC was combined with electrospray ionization tandem mass spectrometry and detection was performed by multiple-reaction monitoring. Stable-isotope-labeled 5FU (1,3-15N2-5FU) was

  12. Theoretische en practische aspecten van het gebruik van micro-HPLC

    NARCIS (Netherlands)

    de Fluiter P; Jansen EHJM

    1992-01-01

    A practical and theoretical approach for the implementation of micro high performance liquid chromatography (HPLC) is described. A new simple and rapid test procedure was developed in wich a HPLC system can be validated for its suitability for micro-bore columns. It appeared that the detector

  13. Size exclusion HPLC of proteins for evaluation of durum wheat quality

    Science.gov (United States)

    The present research aimed to assess size exclusion HPLC (SE-HPLC) in protein molecular weight distribution determination for quality evaluation of durum semolina. Semolina samples were milled from 13 durum genotypes grown at 7 locations in 2009 and 2010 in ND. Sodium dodecyl sulfate (SDS) buffer ...

  14. Separation, purification and identification of flavonoid glycosides using reversed phase hplc

    International Nuclear Information System (INIS)

    Hasan, A.; Khan, M.A.

    2002-01-01

    Optimal high performance liquid chromatography (HPLC) separation conditions and semi-preparative scale isolation of flavonoid glycosides from three plant species namely Vitex nagunda, Rubus ulmifolious and Malotus philipensis is reported. Identification of purified flavonoid glycoside was achieved using spiking technique in HPLC. (author)

  15. Hip morphologic measurements in an Egyptian population.

    Science.gov (United States)

    Aly, Tarek A

    2011-04-11

    The study of acetabular morphology has shown that there are geographic differences in the morphology and prevalence of acetabular dysplasia among different ethnic groups. However, few data exist on the shape of the acetabulum in various populations around the world. In this study, we examined samples of pelvic radiographs from Egyptian adults. Acetabular dysplasia in adults is characterized by a shallow and relatively vertical acetabulum.The aim of this study was to examine acetabular morphology to determine the prevalence of hip dysplasia in adult Egyptians. This included 244 adults, 134 men and 110 women between 18 and 60 years, who were used to measure center edge angle, acetabular Sharp angle, acetabular head index on anteroposterior radiographic views of the hip joints, and vertical center anterior margin angle on false profile views. The radiographs were taken of patients with no hip complaints at Tanta University Hospital.The results were statistically studied according to the age, height, and weight of patients. The prevalence of acetabular dysplasia was 2.25% for Egyptian men and 3.6% for women with respect to center edge angles, vertical center anterior margin angle, and acetabular head index.We concluded that gender variations in the morphology of the acetabulum and sex influences geometrical measurements of the acetabulum. Egyptian women were more dysplastic than men using the 4 parameters of hip measurements. There are also racial variations in hip morphology. Copyright 2011, SLACK Incorporated.

  16. [Study on the fingerprint of Morus alba from different habitats by HPLC].

    Science.gov (United States)

    Chen, Cheng; Li, Hong-Bo; Wang, Liu-Ping; Li, Yun-Rong; Xin, Ning

    2012-12-01

    To establish HPLC fingerprint of Morus alba from different habitats by HPLC and provide basis for its quality control. HPLC analysis was performed on an Agilent XDB C18 Column (4.6 mm x 250 mm, 5 microm), gradient eluted composed of acetonitrile and 0.3% phosphate acid. The column temperature was set at 35 degrees C and the flow rate was 0.5 mL/min. The detective wavelength was 290 nm. The HPLC fingerprint for 10 batches of Morus alba was studied on their similarity. There were twelve common peaks in the fingerprint. The similarity of 7 batches was above 0.9 and the other batches had low similarity. The HPLC fingerprint can be used for quality control of Morus alba with high characteristics and specificity.

  17. MCR-ALS APLICADO NO MONITORAMENTO QUANTITATIVO DO PROCESSO DE ELETRODEGRADAÇÃO DA ATRAZINA USANDO ESPECTROS UV: RESULTADOS COMPARATIVOS COM HPLC-DAD COMO UM MÉTODO DE REFERÊNCIA

    Directory of Open Access Journals (Sweden)

    Thálisson S. Souza

    2016-02-01

    Full Text Available Electrodegradation of atrazine in water was performed using homemade (PA and PB and purchased (PC boron-doped diamond anodes. The degradation was monitored off-line by analyzing total organic carbon and high performance liquid chromatography with diode array detector (HPLC-DAD and at-line by UV spectroscopy. The spectra were recorded every 2 min. The rank deficiency problem was resolved by assembling an augmented column-wise matrix. HPLC was employed to separate the original and byproducts degradation components. Aiming the same goal, multivariate curve resolution - alternating least squares (MCR-ALS was applied to resolve the UV spectroscopic data. Comparison between HPLC and MCR-ALS separations is presented. By using MCR-ALS the spectra of atrazine and two byproducts were successfully resolved and the resulted concentration profiles properly represented the system studied. The ALS explained variance (R2 for PA, PB and PC was equal to 99.99% for all of them and the lack of fit for PA, PB and PC were 0.39, 0.34 and 0.54 respectively. The correlation (R between the recovered and pure spectra were calculate for each electrodegradation, validating the MCR-ALS results. The average R was equal to 0.997. The spectral and concentration profiles described with this new approach are in agreement with HPLC-DAD results. The proposed method is an alternative to classical analyses for monitoring of the degradation process, mainly due to the simplicity, fast results and economy.

  18. Multivariate analysis of elution parameters for RP-HPLC with charged aerosol detection of sucrose caprate regioisomers

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    2012-01-01

    and Environmental Engineering, Aalborg University, Denmark Sugar fatty acid monoesters have been shown to possess antibiotic and insecticidal properties. The physical and chemical properties of sugar fatty acid esters depend on the saccharide moiety, fatty acid chain length, and both position and degree...... for sucrose caprate regioisomers. As a sensitive method based on mass detection, charged aerosol detection was used. The investigation was conducted using design-of-experiments (DOE) methodology for development and prediction of elution strategies. The elution profiles were described by a number of important......BIOCAT2012, Hamburg University of Technology Book of Abstracts, p290 ISBN 987-3-941492 L73) Multivariate analysis of elution parameters for RP-HPLC with charged aerosol detection of sucrose caprate regioisomers Aleksander Lie and Lars Haastrup Pedersen Department of Biotechnology, Chemistry...

  19. Systematic HPLC/ESI-High Resolution-qTOF-MS Methodology for Metabolomic Studies in Nonfluorescent Chlorophyll Catabolites Pathway

    Directory of Open Access Journals (Sweden)

    José Julián Ríos

    2015-01-01

    Full Text Available Characterization of nonfluorescent chlorophyll catabolites (NCCs and dioxobilane-type nonfluorescent chlorophyll catabolite (DNCC in peel extracts of ripened lemon fruits (Citrus limon L. was performed by HPLC/ESI-high resolution-qTOF-MS method. Compounds were identified in samples on the basis of measured accurate mass, isotopic pattern, and characteristic fragmentation profile with an implemented software postprocessing routine. Three NCC structures already identified in other vegetal tissues were present in the lemon fruit peels (Cl-NCC1; Cl-NCC2; Cl-NCC4 while a new structure not defined so far was characterized (Cl-NCC3. This catabolite exhibits an exceptional arrangement of the peripheral substituents, allowing concluding that the preferences for the NCC modifications could be a species-related matter.

  20. Süt Proteinlerinin RP-HPLC ile Saptanması (İngilizce

    Directory of Open Access Journals (Sweden)

    Zerrin Yüksel

    2015-02-01

    Full Text Available Bu çalışmada, κ-, α- and β-kazein ile α-laktalbumin and β-laktoglobulin, bir RP kolonunun kullanıldığı HPLC-UV ile basit ve hızlı bir yöntem geliştirilerek saptanmıştır. Gradient elüsyonu, 1 ml/dk akış hızında ve 25 oC sıcaklıkta iki çözücü karışımı kullanılarak yürütülmüştür. A çözücüsü asetonitril: su:trifloroasetik asit (100:900:1 ve B çözücüsü asetonitril: su: trifloroasetik asit (100:900:1 karışımlarından oluşmaktadır. Akış, bir UV dedektörü kullanılarak 220 nm’de kaydedilmiştir. Farklı yöntemler kullanılarak RP-HPLC analizi için hazırlanan örneklerde, süt proteinlerine ait farklı kromatografik profiller elde edilmiştir. Diğer örnek hazırlama yöntemlerine kıyasla, enjeksiyondan önce belirtilen oranlarda A ve B çözücülerinin kullanıldığı örnek hazırlama yöntemi ile separasyonun daha keskin ve efektif olduğu ortaya konulmuştur. Bu çalışmada ortaya konulan örnek hazırlama tekniği ve elusyon pratiği ile, süt proteinlerinin analizi basit, hızlı ve duyarlı bir şekilde gerçekleştirilmiştir.

  1. Profile analysis of microparticles

    International Nuclear Information System (INIS)

    Konarski, P.; Iwanejko, I.; Mierzejewska, A.

    2001-01-01

    Depth resolved analyses of several types of microparticles are presented. Particles for secondary ion mass spectrometry (SIMS) depth profile analysis were collected in the working environment of glass plant, steelworks and welding station using eight-stage cascade impactor with particle size range of 0.3 μm to 15 μm. Ion beam sputtering and sample rotation technique allowed to describe morphology i.e. the elemental structure of collected sub-micrometer particles. Also model particles Iriodin 221 (Merck) were depth profiled. The core-shell structure is found for all types of investigated particles. Steelworks particles consist mainly of iron and manganese cores. At the shells of these microparticles: lead, chlorine and fluorine are found. The particles collected in the glass-works consist mainly of lead-zirconium glass cores covered by carbon and copper. Stainless-steel welding particles compose of iron, manganese and chromium cores covered by a shell rich in carbon, chlorine and fluorine. Sample rotation technique applied in SIMS appears to be an effective tool for environmental microparticle morphology studies

  2. Profiling cancer

    DEFF Research Database (Denmark)

    Ciro, Marco; Bracken, Adrian P; Helin, Kristian

    2003-01-01

    In the past couple of years, several very exciting studies have demonstrated the enormous power of gene-expression profiling for cancer classification and prediction of patient survival. In addition to promising a more accurate classification of cancer and therefore better treatment of patients......, gene-expression profiling can result in the identification of novel potential targets for cancer therapy and a better understanding of the molecular mechanisms leading to cancer....

  3. Morphology of PVD films

    International Nuclear Information System (INIS)

    Carr, M.J.; Grotzky, V.K.; Helms, C.J.; Johns, W.L.; Naimon, E.R.; Rafalski, A.L.; Smith, C.J.

    1982-01-01

    Experimental data show that the morphology of PVD chromium coatings is dependent on substrate temperature, deposition rate, and the oxygen content of the chromium source material. For chromium containing about 700-ppM oxygen, a variety of morphologies can form depending on substrate temperature and deposition rate. For chromium contaning 1000 to 2000 ppM of oxygen, porous coatings of the Type IV variety are produced over essentially the full range of temperatures and rates possible with current coating equipment. For chromium containing less than about 400 ppM of oxygen, dense coatings of the Type I variety are produced over the range of temperatures and rates investigated

  4. Phytohormone Profiling across the Bryophytes.

    Directory of Open Access Journals (Sweden)

    Lenka Záveská Drábková

    Full Text Available Bryophytes represent a very diverse group of non-vascular plants such as mosses, liverworts and hornworts and the oldest extant lineage of land plants. Determination of endogenous phytohormone profiles in bryophytes can provide substantial information about early land plant evolution. In this study, we screened thirty bryophyte species including six liverworts and twenty-four mosses for their phytohormone profiles in order to relate the hormonome with phylogeny in the plant kingdom.Samples belonging to nine orders (Pelliales, Jungermanniales, Porellales, Sphagnales, Tetraphidales, Polytrichales, Dicranales, Bryales, Hypnales were collected in Central and Northern Bohemia. The phytohormone content was analysed with a high performance liquid chromatography electrospray tandem-mass spectrometry (HPLC-ESI-MS/MS.As revealed for growth hormones, some common traits such as weak conjugation of both cytokinins and auxins, intensive production of cisZ-type cytokinins and strong oxidative degradation of auxins with abundance of a major primary catabolite 2-oxindole-3-acetic acid were pronounced in all bryophytes. Whereas apparent dissimilarities in growth hormones profiles between liverworts and mosses were evident, no obvious trends in stress hormone levels (abscisic acid, jasmonic acid, salicylic acid were found with respect to the phylogeny.The apparent differences in conjugation and/or degradation strategies of growth hormones between liverworts and mosses might potentially show a hidden link between vascular plants and liverworts. On the other hand, the complement of stress hormones in bryophytes probably correlate rather with prevailing environmental conditions and plant survival strategy than with plant evolution.

  5. Magnetic Ligand Fishing as a Targeting Tool for HPLC-HRMS-SPE-NMR: α-Glucosidase Inhibitory Ligands and Alkylresorcinol Glycosides from Eugenia catharinae.

    Science.gov (United States)

    Wubshet, Sileshi G; Brighente, Inês M C; Moaddel, Ruin; Staerk, Dan

    2015-11-25

    A bioanalytical platform combining magnetic ligand fishing for α-glucosidase inhibition profiling and HPLC-HRMS-SPE-NMR for structural identification of α-glucosidase inhibitory ligands, both directly from crude plant extracts, is presented. Magnetic beads with N-terminus-coupled α-glucosidase were synthesized and characterized for their inherent catalytic activity. Ligand fishing with the immobilized enzyme was optimized using an artificial test mixture consisting of caffeine, ferulic acid, and luteolin before proof-of-concept with the crude extract of Eugenia catharinae. The combination of ligand fishing and HPLC-HRMS-SPE-NMR identified myricetin 3-O-α-L-rhamnopyranoside, myricetin, quercetin, and kaempferol as α-glucosidase inhibitory ligands in E. catharinae. Furthermore, HPLC-HRMS-SPE-NMR analysis led to identification of six new alkylresorcinol glycosides, i.e., 5-(2-oxopentyl)resorcinol 4-O-β-D-glucopyranoside, 5-propylresorcinol 4-O-β-D-glucopyranoside, 5-pentylresorcinol 4-O-[α-D-apiofuranosyl-(1→6)]-β-D-glucopyranoside, 5-pentylresorcinol 4-O-β-D-glucopyranoside, 4-hydroxy-3-O-methyl-5-pentylresorcinol 1-O-β-D-glucopyranoside, and 3-O-methyl-5-pentylresorcinol 1-O-[β-D-glucopyranosyl-(1→6)]-β-D-glucopyranoside.

  6. Comparison of two methods of surface profile extraction from multiple ultrasonic range measurements

    NARCIS (Netherlands)

    Barshan, B; Baskent, D

    Two novel methods for surface profile extraction based on multiple ultrasonic range measurements are described and compared. One of the methods employs morphological processing techniques, whereas the other employs a spatial voting scheme followed by simple thresholding. Morphological processing

  7. Needlelike morphology of aspartame

    NARCIS (Netherlands)

    Cuppen, H.M.; van Eerd, A.R.T.; Meekes, H.L.M.

    2004-01-01

    The needlelike morphology of aspartame form II-A is studied by means of Monte Carlo simulations. Growth simulations for all F faces show merely three faces with a nucleation barrier for growth: two side faces and one top face. Calculations of the energies involved in the growth for a few

  8. Morphology at the Rijksherbarium

    NARCIS (Netherlands)

    Heel, van W.A.

    1979-01-01

    In the following the role of morphology, anatomy and palynology in systematics at the Rijksherbarium will be discussed, as far as flowering plants are concerned. It will be demonstrated that most of the research in this field is rooted in the interest of individual workers, and that no planning was

  9. Applications of HPLC/MS in the analysis of traditional Chinese medicines

    Science.gov (United States)

    Li, Miao; Hou, Xiao-Fang; Zhang, Jie; Wang, Si-Cen; Fu, Qiang; He, Lang-Chong

    2012-01-01

    In China, traditional Chinese medicines (TCMs) have been used in clinical applications for thousands of years. The successful hyphenation of high-Performance liquid chromatography (HPLC) and mass spectrometry (MS) has been applied widely in TCMs and biological samples analysis. Undoubtedly, HPLC/MS technique has facilitated the understanding of the treatment mechanism of TCMs. We reviewed more than 350 published papers within the last 5 years on HPLC/MS in the analysis of TCMs. The present review focused on the applications of HPLC/MS in the component analysis, metabolites analysis, and pharmacokinetics of TCMs etc. 50% of the literature is related to the component analysis of TCMs, which show that this field is the most populär type of research. In the metabolites analysis, HPLC coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry has been demonstrated to be the powerful tool for the characterization of structural features and fragmentation behavior patterns. This paper presented a brief overview of the applications of HPLC/MS in the analysis of TCMs. HPLC/MS in the fingerprint analysis is reviewed elsewhere. PMID:29403684

  10. Morphologic variations of periwinkle and profiles of periwinkle ...

    African Journals Online (AJOL)

    Periwinkles are invertebrates rich in protein and omega-3 fatty acids. These make them relished delicacies. Three hundred and fifteen (315) individual periwinkles were hand-picked from mangrove swamp river banks and intertidal zones of Twon-Brass in Bayelsa State and Abonnema town of Rivers State. Shell length and ...

  11. HPLC analysis of prostaglandin metabolites plasma from irradiated rats

    International Nuclear Information System (INIS)

    Walden, T.L. Jr.; Catravas, G.N.

    1985-01-01

    The authors used RP-HPLC to quantitatively and qualitatively evaluate the PG metabolites in the plasma of rats during the first 24 hrs following a 10 Gy whole body dose of cobalt 60 gamma rays. The PGs and other arachidonic acid metabolites in plasma were extracted and then covalently attached to a fluroescent dye to enhance detection. A number of PGs and their metabolites were observed in the irradiated sample, including: 13,14 dihydro -15 keto PGE/sub 2/ and 13,14, dihydro -15 keto PGF/sub 2/, and their respective precursors, PGE/sub 2/ and PGF/sub 2/. The two major compounds present in the plasma samples were 13,14 dihydro -15 keto PFG/sub 2/ and another compound which is as yet unidentified. The levels of the individual PGs within a sample varied with time after irradiation, and the time at which a PG reached a peak level in the plasma depended on the particular PG in question. 13,14 dihdyro -15 keto PGD/sub 2/ was observed to reach a peak plasma concentration at 6 hours postirradiation, and at that time was at least 20 times higher than control levels

  12. [HPLC Specific Fingerprint of Alcohol Extract of Andrographis paniculata].

    Science.gov (United States)

    Liu, Fei-fei; Fan, Chun-lin; Huang, Xiao-jun; Wang, Gui-yang; Wang, Ying; Ye, Wen-cai

    2015-07-01

    To establish the specific fingerprint of alcohol extract of Andrographis paniculata by HPLC. The analysis was performed on Cosmosil 5C18 -MS-II (250 mm x 4. 6 mm, 5 µm) column, with gradient phase consisting of acetonitrile and water at the flow rate of 1. 0 mL/min. The UV detection wavelength was set at 225 nm, and column temperature was 30 °C. The specific fingerprint chromatogram was established and seven common peaks were identified by comparison with the reference standards and LC-MS. The relative retention times were 1. 00 (No. 1, andrographolide), 1. 04 (No. 2, deoxyandrographoside), 1. 07 (No. 3, isoandrographolide), 1. 10 (No. 4, 14-deoxy-11, 12-didehydroandrographoside), 1. 50 (No. 5, neoandrographolide), 1. 75 ( No. 6, deoxyandrographolide) and 1. 79 (No. 7, dehydroandrographolide). The method is simple and reproducible with high precision, which can provide the basis for the quality control and evaluation of alcohol extract of Andrographis paniculata and its preparations.

  13. Measurement of purine derivatives and creatinine in urine by HPLC

    International Nuclear Information System (INIS)

    Piani, B.; Fabro, C.; Susmel, P.

    2004-01-01

    Two HPLC methods to measure the purine derivatives (PD, including allantoin, uric acid, hypoxanthine and xanthine) and creatinine content in urine are described. PD separation and quantification were achieved using two Spherisorb ODS 2 reversed phase columns connected in series (4.6 x 250 mm) and a Spherisorb ODS 2 Waters pre-column and a Perkin Elmer pump with an auto sampler. The mobile phase was NH 4 H 2 PO 4 :NH 4 H 2 PO 4 -acetonitrile (80:20), which was used at a flow rate of 0.8 ml/min and the detection wavelength was at 190 nm. The average recoveries of standard compounds added to urine samples were satisfactory (92-106%) and the low detection limits (0.7-3.4 μM) permitted the precise determination of these compounds in urine. Separation and quantification of creatinine was achieved using one Spherisorb ODS 2 reversed phase column (4.6 x 250 mm) and one Spherisorb ODS 2 Waters pre-column and a Perkin Elmer pump with an auto sampler. The mobile phase was NH 4 H 2 PO 4 :NH 4 H 2 PO 4 -acetonitrile (80:20), used at a flow rate of 1.00 ml/min and the detection was at 190 nm. The mean recovery (3 measurements) of standard solution added to urine samples was 101%; detection limit was 7.9 μM. (author)

  14. New validated method for piracetam HPLC determination in human plasma.

    Science.gov (United States)

    Curticapean, Augustin; Imre, Silvia

    2007-01-10

    The new method for HPLC determination of piracetam in human plasma was developed and validated by a new approach. The simple determination by UV detection was performed on supernatant, obtained from plasma, after proteins precipitation with perchloric acid. The chromatographic separation of piracetam under a gradient elution was achieved at room temperature with a RP-18 LiChroSpher 100 column and aqueous mobile phase containing acetonitrile and methanol. The quantitative determination of piracetam was performed at 200 nm with a lower limit of quantification LLQ=2 microg/ml. For this limit, the calculated values of the coefficient of variation and difference between mean and the nominal concentration are CV%=9.7 and bias%=0.9 for the intra-day assay, and CV%=19.1 and bias%=-7.45 for the between-days assay. For precision, the range was CV%=1.8/11.6 in the intra-day and between-days assay, and for accuracy, the range was bias%=2.3/14.9 in the intra-day and between-days assay. In addition, the stability of piracetam in different conditions was verified. Piracetam proved to be stable in plasma during 4 weeks at -20 degrees C and for 36 h at 20 degrees C in the supernatant after protein precipitation. The new proposed method was used for a bioequivalence study of two medicines containing 800 mg piracetam.

  15. Identification of Sulfanilamide, Phenazone, and Lidocaine hydrochloride by HPLC Technique

    International Nuclear Information System (INIS)

    Noaba, R.

    2009-01-01

    A sensitive and accurate method was developed for the analysis of sulfanilamide, phenazone, and lidocaine hydrochloride content in pure form and pharmaceutical preparations using HPLC technique. Analysis was performed on column had the following specifications: SHIM-PACK CLC(M) C18(100A 0 , 5μm, 4.6 x 250 mm). And mobile phase consisting of tow phases: the first was methanol, the second consisting of pure form of [water, icy acetic acid, triethylamine in rate (240: 7: 3 v/v/v) respectively], and the two phases were mixed in rate (20:80) respectively, flow rate was 1.5 ml/min, at temperature 300 C, and detector in the ultraviolet range at wavelength 254 nm, consequently. We could separate and determinate the studied compounds in its mixtures, and reached to excellent linearity for each one with correlation coefficients equivalent to (0.9999). This supposed method was applied on prepared samples and pharmaceutical preparation contains of the three studied compounds. The relative standard deviations RSD (n=5) was smaller than (1.99%) for prepared samples and (2.11%) for the pharmaceutical preparation. So this method proved to be sensitive, accurate, is useful for quantitative control of pharmaceutical products. (author)

  16. HPLC retention thermodynamics of grape and wine tannins.

    Science.gov (United States)

    Barak, Jennifer A; Kennedy, James A

    2013-05-08

    The effect of grape and wine tannin structure on retention thermodynamics under reversed-phase high-performance liquid chromatography conditions on a polystyrene divinylbenzene column was investigated. On the basis of retention response to temperature, an alternative retention factor was developed to approximate the combined temperature response of the complex, unresolvable tannin mixture. This alternative retention factor was based upon relative tannin peak areas separated by an abrupt change in solvent gradient. Using this alternative retention factor, retention thermodynamics were calculated. Van't Hoff relationships of the natural log of the alternative retention factor against temperature followed Kirchoff's relationship. An inverse quadratic equation was fit to the data, and from this the thermodynamic parameters for tannin retention were calculated. All tannin fractions exhibited exothermic, spontaneous interaction, with enthalpy-entropy compensation observed. Normalizing for tannin size, distinct tannin compositional effects on thermodynamic parameters were observed. The results of this study indicate that HPLC can be valuable for measuring the thermodynamics of tannin interaction with a hydrophobic surface and provides a potentially valuable alternative to calorimetry. Furthermore, the information gathered may provide insight into understanding red wine astringency quality.

  17. Diversity oriented high-throughput screening of 1,3,4-oxadiazole modified chlorophenylureas and halogenobenzamides by HPLC with peptidomimetic calixarene-bonded stationary phases.

    Science.gov (United States)

    Bazylak, Grzegorz; Malak, Anna; Ali, Imran; Borowiak, Teresa; Dutkiewicz, Grzegorz

    2008-06-01

    Retention profiles in series of the neutral and highly hydrophobic 1,3,4-oxadiazoles containing chlorophenylurea and halogenobenzamide moiety and indicating analgesic activity were determined in the isocratic standard- and narrow-bore HPLC systems employing, respectively, various octadecylsilica and different calixarene bonded stationary phases. When acetonitrile - 2.65 mM phosphoric acid (55 : 45, %, v/v), pH* 3.25, mobile phase was applied retention of these compounds increased with decline of their overall hydrophobicity according to the general preference of more polar compounds by calixarene cavity in time of its non-specific host-guest supramolecular interactions with halogenated substances. The size of calixarene nanocavity and its upper-rim substitution did not change the observed retention order, resolution and selectivity of separation for oxadiazoles. Compared to the retention on the non-end-capped and the highly-end-capped octadecylsilica HPLC column a most improved separation of some regioisomers of halogenated 1,3,4-oxadiazoles were observed on both used calixarene-type HPLC supports. In addition, preliminary data on the self-assembled supramolecular crystal structure of exemplary 1,3,4-oxadiazolchlorophenylurea with cis-elongated conformation was reported and formation of the monovalent inclusion host-guest complexes between 1,3,4-oxadiazoles and each calixarene-type stationary phase was studied with molecular modelling MM+ and AM1 methods. The structural, isomeric and energetic factors leading to the hydrogen bond stabilized inclusion complexes between these species were considered and used for explanation of observed retention sequence and selectivity of 1,3,4-oxadiazoles separation in applied calixarene-based HPLC systems. All these data would be useful in future development of optimized procedures enabling encapsulation of 1,3,4-oxadiazolurea-type drugs with calixarenes.

  18. Associations between the Cervical Vertebral Column and Craniofacial Morphology

    DEFF Research Database (Denmark)

    Sonnesen, Ane Liselotte

    2010-01-01

    Aim. To summarize recent studies on morphological deviations of the cervical vertebral column and associations with craniofacial morphology and head posture in nonsyndromic patients and in patients with obstructive sleep apnoea (OSA). Design. In these recent studies, visual assessment of the cerv......Aim. To summarize recent studies on morphological deviations of the cervical vertebral column and associations with craniofacial morphology and head posture in nonsyndromic patients and in patients with obstructive sleep apnoea (OSA). Design. In these recent studies, visual assessment...... of the cervical vertebral column and cephalometric analysis of the craniofacial skeleton were performed on profile radiographs of subjects with neutral occlusion, patients with severe skeletal malocclusions and patients with OSA. Material from human triploid foetuses and mouse embryos was analysed histologically....... Results. Recent studies have documented associations between fusion of the cervical vertebral column and craniofacial morphology, including head posture in patients with severe skeletal malocclusions. Histological studies on prenatal material supported these findings. Conclusion. It is suggested...

  19. Electrochemically Pretreated Carbon Microfiber Electrodes as Sensitive HPLC-EC Detectors

    Directory of Open Access Journals (Sweden)

    Zdenka Bartosova

    2012-01-01

    Full Text Available The paper focuses on the analysis and detection of electroactive compounds using high-performance liquid chromatography (HPLC combined with electrochemical detection (EC. The fabrication and utilization of electrochemically treated carbon fiber microelectrodes (CFMs as highly sensitive amperometric detectors in HPLC are described. The applied pretreatment procedure is beneficial for analytical characteristics of the sensor as demonstrated by analysis of the model set of phenolic acids. The combination of CFM with separation power of HPLC technique allows for improved detection limits due to unique electrochemical properties of carbon fibers. The CFM proved to be a promising tool for amperometric detection in liquid chromatography.

  20. Transfusion Associated Peak in Hb HPLC Chromatogram – a Case Report

    Science.gov (United States)

    Jain, Sonal; Dass, Jasmita; Pati, Hara Prasad

    2012-01-01

    High performance liquid chromatography (HPLC) and electrophoresis are commonly used to diagnose various hemoglobinopathies. However, insufficient information about the transfusion history can lead to unexpected and confusing results. We are reporting a case of Juvenile myelomonocytic leukemia (JMML) in which HbHPLC was done to quantify fetal hemoglobin (HbF). The chromatogram showed elevated HbF along with a peak in the HbD window. A transfusion acquired peak was suspected based on the unexpectedly low percentage of HbD and was subsequently confirmed using parental HbHPLC. PMID:22348188

  1. Determination of sulfonamides and trimethoprim using high temperature HPLC with simultaneous temperature and solvent gradient.

    Science.gov (United States)

    Giegold, Sascha; Teutenberg, Thorsten; Tuerk, Jochen; Kiffmeyer, Thekla; Wenclawiak, Bernd

    2008-10-01

    A fast HPLC method for the analysis of eight selected sulfonamides (SA) and trimethoprim has been developed with the use of high temperature HPLC. The separation could be achieved in less than 1.5 min on a 50 mm sub 2 microm column with simultaneous solvent and temperature gradient programming. Due to the lower viscosity of the mobile phase and the increased mass transfer at higher temperatures, the separation could be performed on a conventional HPLC system obtaining peak widths at half height between 0.6 and 1.3 s.

  2. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  3. HPLC-RID-DAD-MS analysis of 18F-Fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Macasek, F.; Buriova, E.; Bruder, P.

    2001-01-01

    Objective of new method of FDG analysis development is to replace existing tests by more complex assay. In this work, a liquid chromatography/refractive index detector/diode array detector/mass spectrometric detector combination (HPLC/RID/DAD/MSD) was used for development of a complex routine technique. Optimization of the HPLC/MS analysis was performed investigating MSD analytical signal as a function of various eluent composition. HPLC-RID-DAD-MSD analysis has potentiality of a complex quality control of radiopharmaceuticals, FDG in particular, providing information about: isotope composition; chemical composition; biochemical composition; radiation stability; pharmacodynamics. (author)

  4. Simultaneous qualification and quantification of baccharane glycosides in Impatientis Semen by HPLC-ESI-MSD and HPLC-ELSD.

    Science.gov (United States)

    Li, Hui-Jun; Yu, Jun-Jie; Li, Ping

    2011-03-25

    This study presents a high performance liquid chromatography (HPLC) with electrospray ionization mass spectrometric detection (ESI-MSD) and evaporative light scattering detection (ELSD) method for the simultaneous qualification and quantification of eight major baccharane glycosides, namely hosenlosides A, B, C, F, G, K, L, and M in Impatientis Semen, a Chinese herbal medicine derived from the seeds of Impatiens balsamina L. In order to achieve optimum performance, several extraction parameters (including extraction solvent, extraction mode, extraction time) were optimized. The baccharane glycosides were separated on a Shim-pack CLC-ODS column with gradient elution of water and methanol. Temperature for the ELSD drift tube was set at 98°C and the nitrogen flow rate was 2.7l/min. The unambiguous identities of the analytes were realized by comparing retention times and mass data with those of reference compounds. The developed method was fully validated in terms of linearity, sensitivity, precision, repeatability, recovery as well as robustness, and subsequently applied to evaluate the quality of 14 batches of Impatientis Semen commercial samples from different collections. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Online identification of chlorogenic acids, sesquiterpene lactones, and flavonoids in the Brazilian arnica Lychnophora ericoides Mart. (Asteraceae) leaves by HPLC-DAD-MS and HPLC-DAD-MS/MS and a validated HPLC-DAD method for their simultaneous analysis.

    Science.gov (United States)

    Gobbo-Neto, Leonardo; Lopes, Norberto P

    2008-02-27

    Lychnophora ericoides Mart. (Asteraceae, Vernonieae) is a plant, endemic to Brazil, with occurrence restricted to the "cerrado" biome. Traditional medicine employs alcoholic and aqueous-alcoholic preparations of leaves from this species for the treatment of wounds, inflammation, and pain. Furthermore, leaves of L. ericoides are also widely used as flavorings for the Brazilian traditional spirit "cachaça". A method has been developed for the extraction and HPLC-DAD analysis of the secondary metabolites of L. ericoides leaves. This analytical method was validated with 11 secondary metabolites chosen to represent the different classes and polarities of secondary metabolites occurring in L. ericoides leaves, and good responses were obtained for each validation parameter analyzed. The same HPLC analytical method was also employed for online secondary metabolite identification by HPLC-DAD-MS and HPLC-DAD-MS/MS, leading to the identification of di- C-glucosylflavones, coumaroylglucosylflavonols, flavone, flavanones, flavonols, chalcones, goyazensolide, and eremantholide-type sesquiterpene lactones and positional isomeric series of chlorogenic acids possessing caffeic and/or ferulic moieties. Among the 52 chromatographic peaks observed, 36 were fully identified and 8 were attributed to compounds belonging to series of caffeoylferuloylquinic and diferuloylquinic acids that could not be individualized from each other.

  6. Analysis of sesquiterpene lactones, lignans, and flavonoids in wormwood (Artemisia absinthium L.) using high-performance liquid chromatography (HPLC)-mass spectrometry, reversed phase HPLC, and HPLC-solid phase extraction-nuclear magnetic resonance.

    Science.gov (United States)

    Aberham, Anita; Cicek, Serhat Sezai; Schneider, Peter; Stuppner, Hermann

    2010-10-27

    Today, the medicinal use of wormwood (Artemisia absinthium) is enjoying a resurgence of popularity. This study presents a specific and validated high-performance liquid chromatography (HPLC)-diode array detection method for the simultaneous determination and quantification of bioactive compounds in wormwood and commercial preparations thereof. Five sesquiterpene lactones, two lignans, and a polymethoxylated flavonoid were baseline separated on RP-18 material, using a solvent gradient consisting of 0.085% (v/v) o-phosphoric acid and acetonitrile. The flow rate was 1.0 mL/min, and chromatograms were recorded at 205 nm. The stability of absinthin was tested exposing samples to light, moisture, and different temperatures. Methanolic and aqueous solutions of absinthin were found to be stable for up to 6 months. This was also the case when the solid compound was kept in the refrigerator at -35 °C. In contrast, the colorless needles, when stored at room temperature, turned yellow. Three degradation compounds (anabsin, anabsinthin, and the new dimer 3'-hydroxyanabsinthin) were identified by HPLC-mass spectrometry and HPLC-solid-phase extraction-nuclear magnetic resonance and quantified by the established HPLC method.

  7. Morphology of leukaemias

    Directory of Open Access Journals (Sweden)

    W. Ladines-Castro

    2016-04-01

    Full Text Available Acute leukaemias are characterised by uncontrolled proliferation of immature blood cells with lymphoid or myeloid lineage. Morphological classification is based on the identification of the leukaemia cell line and its stage of differentiation. The first microscopic descriptions dating from the 1930s pointed to 2 different types of leukaemia cells: lymphoid and myeloid. In 1976, the consensus that led to the French-American-British (FAB classification was achieved. This includes criteria for identifying myeloid and lymphoid leukaemias, and gives a list of morphological subtypes, describing how these affect the patient's prognosis. Today, despite new classifications based on sophisticated studies, FAB classification is widely used by experts due to its technical simplicity, good diagnostic reliability and cost-effectiveness.

  8. Controls on alluvial fans morphology

    Science.gov (United States)

    Delorme, P.; Devauchelle, O.; Lajeunesse, E.; Barrier, L.; Métivier, F.

    2017-12-01

    Using laboratory experiments, we investigate the influence of water and sediment discharges on the morphology of an alluvial fan. In our flume, a single-thread laminar river deposits corundum sand (0.4 mm) into a conical fan. We record the fan progradation with top-view images, and measure its shape using the deformation of a Moiré pattern. The fan remains virtually self-affine as it grows, with a nearly constant slope. We find that, when the sediment discharge is small, the longitudinal slope of the fan remains close to that of a river at the threshold for sediment transport. A higher sediment discharge causes the fan's slope to depart from the threshold value. Due to the downstream decrease of the sediment load, this slope gets shallower towards the fan's toe. This mechanism generates a slightly concave fan profile. This suggests that the proximal slope of an alluvial fan could be a proxy for the sediment flux that feeds the fan.Finally, we discuss the applicability of these results to natural systems.

  9. [Comparative data regarding two HPLC methods for determination of isoniazid].

    Science.gov (United States)

    Gârbuleţ, Daniela; Spac, A F; Dorneanu, V

    2009-01-01

    For the determination of isoniazide (isonicotinic acid hydrazide - HIN) two different HPLC methods were developed and validated. Both experiments were performed using a Waters 2695 liquid chromatograph and a UV - Waters 2489 detector. The first method (I) used a Nucleosil 100-10 C18 column (250 x 4.6 mm), a mobile phase formed by a mixture of acetonitrile/10(-2) M oxalic acid (80/20) and a flow of 1.5 mL/ min; detection was done at 230 nm. The second method (II) used a Luna 100-5 C18 column (250 x 4.6 mm), a mobile phase formed by a mixture of methanol/acetate buffer, pH = 5.0 (20/ 80), a flow of 1 mL/min; detection was done at 270 nm. Both methods were validated, the correlation coefficients were 0.9998 (I) and 0.9999 (II), the detection limits were 0.6 microg/mL (I) and 0.055 microg/mL (II), the quantitation limits were 1.9 microg/mL (I) and 0.2 microg/ mL (II). There were also studied: the system precision (RSD = 0.1692% (I) and 0.2000% (II)), the method precision (RSD = 1.1844% (I) and 0.6170% (II)) and the intermediate precision (RSD = 1.8058% (I) and 0.5970% (II)). The accuracy was good, the calculated recoveries were 102.66% (I) and 101.36 (II). Both validated methods were applied for HIN determination from tablets with good and comparable results.

  10. Analysis of cesium extracting solvent using GCMS and HPLC

    International Nuclear Information System (INIS)

    White, T.L.; Herman, C.C.; Crump, S.L.; Marinik, A.R.; Lambert, D.P.; Eibling, R.E.

    2007-01-01

    A high-level waste (HLW) remediation process scheduled to begin in 2007 at the Savannah River Site is the Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU). The MCU will use a hydrocarbon solvent (diluent) containing a cesium extractant, a calix[4]arene compound, to extract radioactive cesium from caustic HLW. The resulting decontaminated HLW waste or raffinate will be processed into grout at the Saltstone Production Facility (SPF). The cesium containing CSSX stream will undergo washing with dilute nitric acid followed by stripping of the cesium nitrate into a very dilute nitric acid or the strip effluent stream and the CSSX solvent will be recycled. The Defense Waste Processing Facility (DWPF) will receive the strip effluent stream and immobilize the cesium into borosilicate glass. Excess CSSX solvent carryover from the MCU creates a potential flammability problem during DWPF processing. Bench-scale DWPF process testing was performed with simulated waste to determine the fate of the CSSX solvent components. A simple high performance liquid chromatography (HPLC) method was developed to identify the modifier (which is used to increase Cs extraction and extractant solubility) and extractant within the DWPF process. The diluent and trioctylamine (which is used to suppress impurity effect and ion-pair disassociation) were determined using gas chromatography mass spectroscopy (GCMS). To close the organic balance, two types of sample preparation methods were needed. One involved extracting aqueous samples with methylene chloride or hexane, and the second was capturing the off gas of the DWPF process using carbon tubes and rinsing the tubes with carbon disulfide for analysis. This paper addresses the development of the analytical methods and the bench-scale simulated waste study results. (author)

  11. Forensic intoxication with clobazam: HPLC/DAD/MSD analysis.

    Science.gov (United States)

    Proença, Paula; Teixeira, Helena; Pinheiro, João; Marques, Estela P; Vieira, Duarte Nuno

    2004-07-16

    Clobazam (Castillium, Urbanil), a benzodiazepine often used as an anxiolytic and in the treatment of epilepsy, is considered a relatively safe drug. The authors present a fatal case with a 49-year-old female, found dead at home. She had been undergoing psychiatric treatment and was a chronic alcoholic. The autopsy findings were unremarkable, except for multivisceral congestion, steatosis and a small piece of a plastic blister pack in the stomach. Bronchopneumonia, bronchitis and bronchiolitis were also diagnosed. Anhigh-performance liquid chromatography (HPLC)/diode array detector (DAD)/mass spectrometry detection (MSD) with electrospray method was developed in order to detect, confirm and quantify clobazam in the post-mortem samples. In the chromatographic separation, a reversed-phase column C18 (2.1 x 150 mm, 3.5 microm) was used with a mobile phase of methanol and water, at a 0.25 ml/min flow rate. Carbonate buffer (pH 10.5) and 20 microl of prazepam (100 microg/ml) as internal standard were added to the samples. A simple and reliable liquid-liquid extraction method for the determination of clobazam in post-mortem samples was described. Calibration curves for clobazam were performed in blood, achieving linearity between 0.01 and 10 microg/ml and a detection limit of 1.0 ng/ml. The clobazam concentration found in post-mortem blood was 3.9 microg/ml, higher than the reported therapeutic concentration (0.1-0.4 microg/ml). The simultaneous acquisition by photodiode array detection and mass spectrometry detection results allowed benzodiazepines to be identified with sufficient certainty. An examination of all the available information suggested that death resulted from respiratory depression due to clobazam toxicity.

  12. Rapid HPLC-MS method for the simultaneous determination of tea catechins and folates.

    Science.gov (United States)

    Araya-Farias, Monica; Gaudreau, Alain; Rozoy, Elodie; Bazinet, Laurent

    2014-05-14

    An effective and rapid HPLC-MS method for the simultaneous separation of the eight most abundant tea catechins, gallic acid, and caffeine was developed. These compounds were rapidly separated within 9 min by a linear gradient elution using a Zorbax SB-C18 packed with sub 2 μm particles. This methodology did not require preparative and semipreparative HPLC steps. In fact, diluted tea samples can be easily analyzed using HPLC-MS as described in this study. The use of mass spectrometry detection for quantification of catechins ensured a higher specificity of the method. The percent relative standard deviation was generally lower than 4 and 7% for most of the compounds tested in tea drinks and tea extracts, respectively. Furthermore, the method provided excellent resolution for folate determination alone or in combination with catechins. To date, no HPLC method able to discriminate catechins and folates in a quick analysis has been reported in the literature.

  13. Which method for quantifying urinary albumin excretion gives what outcome? A comparison of immunonephelometry with HPLC

    NARCIS (Netherlands)

    Brinkman, JW; Bakker, SJL; Gansevoort, RT; Hillege, HL; Kema, IP; Gans, ROB; De Jong, PE; De Zeeuw, D

    2004-01-01

    Background. Microalbuminuria has recently been identified as an independent risk factor for cardiovascular disease in the general population. Immunochemical urinary albumin assays only detect immunoreactive intact albumin. High performance liquid chromatography (HPLC) is able to detect both

  14. HPLC for simultaneous quantification of total ceramide, glucosylceramide, and ceramide trihexoside concentrations in plasma

    NARCIS (Netherlands)

    Groener, Johanna E. M.; Poorthuis, Ben J. H. M.; Kuiper, Sijmen; Helmond, Mariette T. J.; Hollak, Carla E. M.; Aerts, Johannes M. F. G.

    2007-01-01

    BACKGROUND: Simple, reproducible assays are needed for the quantification of sphingolipids, ceramide (Cer), and sphingoid bases. We developed an HPLC method for simultaneous quantification of total plasma concentrations of Cer, glucosylceramide (GlcCer), and ceramide trihexoside (CTH). METHODS:

  15. Automated precolumn derivatization procedures in HPLC for biomedical and clinical applications

    NARCIS (Netherlands)

    Wolf, Johannes Hendrik

    1992-01-01

    This thesis describes three automated precolumn derivatization procedures for the analysis of carboxylic group-containing compounds. After derivatization with a suitable label, the derivatives are separated on reversed-phashed HPLC and detected by fluorescence. ... Zie: Summary

  16. [HPLC fingerprint analysis of flavonoids of phyllanthi fructus from different habitats].

    Science.gov (United States)

    Wang, Fei; Wang, Shuai; Meng, Xian-sheng; Bao, Yong-rui; Zhu, Ying-huan

    2014-11-01

    To establish the HPLC fingerprint of flavonoids of Phyllanthi Fructus from different habitats. HPLC method was adopted. The flavonoids composition of Phyllanthi Fructus from 10 different habitats was determined on an Agilent C, chromatographic column with 0. 5% formic acid water (A)-acetonitrile (B) as the mobile phase in gradient elution under the wavelength of 254 nm. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus were established to evaluate the qualitiy of them. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus from 10 different habitats were established. 18 common peaks were found and the similarities of them were more than 0. 90 except the ones from Guangxi and Guangdong. The method is simple, accurate and repeatable. It can be used for research and quality control of the effective components in Phyllanthi Fructus.

  17. Development and Validation of a RP-HPLC Method for the ...

    African Journals Online (AJOL)

    Development and Validation of a RP-HPLC Method for the Simultaneous Determination of Rifampicin and a Flavonoid Glycoside - A Novel ... range, accuracy, precision, limit of detection, limit of quantification, robustness and specificity.

  18. Antioxidant, antiinflammatory activities and HPLC analysis of South African Salvia species

    CSIR Research Space (South Africa)

    Kamatou, GGP

    2010-03-01

    Full Text Available -performance liquid chromatography (HPLC) was used to identify various compounds in the extracts. Betulafolientriol oxide and rosmarinic acid were detected in all the species investigated, and rosmarinic acid, carnosic acid, carnosol and oleanolic acid/ursolic acid...

  19. Development and Validation of a Stability-Indicating RP-HPLC ...

    African Journals Online (AJOL)

    Development and Validation of a Stability-Indicating RP-HPLC Method for ... of Paracetamol, Tramadol HCl and Domperidone in a Combined Dosage Form. ... testing, as well as for quality control of the combined drugs in pharmaceutical ...

  20. Automated and unbiased classification of chemical profiles from fungi using high performance liquid chromatography

    DEFF Research Database (Denmark)

    Hansen, Michael Edberg; Andersen, Birgitte; Smedsgaard, Jørn

    2005-01-01

    In this paper we present a method for unbiased/unsupervised classification and identification of closely related fungi, using chemical analysis of secondary metabolite profiles created by HPLC with UV diode array detection. For two chromatographic data matrices a vector of locally aligned full sp...

  1. Effects of tetracycline administration on the proteomic profile of pig muscle samples (L. dorsi)

    DEFF Research Database (Denmark)

    Gratacos-Cubarsi, M.; Castellari, M.; Hortos, M.

    2008-01-01

    Effect of tetracycline (TC) administration on the proteomic profile of pig muscle was evaluated by 2D electrophoresis and MALDI-TOF mass spectrometry. The TC content at slaughter was determined in L. dorsi samples by HPLC-DAD. Mean residual concentration of TC in the muscle of treated animals, ca...

  2. Morphology targets: What do seedling morphological attributes tell us?

    Science.gov (United States)

    Jeremiah R. Pinto

    2011-01-01

    Morphology is classically defined as the form and structure of individual organisms, as distinct from their anatomy or physiology. We use morphological targets in the nursery because they are easy to measure, and because we can often quantitatively link seedling morphological traits with survival and growth performance in the field. In the 20 years since the Target...

  3. Simultaneous qualitative and quantitative analysis of phenolic acids and flavonoids for the quality control of Apocynum venetum L. leaves by HPLC-DAD-ESI-IT-TOF-MS and HPLC-DAD.

    Science.gov (United States)

    An, Haijuan; Wang, Hong; Lan, Yuexiang; Hashi, Yuki; Chen, Shizhong

    2013-11-01

    A reliable method based on high performance liquid chromatography-diode array detector-electrospray ionization-ion trap-time of flight-mass spectrometry (HPLC-DAD-ESI-IT-TOF-MS) was developed for the identification of phenolic acids and flavonoids in Apocynum venetum L. leaves and its adulterant, Pocynum hendersonii (Hook. f.) Woodson leaves. A total of 21 compounds were identified or tentatively identified, including 4 phenolic acids and 17 flavonoids. 3-O-caffeoylquinic acid (3-CQA) and caffeic acid were detected for the first time in A. venetum leaves; 4-O-caffeoylquinic acid (4-CQA), 3-CQA, caffeic acid, quercetin-3-O-(6"-O-malonyl)-galactoside, quercetin-3-O-(6"-O-malonyl)-glucoside, kaempferol-3-O-(6"-O-malonyl)-glucoside, kaempferol-3-O-(6"-O-acetyl)-glucoside, and kaempferol-3-O-dihexoside were detected for the first time in P. hendersonii leaves. Cluster analysis was employed to analyze 24 batches of A. venetum leaves and 5 batches of P. hendersonii leaves collected from various regions in China. The analysis, which was based on the 21 compounds, indicated that profiles of these compounds were distinct between the two species, and among A. venetum leaf samples from different origins. 18 of these 21 compounds were selected as the markers and simultaneously analyzed by HPLC-DAD for the first time. The quantitative analytical method was validated and subsequently applied to the comprehensive quality evaluation of 24 batches of A. venetum leaves. © 2013 Elsevier B.V. All rights reserved.

  4. HPLC Analysis of nine corticosteroids in “natural creams” for atopic eczema

    OpenAIRE

    Ameti, Agim; Poposka, Zaklina; Memeti, Shaban; Shishovska, Maja; Mustafa, Zana; Starkoska, Katerina; Arsova-Sarafinovska, Zorica

    2013-01-01

    Purpose: The aim of the study was to determine whether “natural creams” sold for treatment of childhood atopic eczema illegally contain corticosteroids with a newly developed rapid and simple HPLC analysis with UV detection. Material and Methods: HPLC analysis was performed using a Schimadzu LC-2010 chromatographic system (Schimadzu, Kyoto, Japan) consisting of a LC-20AT Prominence liquid chromatography pump with DGU-20A5 Prominence degasser, a SPD-M20A Prominence Diode Array Detector, and...

  5. Expermental Studies of quantitative evaluation using HPLC and safety of Sweet Bee Venom

    OpenAIRE

    Ki Rok Kwon; Ching Seng Chu; Hee Soo Park; Min Ki Kim; Bae Chun Cha; Eun Lee

    2007-01-01

    Objectives : This study was conducted to carry out quantitative evaluation and safety of Sweet Bee Venom. Methods : Content analysis was done using HPLC, measurement of LD50 was conducted intravenous, subcutaneous, and intra-muscular injection to the ICR mice. Results : 1. According to HPLC analysis, removal of the enzymes containing phospholipase A2 was successfully rendered on Sweet Bee Venom. And analyzing melittin content, Sweet Bee Venom contained 12% more melittin than Bee Venom. ...

  6. Development of HPLC Protocol and Simultaneous Quantification of Four Free Flavonoids from Dracocephalum heterophyllum Benth.

    OpenAIRE

    Numonov, Sodik Rakhmonovich; Qureshi, Muhammad Nasimullah; Aisa, Haji Akber

    2015-01-01

    Quantification of the four flavonoids, namely, luteolin, kaempferol, diosmetin, and chrysosplenetin, has been performed for the first time in 80% ethanolic extract of Dracocephalum heterophyllum B. through HPLC coupled to UV detector after optimization of extracting solvent and chromatographic conditions. Total flavonoids quantified were 0.324 mg/mL of the extract. HPLC analysis delivered contents of the luteolin, kaempferol, diosmetin, and chrysosplenetin as 0.08%, 0.14%, 0.28%, and 0.79% of...

  7. Extraction and Quantitative HPLC Analysis of Coumarin in Hydroalcoholic Extracts of Mikania glomerata Spreng: ("guaco" Leaves

    Directory of Open Access Journals (Sweden)

    Celeghini Renata M. S.

    2001-01-01

    Full Text Available Methods for preparation of hydroalcoholic extracts of "guaco" (Mikania glomerata Spreng. leaves were compared: maceration, maceration under sonication, infusion and supercritical fluid extraction. Evaluation of these methods showed that maceration under sonication had the best results, when considering the ratio extraction yield/extraction time. A high performance liquid chromatography (HPLC procedure for the determination of coumarin in these hydroalcoholic extracts of "guaco" leaves is described. The HPLC method is shown to be sensitive and reproducible.

  8. HPLC-DAD-MS(n) characterisation of carotenoids from apricots and pumpkins for the evaluation of fruit product authenticity.

    Science.gov (United States)

    Kurz, Christina; Carle, Reinhold; Schieber, Andreas

    2008-09-15

    Carotenoids including carotenoid esters from six apricot (Prunus armeniaca L.) cultivars and from eight cultivars from three pumpkin species (Cucurbita maxima Duch., Cucurbita pepo L., and Cucurbita moschata Duch.) were extracted without saponification, separated on a C-30 reversed-phase column and characterised by high-performance liquid chromatography/atmospheric pressure chemical ionisation-mass spectrometry (LC-MS). The predominant free carotenoids were quantified by HPLC with diode array detection. In contrast to previously published data, α-carotene could not be detected in apricots. Although the pumpkins showed significant differences in their free carotenoid profiles, major unesterified compounds different from those found in apricots could be determined. However, due to the natural heterogeneity, authentication of the apricot products cannot be accomplished exclusively using the profile of free carotenoids. Therefore, the investigations were extended to carotenoid esters. The xanthophyll ester profiles in pumpkins significantly differed from those in apricots in that the latter also contained both saturated and unsaturated fatty acids, whereas in pumpkins exclusively saturated fatty acids were detected. Admixtures of lower cost pumpkins could be detected in quantities of ⩾5% by increased contents of lutein and zeaxanthin, and by the appearance of antheraxanthin and α-carotene, respectively, depending on the added pumpkin cultivar, as well as the presence of characteristic lutein and antheraxanthin esters. However, pronounced differences in the carotenoid profiles of the investigated pumpkins and the partly minor amount of characteristic compounds lead to limitations of the detection of 5% level of admixture of pumpkin to apricot and of the method in general. Copyright © 2008 Elsevier Ltd. All rights reserved.

  9. Development of a new rapid HPLC method for the fractionation of histones

    International Nuclear Information System (INIS)

    Gurley, L.R.; Valdez, J.G.; Prentice, D.A.; Spall, W.D.

    1983-01-01

    To study histone functions, it is necessary to fractionate the histones into their five classes (H1, H2A, H2B, H3 and H4) and then to subfractionate these classes into variants having slightly different primary structures and into different phosphorylated and acetylated forms. With the advent of high-performance liquid chromatography (HPLC), it was hoped that laborious and time-consuming conventional methods could be replaced by a simple, rapid, high-resolving HPLC method for fractionating histones. However, problems of irreversible adsorption of the histones to HPLC column packings discouraged this development. Our laboratory has now determined that the strong adsorption of histones to HPLC columns results from two different forces: (1) polar interactions between the histones and the silanol groups of silica-based HPLC column packing, and (2) hydrophobic interactions between the histones and the bound organic phase of the column packings. By minimizing these forces, we have succeeded in developing an HPLC method suitable for histone studies

  10. Very Deep Convolutional Neural Networks for Morphologic Classification of Erythrocytes.

    Science.gov (United States)

    Durant, Thomas J S; Olson, Eben M; Schulz, Wade L; Torres, Richard

    2017-12-01

    Morphologic profiling of the erythrocyte population is a widely used and clinically valuable diagnostic modality, but one that relies on a slow manual process associated with significant labor cost and limited reproducibility. Automated profiling of erythrocytes from digital images by capable machine learning approaches would augment the throughput and value of morphologic analysis. To this end, we sought to evaluate the performance of leading implementation strategies for convolutional neural networks (CNNs) when applied to classification of erythrocytes based on morphology. Erythrocytes were manually classified into 1 of 10 classes using a custom-developed Web application. Using recent literature to guide architectural considerations for neural network design, we implemented a "very deep" CNN, consisting of >150 layers, with dense shortcut connections. The final database comprised 3737 labeled cells. Ensemble model predictions on unseen data demonstrated a harmonic mean of recall and precision metrics of 92.70% and 89.39%, respectively. Of the 748 cells in the test set, 23 misclassification errors were made, with a correct classification frequency of 90.60%, represented as a harmonic mean across the 10 morphologic classes. These findings indicate that erythrocyte morphology profiles could be measured with a high degree of accuracy with "very deep" CNNs. Further, these data support future efforts to expand classes and optimize practical performance in a clinical environment as a prelude to full implementation as a clinical tool. © 2017 American Association for Clinical Chemistry.

  11. Micropropagation and validation of genetic and biochemical fidelity among regenerants of Nothapodytes nimmoniana (Graham) Mabb. employing ISSR markers and HPLC.

    Science.gov (United States)

    Prakash, Lokesh; Middha, Sushil Kumar; Mohanty, Sudipta Kumar; Swamy, Mallappa Kumara

    2016-12-01

    An in vitro protocol has been established for clonal propagation of Nothapodytes nimmoniana which is an important source of Camptothecin (CPT). Elite source was identified based on the chemical potency to accumulate the optimum level of CPT. Different types and concentrations of plant growth regulators were used to study their effect on inducing multiple shoots from the explants regenerated from embryos of N. nimmoniana. Of these, a combination of N6-benzyladenine (0.2 mg L -1 ) and Indole-3-butyric acid (IBA) (0.1 mg L -1 ) proved optimum for differentiating multiple shoots in 90.6 % of the cultures with an average of 10.24 shoots per explant obtained within 8 weeks of inoculation. Nearly, 92 % of the excised in vitro shoots rooted on half strength Murashige and Skoog (MS) medium containing 0.05 % activated charcoal, supplemented with 1-naphthaleneacetic acid and IBA at 0.1 mg L -1 each. The micropropagated plants were evaluated for their genetic fidelity by employing inter simple sequence repeats (ISSR) markers. Ten individuals, randomly chosen from a population of 145 regenerants, were compared with the donor plant. The regenerated plants were also evaluated for their chemical potency using high-performance liquid chromatography (HPLC) analysis of CPT content. The true-to-type nature of the micropropagated plants was confirmed based on their monomorphic banding profiles with that of the mother plants using ISSR markers. Besides, HPLC evaluation of the CPT content confirmed the existence of chemical uniformity among the regenerated plants and the elite mother plant.

  12. RP-HPLC method for simultaneous estimation of vigabatrin, gamma-aminobutyric acid and taurine in biological samples.

    Science.gov (United States)

    Police, Anitha; Shankar, Vijay Kumar; Narasimha Murthy, S

    2018-02-15

    Vigabatrin is used as first line drug in treatment of infantile spasms for its potential benefit overweighing risk of causing permanent peripheral visual field defects and retinal damage. Chronic administration of vigabatrin in rats has demonstrated these ocular events are result of GABA accumulation and depletion of taurine levels in retinal tissues. In vigabatrin clinical studies taurine plasma level is considered as biomarker for studying structure and function of retina. The analytical method is essential to monitor taurine levels along with vigabatrin and GABA. A RP-HPLC method has been developed and validated for simultaneous estimation of vigabatrin, GABA and taurine using surrogate matrix. Analytes were extracted from human plasma, rat plasma, retina and brain by simple protein precipitation method and derivatized by naphthalene 2, 3‑dicarboxaldehyde to produce stable fluorescent active isoindole derivatives. The chromatographic analysis was performed on Zorbax Eclipse AAA column using gradient elution profile and eluent was monitored using fluorescence detector. A linear plot of calibration curve was observed in concentration range of 64.6 to 6458, 51.5 to 5150 and 62.5 to 6258 ng/mL for vigabatrin, GABA and taurine, respectively with r 2  ≥ 0.997 for all analytes. The method was successfully applied for estimating levels of vigabatrin and its modulator effect on GABA and taurine levels in rat plasma, brain and retinal tissue. This RP-HPLC method can be applied in clinical and preclinical studies to explore the effect of taurine deficiency and to investigate novel approaches for alleviating vigabatrin induced ocular toxicity. Copyright © 2018. Published by Elsevier B.V.

  13. Chemometrics enhanced HPLC-DAD performance for rapid quantification of carbamazepine and phenobarbital in human serum samples.

    Science.gov (United States)

    Vosough, Maryam; Ghafghazi, Shiva; Sabetkasaei, Masoumeh

    2014-02-01

    This paper describes development and validation of a simple and efficient bioanalytical procedure for simultaneous determination of phenobarbital and carbamazepine in human serum samples using high performance liquid chromatography with photodiode-array detection (HPLC-DAD) regarding a fast elution methodology in less than 5 min. Briefly, this method consisted of a simple deproteinization step of serum samples followed by HPLC analysis on a Bonus-RP column using an isocratic mode of elution with acetonitrile/K2HPO4 (pH=7.5) buffer solution (45:55). Due to the presence of serum endogenous components as non-calibrated components in the sample, second-order calibration based on multivariate curve resolution-alternating least squares (MCR-ALS), has been applied on a set of absorbance matrices collected as a function of retention time and wavelengths. Acceptable resolution and quantification results were achieved in the presence of matrix interferences and the second-order advantage was fully exploited. The average recoveries for carbamazepine and phenobarbital were 89.7% and 86.1% and relative standard deviation values were lower than 9%. Additionally, computed elliptical joint confidence region (EJCR) confirmed the accuracy of the proposed method and indicated the absence of both constant and proportional errors in the predicted concentrations. The developed method enabled the determination of the analytes in different serum samples in the presence of overlapped profiles, while keeping experimental time and extraction steps at minimum. Finally, the serum concentration levels of carbamazepine in three time intervals were reported for morphine-dependents who had received carbamazepine for treating their neuropathic pain. © 2013 Elsevier B.V. All rights reserved.

  14. Effects of soil treatment with abattoir effluent on morphological and ...

    African Journals Online (AJOL)

    The effects of abattoir wastewater treated soil on morphological and biochemical profiles of cowpea seedlings (Vigna unguiculata) grown in gasoline polluted soil was studied. Percentage germination, shoot length, root length and leaf area of cowpea seedlings grown in gasoline treated soil decreased significantly (P ...

  15. Morphology and Classification of the Southern Sombreiro -Warri ...

    African Journals Online (AJOL)

    The soils of the Southern Sombreiro-Warri Deltaic plain surrounded by mangrove forest in Kalabari Kingdom, Eastern Niger Delta were studied to assess their morphological characteristics and classification. Four profile pits were sunk, one in each of the following towns: Degema, Abonnema, Buguma and Tombia.

  16. Characteristic fingerprint based on gingerol derivative analysis for discrimination of ginger (Zingiber officinale) according to geographical origin using HPLC-DAD combined with chemometrics.

    Science.gov (United States)

    Yudthavorasit, Soparat; Wongravee, Kanet; Leepipatpiboon, Natchanun

    2014-09-01

    Chromatographic fingerprints of gingers from five different ginger-producing countries (China, India, Malaysia, Thailand and Vietnam) were newly established to discriminate the origin of ginger. The pungent bioactive principles of ginger, gingerols and six other gingerol-related compounds were determined and identified. Their variations in HPLC profiles create the characteristic pattern of each origin by employing similarity analysis, hierarchical cluster analysis (HCA), principal component analysis (PCA) and linear discriminant analysis (LDA). As results, the ginger profiles tended to be grouped and separated on the basis of the geographical closeness of the countries of origin. An effective mathematical model with high predictive ability was obtained and chemical markers for each origin were also identified as the characteristic active compounds to differentiate the ginger origin. The proposed method is useful for quality control of ginger in case of origin labelling and to assess food authenticity issues. Copyright © 2014 Elsevier Ltd. All rights reserved.

  17. High-performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for the analysis of xenobiotic metabolites in rat urine: application to the metabolites of 4-bromoaniline.

    Science.gov (United States)

    Nicholson, J K; Lindon, J C; Scarfe, G; Wilson, I D; Abou-Shakra, F; Castro-Perez, J; Eaton, A; Preece, S

    2000-02-01

    The use of HPLC-ICP-MS for the profiling and quantification of the metabolites of 4-bromoaniline following reversed-phase gradient chromatography is demonstrated. In the 0-8 h post dose sample, which contained the highest concentrations of compound-related material, it was possible to detect at least 16 metabolites of the compound. The methodology described offers the possibility of obtaining metabolite profiles and quantification for drugs and other xenobiotics in biological fluids and excreta without the requirement for radiolabelled tracers.

  18. Characterisation of Vranec, Cabernet sauvignon and Merlot wines based on their chromatic and anthocyanin profiles

    OpenAIRE

    Dimitrovska Maja; Tomovska Elena; Bocevska Mirjana

    2013-01-01

    Wines of three different grape varieties, Vranec, Cabernet Sauvignon and Merlot were examined for their characterisation in terms of anthocyanin and chromatic profiles, total polyphenols and antioxidant potential. Total, monomeric, polymeric and copigmented anthocyanins were determined by spectrophotometry and the individual anthocyanin compounds were quantified using HPLC-DAD. Chromatic profile was evaluated according to colour density, hue, % red, % blue, % yellow and brilliance (% dA...

  19. Morphological analysis of ionomers

    International Nuclear Information System (INIS)

    1990-01-01

    This report discusses the progress made during the period of April 1st, 1989 and March 31st, 1990. Topics covered are: SANS of Telechelic Ionomers, SANS of Sulfonated Polyurethanes, Effect of Matrix Polarity and Ambient Aging on the Morphology of Sulfonated Polyurethane Ionomers, Adhesive Sphere Model for Analysis of SAXS Data from Ionomers, Comparison of Structure-Property Relationships in Carboxylated and Sulfonated Polyurethane Ionomers, Development of a Liquid-like Hard Sphere Model for Deformed Ionomer Samples, and Polymer Synthesis for Proposed Research

  20. Experimental impact crater morphology

    Science.gov (United States)

    Dufresne, A.; Poelchau, M. H.; Hoerth, T.; Schaefer, F.; Thoma, K.; Deutsch, A.; Kenkmann, T.

    2012-04-01

    The research group MEMIN (Multidisciplinary Experimental and Impact Modelling Research Network) is conducting impact experiments into porous sandstones, examining, among other parameters, the influence of target pore-space saturation with water, and projectile velocity, density and mass, on the cratering process. The high-velocity (2.5-7.8 km/s) impact experiments were carried out at the two-stage light-gas gun facilities of the Fraunhofer Institute EMI (Germany) using steel, iron meteorite (Campo del Cielo IAB), and aluminium projectiles with Seeberg Sandstone as targets. The primary objectives of this study within MEMIN are to provide detailed morphometric data of the experimental craters, and to identify trends and characteristics specific to a given impact parameter. Generally, all craters, regardless of impact conditions, have an inner depression within a highly fragile, white-coloured centre, an outer spallation (i.e. tensile failure) zone, and areas of arrested spallation (i.e. spall fragments that were not completely dislodged from the target) at the crater rim. Within this general morphological framework, distinct trends and differences in crater dimensions and morphological characteristics are identified. With increasing impact velocity, the volume of craters in dry targets increases by a factor of ~4 when doubling velocity. At identical impact conditions (steel projectiles, ~5km/s), craters in dry and wet sandstone targets differ significantly in that "wet" craters are up to 76% larger in volume, have depth-diameter ratios generally below 0.19 (whereas dry craters are almost consistently above this value) at significantly larger diameters, and their spallation zone morphologies show very different characteristics. In dry craters, the spall zone surfaces dip evenly at 10-20° towards the crater centre. In wet craters, on the other hand, they consist of slightly convex slopes of 10-35° adjacent to the inner depression, and of sub-horizontal tensile

  1. Cluster analysis of historical and modern hard red spring wheat cultivars based on parentage and HPLC analysis of gluten forming proteins

    Science.gov (United States)

    In this study, 30 hard red spring (HRS) wheat cultivars released between 1910 and 2013 were analyzed to determine how they cluster in terms of parentage and protein data, analyzed by reverse-phase HPLC (RP-HPLC) of gliadins, and size-exclusion HPLC (SE-HPLC) of unreduced proteins. Dwarfing genes in...

  2. Morphology of urethral tissues

    Science.gov (United States)

    Müller, Bert; Schulz, Georg; Herzen, Julia; Mushkolaj, Shpend; Bormann, Therese; Beckmann, Felix; Püschel, Klaus

    2010-09-01

    Micro computed tomography has been developed to a powerful technique for the characterization of hard and soft human and animal tissues. Soft tissues including the urethra, however, are difficult to be analyzed, since the microstructures of interest exhibit X-ray absorption values very similar to the surroundings. Selective staining using highly absorbing species is a widely used approach, but associated with significant tissue modification. Alternatively, one can suitably embed the soft tissue, which requires the exchange of water. Therefore, the more recently developed phase contrast modes providing much better contrast of low X-ray absorbing species are especially accommodating in soft tissue characterization. The present communication deals with the morphological characterization of sheep, pig and human urethras on the micrometer scale taking advantage of micro computed tomography in absorption and phase contrast modes. The performance of grating-based tomography is demonstrated for freshly explanted male and female urethras in saline solution. The micro-morphology of the urethra is important to understand how the muscles close the urethra to reach continence. As the number of incontinent patients is steadily increasing, the function under static and, more important, under stress conditions has to be uncovered for the realization of artificial urinary sphincters, which needs sophisticated, biologically inspired concepts to become nature analogue.

  3. Combined HPLC-CUPRAC (cupric ion reducing antioxidant capacity) assay of parsley, celery leaves, and nettle.

    Science.gov (United States)

    Yildiz, Leyla; Başkan, Kevser Sözgen; Tütem, Esma; Apak, Reşat

    2008-10-19

    This study aims to identify the essential antioxidant compounds present in parsley (Petroselinum sativum) and celery (Apium graveolens) leaves belonging to the Umbelliferae (Apiaceae) family, and in stinging nettle (Urtica dioica) belonging to Urticaceae family, to measure the total antioxidant capacity (TAC) of these compounds with CUPRAC (cupric ion reducing antioxidant capacity) and ABTS spectrophotometric methods, and to correlate the TAC with high performance liquid chromatography (HPLC) findings. The CUPRAC spectrophotometric method of TAC assay using copper(II)-neocuproine (2,9-dimethyl-1,10-phenanthroline) as the chromogenic oxidant was developed in our laboratories. The individual antioxidant constituents of plant extracts were identified and quantified by HPLC on a C18 column using a modified mobile phase of gradient elution comprised of MeOH-0.2% o-phosphoric acid and UV detection for polyphenols at 280 nm. The TAC values of HPLC-quantified antioxidant constituents were found, and compared for the first time with those found by CUPRAC. The TAC of HPLC-quantified compounds accounted for a relatively high percentage of the observed CUPRAC capacities of plant extracts, namely 81% of nettle, 60-77% of parsley (in different hydrolyzates of extract and solid sample), and 41-57% of celery leaves (in different hydrolyzates). The CUPRAC total capacities of the 70% MeOH extracts of studied plants (in the units of mmol trolox g(-1)plant) were in the order: celery leaves>nettle>parsley. The TAC calculated with the aid of HPLC-spectrophotometry did not compensate for 100% of the CUPRAC total capacities, because all flavonoid glycosides subjected to hydrolysis were either not detectable with HPLC, or not converted to the corresponding aglycons (i.e., easily detectable and quantifiable with HPLC) during the hydrolysis step.

  4. VERIFICATION HPLC METHOD OF QUANTITATIVE DETERMINATION OF AMLODIPINE IN TABLETS

    Directory of Open Access Journals (Sweden)

    Khanin V. A

    2014-10-01

    a volume of 100.0 ml. Preparation of the working standard solution sample amlodipine besylate. 50.0 mg of amlodipine RCC dissolved in methanol and dilute with the same solvent to 50.0 ml. 5.0 ml of this solution argue with methanol to volume 100.0 ml. Before the major controlled trials validated the existence of documents certifying the suitability vykorystovanoho equipment, raw materials and chemicals. Validation of the methodology was carried out in accordance with the requirements of SPhU. Results & discussion. Linearity methods defined within 80-120% of nominal concentrations. The linearity of the methods supported by the entire range of concentrations studied (b=0.9845, Sb=0,01473, a=1.5282, Sa=1.4956, S0=0.5486, r=0.9992. It is proved that the validated method characterized by sufficient convergence and accuracy over the entire range of concentrations (ΔZ=1.03, δ%=0.09. Conclusion. During verification methods of quantitative determination of amlodipine besylate tablets were studied characteristics validated HPLC method: accuracy, linearity, precision, specificity, and internal laboratory precision. Validation technique characteristics do not exceed the critical value of error (1.6% and characterized by qualitative analytical indicators. This technique can be correctly reproduced in the laboratory conditions, and is independent of the excipients.

  5. Chemical profiling and antioxidant activity of Bolivian propolis.

    Science.gov (United States)

    Nina, Nélida; Quispe, Cristina; Jiménez-Aspee, Felipe; Theoduloz, Cristina; Giménez, Alberto; Schmeda-Hirschmann, Guillermo

    2016-04-01

    Propolis is a relevant research subject worldwide. However, there is no information so far on Bolivian propolis. Ten propolis samples were collected from regions with high biodiversity in the main honey production places in Bolivia and were analyzed for their total phenolics (TP), flavonoids (TF) and antioxidant activity. The chemical profiles of the samples were assessed by TLC, HPLC-DAD, HPLC-DAD-MS/MS(n) and NMR analysis. TP, TF, TLC and NMR analysis showed significant chemical differences between the samples. Isolation of the main constituents by chromatography and identification by HPLC-DAD-MS/MS(n) achieved more than 35 constituents. According to their profiles, the Bolivian propolis can be classified into phenolic-rich and triterpene-rich samples. Propolis from the valleys (Cochabamba, Chuquisaca and Tarija) contained mainly prenylated phenylpropanoids, while samples from La Paz and Santa Cruz contained cycloartane and pentacyclic triterpenes. Phenolic-rich samples presented moderate to strong antioxidant activity while the triterpene-rich propolis were weakly active. High chemical diversity and differential antioxidant effects were found in Bolivian propolis. Our results provide additional evidence on the chemical composition and bioactivity of South American propolis. © 2015 Society of Chemical Industry.

  6. Simultaneous detection of water-soluble vitamins using the High Performance Liquid Chromatography (HPLC - a review

    Directory of Open Access Journals (Sweden)

    Rosemond Godbless Dadzie

    2014-01-01

    Full Text Available The water-soluble vitamins (WSV: ascorbic acid (vitamin C, thiamine (B1, riboflavin (B2, niacin (B3, panthothenic acid (B5, pyridoxine, and pyridoxal (B6, folic acid (B9, biotin(B8 , and B12 are very essential in the diet of humankind. As a result of ever increasing pressures from both consumers and legal enforcers, to specify accurately nutritive compositions of WSV that are present in food materials, many researchers have attempted to fill this niche through the provision of highly sensitive and rapid high performance liquid chromatography (HPLC procedures. In view of the health benefits of WSV, a replete of HPLC methods have been developed for simultaneous determination of their contents in nature and fortified food samples, nutritional supplements, as well as blood plasmas. The rate of losses of these vitamins during food processing and analysis, in addition to their transient dynamics, presents complexities in developing a highly sensitive HPLC procedure for their simultaneous separations and assays. This review critically assesses the different HPLC procedures developed by researchers and available in the open literature for simultaneous determination of water-soluble vitamins (WSV in dried tropical fruits materials. The study revealed that not a single chromatographic run developed by researchers can simultaneously elute all the WSV at a time. However, the HPLC procedures that are capable of determining all the WSV were coupled with electrospray ionization mass spectroscopy (ESI-MS, thus making the set-up expensive.

  7. Comparison of transferrin isoform analysis by capillary electrophoresis and HPLC for screening congenital disorders of glycosylation.

    Science.gov (United States)

    Dave, Mihika B; Dherai, Alpa J; Udani, Vrajesh P; Hegde, Anaita U; Desai, Neelu A; Ashavaid, Tester F

    2018-01-01

    Transferrin, a major glycoprotein has different isoforms depending on the number of sialic acid residues present on its oligosaccharide chain. Genetic variants of transferrin as well as the primary (CDG) & secondary glycosylation defects lead to an altered transferrin pattern. Isoform analysis methods are based on charge/mass variations. We aimed to compare the performance of commercially available capillary electrophoresis CDT kit for diagnosing congenital disorders of glycosylation with our in-house optimized HPLC method for transferrin isoform analysis. The isoform pattern of 30 healthy controls & 50 CDG-suspected patients was determined by CE using a Carbohydrate-Deficient Transferrin kit. The results were compared with in-house HPLC-based assay for transferrin isoforms. Transferrin isoform pattern for healthy individuals showed a predominant tetrasialo transferrin fraction followed by pentasialo, trisialo, and disialotransferrin. Two of 50 CDG-suspected patients showed the presence of asialylated isoforms. The results were comparable with isoform pattern obtained by HPLC. The commercial controls showed a <20% CV for each isoform. Bland Altman plot showed the difference plot to be within +1.96 with no systemic bias in the test results by HPLC & CE. The CE method is rapid, reproducible and comparable with HPLC and can be used for screening Glycosylation defects. © 2017 Wiley Periodicals, Inc.

  8. Chromatographic profiles of extractives from leaves of Eugenia uniflora

    Directory of Open Access Journals (Sweden)

    Isabelle C.F. Bezerra

    Full Text Available ABSTRACT Eugenia uniflora L., Myrtaceae, popularly known as “pitanga”, is used in traditional medicine due the properties attributed to its chemical content, these being mainly hydrolysable tannins and flavonoids. This study provides a qualitative and quantitative evaluation of chemical profile from leaves of E. uniflora. The HPLC analysis was carried out on a C18 column (4.6 mm × 250 mm, 5 µm by gradient elution with methanol and water (acidified with trifluoracetic acid; and silica gel Plates 60-F 254 with 10–12 µm and 5–6 µm particles, respectively for TLC and High HPTLC analysis. The chromatographic data obtained from HPLC, TLC and HPTLC presented bands and peaks related to flavonoids (myricitrin and derivatives and tannins (gallic and ellagic acids, which were observed from different samples. The chromatographic similarities enabled the building of a typical fingerprint for the herbal material. The similarity analysis of the sample data by Pearson correlation showed R values >0.9 among peaks (HPLC and bands (HPTLC. In addition, the analytical methodology developed by HPLC enabled the satisfactory quantification of marker substances [ellagic acid = 0.22% and 0.20% (m/m; gallic acid = 0.20% and 0.43%; myricitrin = 0.42 and 1.74% (m/m in herbal drug and crude extract, respectively]. The procedure was also validated in accordance with the assays required by Brazilian legislation. Thus, the HPTLC and HPLC methods developed in this study provide helpful and simple tools for the quality evaluation both qualitatively and quantitatively of raw materials and extractives from leaves of E. uniflora.

  9. Novel magnetic hollow zein nanoparticles for preconcentration of chlorpyrifos from water and soil samples prior to analysis via high-performance liquid chromatography (HPLC).

    Science.gov (United States)

    Rahimi Moghadam, Mojtaba; Zargar, Behrooz; Rastegarzadeh, Saadat

    2018-04-30

    Herein, magnetically hollow zein nanoparticles were synthesized and used as a magnetic sorbent for the preconcentration of chlorpyrifos and its analysis by high-performance liquid chromatography (HPLC). Morphology of the sorbent was characterized by transmission electron microscopy (TEM). In this study, the effects of important parameters such as pH of the solution, adsorption and desorption time, type and volume of desorption solvent, and salt addition were investigated. Under optimized experimental conditions, the linear range was from 50 to 2000 μg mL-1, and an LOD of 25 μg L-1 was calculated. The relative standard deviations (RSD) varied from 3.8 to 5.1% (n = 5). The enrichment factors for 50 and 100 μg L-1 samples were calculated as 187 and 210, respectively. The developed method was successfully applied in soil and water samples and showed good extraction recoveries.

  10. DEMorphy, German Language Morphological Analyzer

    OpenAIRE

    Altinok, Duygu

    2018-01-01

    DEMorphy is a morphological analyzer for German. It is built onto large, compactified lexicons from German Morphological Dictionary. A guesser based on German declension suffixed is also provided. For German, we provided a state-of-art morphological analyzer. DEMorphy is implemented in Python with ease of usability and accompanying documentation. The package is suitable for both academic and commercial purposes wit a permissive licence.

  11. Monitoring of monosaccharides, oligosaccharides, ethanol and glycerol during wort fermentation by biosensors, HPLC and spectrophotometry.

    Science.gov (United States)

    Monošík, Rastislav; Magdolen, Peter; Stredanský, Miroslav; Šturdík, Ernest

    2013-05-01

    The aim of the present study was to analyze sugar levels (namely maltose, maltotriose, glucose and fructose) and alcohols (ethanol and glycerol) during the fermentation process in wort samples by amperometric enzymatic biosensors developed by our research group for industrial application, HPLC and spectrophotometry, and to compare the suitability of the presented methods for determination of individual analytes. We can conclude that for the specific monitoring of maltose or maltotriose only the HPLC method was suitable. On the other hand, biosensors and spectrophotometry reflected a decrease in total sugar concentration better and were able to detect both glucose and fructose in the later stages of fermentation, while HPLC was not. This can be attributed to the low detection limits and good sensitivity of the proposed methods. For the ethanol and glycerol analysis all methods proved to be suitable. However, concerning the cost expenses and time analysis, biosensors represented the best option. Copyright © 2012 Elsevier Ltd. All rights reserved.

  12. ANALISIS RESIDU KLORPIRIFOS DALAM SAYUR-SAYURAN DENGAN TEKNIK HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC

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    Aman Sentosa Panggabean

    2016-06-01

    Full Text Available The research about analysis of chlorpyrifos residue in vegetables by using High Performance Liquid Chromatography (HPLC technique has been done. To obtain the optimal measurement results, the measurement performed several important parameters in the chromatographic system was composition of mobile phase, volume injection sample, flow rate and pH eluent. Optimum measurement conditions obtained was mobile phase composition (water : methanol with 70 : 30, volume injection sample are 5 mL, flow rate are 0.5mL/menit and pH eluent are 7. The analytical performance that obtained is good showed with the reproducibility value as percentage coefficient variance (% CV was 0.0664%, limit of detection (LOD was 0.44 ppm, with a recovery percentage of > 95%. The results obtained showed the HPLC technique can be used for the routine analysis in the determination of chlorpyrifos for the vegetable samples. Keywords: Chlorpyrifos, Vegetables, HPLC.

  13. Analysis of the extracts of Isatis tinctoria by new analytical approaches of HPLC, MS and NMR.

    Science.gov (United States)

    Zhou, Jue; Qu, Fan

    2011-01-01

    The methods of extraction, separation and analysis of alkaloids and indole glucosinolates (GLs) ofIsatis tinctoria were reviewed. Different analytical approaches such as High-pressure Liquid Chromatography (HPLC), Liquid Chromatography with Electrospray Ionization Mass Spectrometry (LC/ESI/MS), Electrospray Ionization Time-Of-Flight Mass Spectrometry (ESI-TOF-MS), and Nuclear Magnetic Resonance (NMR) were used to validate and identity of these constituents. These methods provide rapid separation, identification and quantitative measurements of alkaloids and GLs of Isatis tinctoria. By connection with different detectors to HPLC such as PDA, ELSD, ESI- and APCI-MS in positive and negative ion modes, complicated compounds could be detected with at least two independent detection modes. The molecular formula can be derived in a second step of ESI-TOF-MS data. But for some constituents, UV and MS cannot provide sufficient structure identification. After peak purification, NMR by semi-preparative HPLC can be used as a complementary method.

  14. Brief on -Hyphenated Methods of HPLC for Determining the Presence of Solutes.

    Directory of Open Access Journals (Sweden)

    Mohamad Taleuzzaman

    2017-02-01

    Full Text Available HPLC is the tool in liquid chromatography is unique because of particle size, smaller particle in the stationary phase, increase efficiency of a separation. However, if the particles are made smaller, capillary action increases and it becomes more difficult to drain the column under gravity. For quantitative analysis different types of detector is used in conjunction with HPLC which give precise and accurate result and it is apply according to the nature of the substance. Various types of detectors used in HPLC are mass spectrometry, infrared spectroscopy, visible spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, nuclear magnetic resonance, conductivity measurement, and refractive index measurement. Each detector has its assets, limitations and sample types for which it is most effective. The recent development of the so-called hyphenated techniques has improved the ability to separate and identify multiple entities within a mixture.

  15. A uHPLC-MS mathematical modeling approach to dry powder inhaler single agglomerate analysis.

    Science.gov (United States)

    Pennington, Justin; Lena, John; Medendorp, Joseph; Ewing, Gary

    2011-10-01

    Demonstration of content uniformity (CU) is critical toward the successful development of dry powder inhalers (DPIs). Methods for unit dose CU determination for DPI products are well-established within the field of respiratory science. Recent advances in the area include a uHPLC-MS method for high-throughput uniformity analysis, which allows for a greater understanding of blending operations as the industry transitions to a quality-by-design approach to development. Further enhancements to this uHPLC-MS method now enable it to determine CU and sample weight at the single agglomerate level, which is roughly 50× smaller than a unit dose. When coupled with optical microscopy-based agglomerate sizing, the enhanced uHPLC-MS method can also predict the density and porosity of individual agglomerates. Expanding analytical capabilities to the single agglomerate level provides greater insights and confidence in the DPI manufacturing process.

  16. A novel HPLC method for separation of uranium from thorium using BEHSA modified semi preparative support

    International Nuclear Information System (INIS)

    Raju, Ch.Siva Kesava; Subramanian, M.S.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2006-01-01

    The determination of uranium and thorium is of great importance with respect to nuclear industry and environmental samples. High performance liquid chromatography (HPLC) has revolutionized as a powerful separation and analytical tool in the field of chemistry, biology, medicine, pharmacy, chemical technology, food science and many more. The major advantages of HPLC are its ability to provide rapid, high performance separations and extending the separations range from laboratory scale to preparative scale purification. HPLC became powerful technique for the separation of uranium and thorium. These methods were widely employed in applications such as separation of uranium from fission products and for the measurement of number of fissions as in the case of burn-up measurements on nuclear reactor fuels

  17. Improved method for HPLC analysis of polyamines, agmatine and aromatic monoamines in plant tissue

    Science.gov (United States)

    Slocum, R. D.; Flores, H. E.; Galston, A. W.; Weinstein, L. H.

    1989-01-01

    The high performance liquid chromatographic (HPLC) method of Flores and Galston (1982 Plant Physiol 69: 701) for the separation and quantitation of benzoylated polyamines in plant tissues has been widely adopted by other workers. However, due to previously unrecognized problems associated with the derivatization of agmatine, this important intermediate in plant polyamine metabolism cannot be quantitated using this method. Also, two polyamines, putrescine and diaminopropane, also are not well resolved using this method. A simple modification of the original HPLC procedure greatly improves the separation and quantitation of these amines, and further allows the simulation analysis of phenethylamine and tyramine, which are major monoamine constituents of tobacco and other plant tissues. We have used this modified HPLC method to characterize amine titers in suspension cultured carrot (Daucas carota L.) cells and tobacco (Nicotiana tabacum L.) leaf tissues.

  18. Validated Reverse Phase HPLC Method for the Determination of Impurities in Etoricoxib

    Directory of Open Access Journals (Sweden)

    S. Venugopal

    2011-01-01

    Full Text Available This paper describes the development of reverse phase HPLC method for etoricoxib in the presence of impurities and degradation products generated from the forced degradation studies. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation of etoricoxib was observed under base and oxidation environment. The drug was found stable in other stress conditions studied. Successful separation of the drug from the process related impurities and degradation products were achieved on zorbax SB CN (250 x 4.6 mm 5 μm particle size column using reverse phase HPLC method. The isocratic method employed with a mixture of buffer and acetonitrile in a ratio of 60:40 respectively. Disodium hydrogen orthophosphate (0.02 M is used as buffer and pH adjusted to 7.20 with 1 N sodium hydroxide solution. The HPLC method was developed and validated with respect to linearity, accuracy, precision, specificity and ruggedness.

  19. The integrated quality assessment of Chinese commercial dry red wine based on a method of online HPLC-DAD-CL combined with HPLC-ESI-MS.

    Science.gov (United States)

    Yu, Hai-Xiang; Sun, Li-Qiong; Qi, Jin

    2014-07-01

    To apply an integrated quality assessment strategy to investigate the quality of multiple Chinese commercial dry red wine samples. A comprehensive method was developed by combining a high performance liquid chromatography-diode array detector-chemiluminescence (HPLC-DAD-CL) online hyphenated system with an HPLC-ESI-MS technique. Chromatographic and H2O2-scavenging active fingerprints of thirteen batches of different, commercially available Chinese dry red wine samples were obtained and analyzed. Twenty-five compounds, including eighteen antioxidants were identified and evaluated. The dominant and characteristic antioxidants in the samples were identified. The relationships between antioxidant potency and the cultivated variety of grape, producing area, cellaring period, and trade mark are also discussed. The results provide the feasibility for an integrated quality assessment strategy to be efficiently and objectively used in quality (especially antioxidant activity) assessment and identification of dry red wine. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  20. Cluster analysis of commercial samples of Bauhinia spp. using HPLC-UV/PDA and MCR-ALS/PCA without peak alignment procedure.

    Science.gov (United States)

    Ardila, Jorge Armando; Funari, Cristiano Soleo; Andrade, André Marques; Cavalheiro, Alberto José; Carneiro, Renato Lajarim

    2015-01-01

    Bauhinia forficata Link. is recognised by the Brazilian Health Ministry as a treatment of hypoglycemia and diabetes. Analytical methods are useful to assess the plant identity due the similarities found in plants from Bauhinia spp. HPLC-UV/PDA in combination with chemometric tools is an alternative widely used and suitable for authentication of plant material, however, the shifts of retention times for similar compounds in different samples is a problem. To perform comparisons between the authentic medicinal plant (Bauhinia forficata Link.) and samples commercially available in drugstores claiming to be "Bauhinia spp. to treat diabetes" and to evaluate the performance of multivariate curve resolution - alternating least squares (MCR-ALS) associated to principal component analysis (PCA) when compared to pure PCA. HPLC-UV/PDA data obtained from extracts of leaves were evaluated employing a combination of MCR-ALS and PCA, which allowed the use of the full chromatographic and spectrometric information without the need of peak alignment procedures. The use of MCR-ALS/PCA showed better results than the conventional PCA using only one wavelength. Only two of nine commercial samples presented characteristics similar to the authentic Bauhinia forficata spp., considering the full HPLC-UV/PDA data. The combination of MCR-ALS and PCA is very useful when applied to a group of samples where a general alignment procedure could not be applied due to the different chromatographic profiles. This work also demonstrates the need of more strict control from the health authorities regarding herbal products available on the market. Copyright © 2015 John Wiley & Sons, Ltd.

  1. Comparison of piracetam measured with HPLC-DAD, HPLC-ESI-MS, DIP-APCI-MS, and a newly developed and optimized DIP-ESI-MS.

    Science.gov (United States)

    Lenzen, Claudia; Winterfeld, Gottfried A; Schmitz, Oliver J

    2016-06-01

    The direct inlet probe-electrospray ionization (DIP-ESI) presented here was based on the direct inlet probe-atmospheric pressure chemical ionization (DIP-APCI) developed by our group. It was coupled to an ion trap mass spectrometer (MS) for the detection of more polar compounds such as degradation products from pharmaceuticals. First, the position of the ESI tip, the gas and solvent flow rates, as well as the gas temperature were optimized with the help of the statistic program Minitab® 17 and a caffeine standard. The ability to perform quantitative analyses was also tested by using different concentrations of caffeine and camphor. Calibration curves with a quadratic calibration regression of R (2) = 0.9997 and 0.9998 for caffeine and camphor, respectively, were obtained. The limit of detection of 2.5 and 1.7 ng per injection for caffeine and camphor were determined, respectively. Furthermore, a solution of piracetam was used to compare established analytical methods for this drug and its impurities such as HPLC-diode array detector (DAD) and HPLC-ESI-MS with the DIP-APCI and the developed DIP-ESI. With HPLC-DAD and 10 μg piracetam on column, no impurity could be detected. With HPLC-ESI-MS, two impurities (A and B) were identified with only 4.6 μg piracetam on column, while with DIP-ESI, an amount of 1.6 μg piracetam was sufficient. In the case of the DIP-ESI measurements, all detected impurities could be identified by MS/MS studies. Graphical Abstract Scheme of the DIP-ESI principle.

  2. Screening and Analysis of the Potential Bioactive Components of Poria cocos (Schw. Wolf by HPLC and HPLC-MSn with the Aid of Chemometrics

    Directory of Open Access Journals (Sweden)

    Ling-Fang Wu

    2016-02-01

    Full Text Available The aim of the present study was to establish a new method based on Similarity Analysis (SA, Cluster Analysis (CA and Principal Component Analysis (PCA to determine the quality of different samples of Poria cocos (Schw. Wolf obtained from Yunnan, Hubei, Guizhou, Fujian, Henan, Guangxi, Anhui and Sichuan in China. For this purpose 15 samples from the different habitats were analyzed by HPLC-PAD and HPLC-MSn. Twenty-three compounds were detected by HPLC-MSn, of which twenty compounds were tentatively identified by comparing their retention times and mass spectrometry data with that of reference compounds and reviewing the literature. The characteristic fragmentations were summarized. 3-epi-Dehydrotumulosic acid (F13, 3-oxo-16α,25-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F4, 3-oxo-6,16α-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F7 and dehydropachymic acid (F15 were deemed to be suitable marker compounds to distinguish between samples of different quality according to CA and PCA. This study provides helpful chemical information for further anti-tumor activity and active mechanism research on P. cocos. The results proved that fingerprint combined with a chemometric approach is a simple, rapid and effective method for the quality discrimination of P. cocos.

  3. Morphological mutants of Neurospora crassa: possible evidence of abnormal morphology due to changes in DNA composition

    Energy Technology Data Exchange (ETDEWEB)

    Chaudhuri, R K; Dutta, S.K. Ojha, M.

    1973-01-01

    DNA from seven experimentally induced morphological mutants and the wild type strain 74A of Neurospora crassa showed typical bimodal denaturation profiles in a Gilford 2400 spectrophotometer. The ''slime'' and ''ropy'' mutants showed a comparatively high proportion of A + T rich DNA sequences. Studies on thermal denaturation, percent hybridization, and thermal stability indicate the DNA sequences of the slime mutant were distinctly different from the normal genomes of parental DNA as well as other wild type DNAs. No such difference was noticed in any other mutant and natural isolate of the species N. crassa tested. These studies indicate possible correlation between a change in DNA nucleotide sequences and abnormal morphogenesis.

  4. Quality control of radiopharmaceuticals with HPLC using aqueous size exclusion spherogel column

    International Nuclear Information System (INIS)

    Vallabhajosula, S.; Goldsmith, S.J.; Lipszyc, H.

    1982-01-01

    The application of HPLC for the analysis and quality control of 99 Tc-radiopharmaceuticals, using a weakly basic anion exchange column, has been reported. This HPLC method for the separation of the components is based on molecular size. 99 Tc-MDP, 99 Tc-HDP and 99 Tc-DTPA were analysed and UV absorption studies carried out on the components. Components of the 99 Tc-MDP separation were injected into rabbits and renal excretion and serial images studied. (U.K.)

  5. Determination of boron in uranium and aluminium by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rao, Radhika M.; Aggarwal, S.K.

    2003-01-01

    Experiments were conducted for the determination of boron in U 3 O 8 powder and aluminium metal using dynamically modified reversed phase high pressure liquid chromatography (RP-HPLC) and using precolumn chromogenic agent viz. curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-1,3-hexane diol (EHD). Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed and used for the determination of boron in aluminium and uranium samples. (author)

  6. Use of HPLC with flow-through radiometric detection for low level environmental analysis

    International Nuclear Information System (INIS)

    Mao, J.; Fackler, P.H.

    1992-01-01

    High Performance Liquid Chromatography with flow-through radiometric detection (HPLC-RAM) is increasingly becoming a standard analytical technique in pharmaceutical, agricultural and chemical industries for monitoring radiolabeled analytes. This paper focuses on the applications of this flow-through radiochromatographic technique for low level aquatic toxicology and environmental fate testing. Examples include parts per billion water, sediment/soil and fish tissue analyses using reverse phase as well as normal phase HPLC. The applications of both homogeneous (liquid) and heterogeneous (solid) flow cell scintillation counting are addressed. Compounds discussed are primarily pesticides and pharmaceuticals

  7. Pharmacokinetic study of arctigenin in rat plasma and organ tissue by RP-HPLC method.

    Science.gov (United States)

    He, Fan; Dou, De-Qiang; Hou, Qiang; Sun, Yu; Kang, Ting-Guo

    2013-01-01

    A high-performance liquid chromatography (HPLC) technique was developed for the determination of arctigenin in plasma and various organs of rats after the oral administration of 30, 50 and 70 mgkg(-1) of arctigenin to the Sprague-Dawley rats. Results showed that the validated HPLC method was simple, fast, reproducible and suitable to the determination of arctigenin in rat plasma and organ tissue and one-compartmental model with zero-order absorption process can well describe the changes of arctigenin concentration in the plasma. The concentration of compound was highest in the spleen, less in the liver and the least in the lung.

  8. [Study on HPLC-FPS of raw and processed fructus polygoni orientalis].

    Science.gov (United States)

    Zhai, Yanjun; Zhao, Min; Zhang, Hui; Chu, Zhengyun; Kang, Tingguo

    2010-03-01

    To establish the HPLC fingerprint method of Fructus Polygoni Orientalis before and after processed by choosing taxifolin as reference to compare the changes of chemical composition. HPLC method was emplyed with a gradient elution phase in a flow rate of 1 mL x min(-1) and the detection wavelength of 270 nm. Twenty marker peaks were marked out in the raw samples and 33 marker peaks in the processed product. Methodology met was consistent with the requirement, similarity was exceeded 0.9. This method is stationary, precise and feasible, which provide references of quality control for Fructus Polygoni Orientalis.

  9. A thin film degradation study of a fluorinated polyether liquid lubricant using an HPLC method

    Science.gov (United States)

    Morales, W.

    1986-01-01

    A High Pressure Liquid Chromatography (HPLC) separation method was developed to study and analyze a fluorinated polyether fluid which is promising liquid lubricant for future applications. This HPLC separation method was used in a preliminary study investigating the catalytic effect of various metal, metal alloy, and ceramic engineering materials on the degradation of this fluid in a dry air atmosphere at 345 C. Using a 440 C stainless steel as a reference catalytic material it was found that a titanium alloy and a chromium plated material degraded the fluorinated polyether fluid substantially more than the reference material.

  10. Principles of Developing Multi-Pesticide Methods Based on HPLC Determination

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    Principles for the development of multi-pesticide methods based on HPLC determination are outlined. Flow charts and block diagrams give guidance on how to proceed stepwise in the set-up of respective analytical methods. Detailed information is provided on what to take into consideration for setting up a pesticide formulation analysis method. HPLC variables like the types of column, solvents and their strength, pH value, eluent modifiers, column temperature, etc, and the influence on the separation and resolution of chromatographic peaks are discussed as well as the necessity and benefits of internal standardization. Examples of system suitability testing experiments are given for illustration. (author)

  11. Differential morphology and image processing.

    Science.gov (United States)

    Maragos, P

    1996-01-01

    Image processing via mathematical morphology has traditionally used geometry to intuitively understand morphological signal operators and set or lattice algebra to analyze them in the space domain. We provide a unified view and analytic tools for morphological image processing that is based on ideas from differential calculus and dynamical systems. This includes ideas on using partial differential or difference equations (PDEs) to model distance propagation or nonlinear multiscale processes in images. We briefly review some nonlinear difference equations that implement discrete distance transforms and relate them to numerical solutions of the eikonal equation of optics. We also review some nonlinear PDEs that model the evolution of multiscale morphological operators and use morphological derivatives. Among the new ideas presented, we develop some general 2-D max/min-sum difference equations that model the space dynamics of 2-D morphological systems (including the distance computations) and some nonlinear signal transforms, called slope transforms, that can analyze these systems in a transform domain in ways conceptually similar to the application of Fourier transforms to linear systems. Thus, distance transforms are shown to be bandpass slope filters. We view the analysis of the multiscale morphological PDEs and of the eikonal PDE solved via weighted distance transforms as a unified area in nonlinear image processing, which we call differential morphology, and briefly discuss its potential applications to image processing and computer vision.

  12. Simultaneous and Direct Determination of Vancomycin and Cephalexin in Human Plasma by Using HPLC-DAD Coupled with Second-Order Calibration Algorithms

    Directory of Open Access Journals (Sweden)

    Le-Qian Hu

    2012-01-01

    Full Text Available A simple, rapid, and sensitive method for the simultaneous determination of vancomycin and cephalexin in human plasma was developed by using HPLC-DAD with second-order calibration algorithms. Instead of a completely chromatographic separation, mathematical separation was performed by using two trilinear decomposition algorithms, that is, PARAFAC-alternative least squares (PARAFAC-ALSs and self-weight-alternative-trilinear-decomposition- (SWATLD- coupled high-performance liquid chromatography with DAD detection. The average recoveries attained from PARAFAC-ALS and SWATLD with the factor number of 4 (N=4 were 101±5% and 102±4% for vancomycin, and 96±3% and 97±3% for cephalexininde in real human samples, respectively. The statistical comparison between PARAFAC-ALS and SWATLD is demonstrated to be similar. The results indicated that the combination of HPLC-DAD detection with second-order calibration algorithms is a powerful tool to quantify the analytes of interest from overlapped chromatographic profiles for complex analysis of drugs in plasma.

  13. Analysis of 26 amino acids in human plasma by HPLC using AQC as derivatizing agent and its application in metabolic laboratory.

    Science.gov (United States)

    Sharma, Gaurav; Attri, Savita Verma; Behra, Bijaylaxmi; Bhisikar, Swapnil; Kumar, Praveen; Tageja, Minni; Sharda, Sheetal; Singhi, Pratibha; Singhi, Sunit

    2014-05-01

    The present study reports the simultaneous analysis of 26 physiological amino acids in plasma along with total cysteine and homocysteine by high-performance liquid chromatography (HPLC) employing 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) as precolumn derivatizing reagent. Separations were carried out using Lichrospher 100 RP-18e (5 μm) 250 × 4.0 mm column connected to 100 CN 4.0 × 4.0 mm guard column on a quaternary HPLC system and run time was 53 min. Linearity of the peak areas for different concentrations ranging from 2.5 to 100 pmol/μL of individual amino acids was determined. A good linearity (R (2) > 0.998) was achieved in the standard mixture for each amino acid. Recovery of amino acids incorporated at the time of derivatization ranged from 95 to 106 %. Using this method we have established the normative data of amino acids in plasma, the profile being comparable to the range reported in literature and identified cases of classical homocystinuria, cobalamin defect/deficiency, non-ketotic hyperglycinemia, hyperprolinemia, ketotic hyperglycinemia, urea cycle defect and maple syrup urine disease.

  14. Characterization of chemical constituents in Rhodiola Crenulate by high-performance liquid chromatography coupled with Fourier-transform ion cyclotron resonance mass spectrometer (HPLC-FT-ICR MS).

    Science.gov (United States)

    Han, Fei; Li, Yanting; Mao, Xinjuan; Xu, Rui; Yin, Ran

    2016-05-01

    In this work, an approach using high-performance liquid chromatography coupled with diode-array detection and Fourier-transform ion cyclotron resonance mass spectrometer (HPLC-FT-ICR MS) for the identification and profiling of chemical constituents in Rhodiola crenulata was developed for the first time. The chromatographic separation was achieved on an Inertsil ODS-3 column (150 mm × 4.6 mm,3 µm) using a gradient elution program, and the detection was performed on a Bruker Solarix 7.0 T mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 48 chemical compounds, including 26 alcohols and their glycosides, 12 flavonoids and their glycosides, 5 flavanols and gallic acid derivatives, 4 organic acids and 1 cyanogenic glycoside were identified or tentatively characterized. The results indicated that the developed HPLC-FT-ICR MS method with ultra-high sensitivity and resolution is suitable for identifying and characterizing the chemical constituents in R. crenulata. And it provides a helpful chemical basis for further research on R. crenulata. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  15. An optimized high-performance liquid chromatography (HPLC method for benzoylmesaconine determination in Radix Aconiti Lateralis Preparata (Fuzi, aconite roots and its products

    Directory of Open Access Journals (Sweden)

    Xu Hongxi

    2008-05-01

    Full Text Available Abstract Background Benzoylmesaconine (BMA is the main Aconitum alkaloid in Radix Aconiti Lateralis Preparata (Fuzi, aconite roots with potent pharmacological activities, such as analgesia and anti-inflammation. The present study developed a simple and reliable method using BMA as a marker compound for the quality control of processed aconite roots and their products. Methods After extraction, a high-performance liquid chromatography (HPLC determination of BMA was conducted on a RP-C18 column by gradient elution with acetonitrile and aqueous phase, containing 0.1% phosphoric acid adjusted with triethylamine to pH 3.0. Results A distinct peak profile was obtained and separation of BMA was achieved. Method validation showed that the relative standard deviations (RSDs of the precision of BMA in all intra-day and inter-day assays were less than 1.36%, and that the average recovery rate was 96.95%. Quantitative analysis of BMA showed that the content of BMA varied significantly in processed aconite roots and their products. Conclusion This HPLC method using BMA as a marker compound is applicable to the quality control of processed aconite roots and their products.

  16. In Vitro Anticariogenic Effects of Drymocallis rupestris Extracts and Their Quality Evaluation by HPLC-DAD-MS3 Analysis

    Directory of Open Access Journals (Sweden)

    Sebastian Granica

    2013-07-01

    Full Text Available In this study, for the first time, we investigated in vitro inhibitory effects of Drymocallis rupestris extracts and their subfractions obtained with solvents of different polarity (aqueous, 50% ethanolic, diethyl ether, ethyl acetate and n-butanolic against bacterial viability and caries virulence factors of Streptococcus spp. strains. The diethyl ether subfraction (PRU2 showed bacteriostatic and bactericidal activity against mutans streptococci, with minimum inhibitory concentrations (MICs in the range of 0.75–1.5 mg/mL and minimum bactericidal concentrations (MBCs in the range of 1.5–3 mg/mL. Furthermore, PRU2 inhibited biofilm formation by Streptococci in a dose-dependent manner. It was also found that all five D. rupestris preparations exhibited diverse inhibitory effects on de novo synthesis of water-insoluble and water-soluble α-d-glucans by glucosyltransferases of the mutans group streptococci. The phytochemical profile of investigated samples was determined by spectrophotometric and chromatographic (HPLC-DAD-MS3 methods. The high polyphenol (total phenol, phenolic acids, tannins, proantocyanidins, and flavonoids contents were found which correlated with anticariogenic activity of the analyzed samples. The results demonstrate that D. rupestris extracts and their subfractions could become useful supplements for pharmaceutical products as a new anticariogenic agent in a wide range of oral care products. Further studies are necessary to clarify which phytoconstituents of D. rupestris are responsible for anticaries properties.

  17. Occurrence of toxigenic fungi and determination of mycotoxins by HPLC-FLD in functional foods and spices in China markets.

    Science.gov (United States)

    Kong, Weijun; Wei, Riwei; Logrieco, Antonio F; Wei, Jianhe; Wen, Jing; Xiao, Xiaohe; Yang, Meihua

    2014-03-01

    Twenty-four samples including 14 functional foods and 10 spices obtained from Chinese markets were examined for their mould profile. The mycotoxin contamination levels were also determined by an optimized HPLC-FLD method. 124 fungal isolates belonging to four different genera were recovered with Aspergillus and Penicillium as predominant fungi, with an incidence of 66.1% and 15.3%, respectively. In functional foods Aspergillus niger section (57.1%) was isolated more frequently, followed by Aspergillus flavi section (50.0%) and Aspergillus ochraceus section (21.4%), with the most contaminated samples being Coix seeds. Similar fungal presence and frequency were encountered in spice with A. niger section group (60.0%) and A. flavi section (40.0%) as main fungi. Cumin and Pricklyash peel samples showed the highest fungal contamination. Four functional foods and three spices were found to be positive at low levels for mycotoxins including aflatoxin B1 (up to 0.26μg/kg) and ochratoxin A (OTA) (5.0μg/kg). The more frequently detected mycotoxin was AFB1 (16.7%). Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Nutritional Composition and Antioxidant Capacity in Edible Flowers: Characterisation of Phenolic Compounds by HPLC-DAD-ESI/MSn

    Directory of Open Access Journals (Sweden)

    Inmaculada Navarro-González

    2014-12-01

    Full Text Available Edible flowers are commonly used in human nutrition and their consumption has increased in recent years. The aim of this study was to ascertain the nutritional composition and the content and profile of phenolic compounds of three edible flowers, monks cress (Tropaeolum majus, marigold (Tagetes erecta and paracress (Spilanthes oleracea, and to determine the relationship between the presence of phenolic compounds and the antioxidant capacity. Proximate composition, total dietary fibre (TDF and minerals were analysed according to official methods: total phenolic compounds (TPC were determined with Folin-Ciocalteu’s reagent, whereas antioxidant capacity was evaluated using Trolox Equivalent Antioxidant Capacity (TEAC and Oxygen Radical Absorbance Capacity (ORAC assays. In addition, phenolic compounds were characterised by HPLC-DAD-MSn. In relation to the nutritional value, the edible flowers had a composition similar to that of other plant foods, with a high water and TDF content, low protein content and very low proportion of total fat—showing significant differences among samples. The levels of TPC compounds and the antioxidant capacity were significantly higher in T. erecta, followed by S. oleracea and T. majus. Thirty-nine different phenolic compounds were tentatively identified, with flavonols being the major compounds detected in all samples, followed by anthocyanins and hydroxycynnamic acid derivatives. In T. erecta small proportions of gallotannin and ellagic acid were also identified.

  19. An HPLC-UV method for the measurement of permeability of marker drugs in the Caco-2 cell assay

    Directory of Open Access Journals (Sweden)

    J.M. Kratz

    2011-06-01

    Full Text Available The Caco-2 cell line has been used as a model to predict the in vitro permeability of the human intestinal barrier. The predictive potential of the assay relies on an appropriate in-house validation of the method. The objective of the present study was to develop a single HPLC-UV method for the identification and quantitation of marker drugs and to determine the suitability of the Caco-2 cell permeability assay. A simple chromatographic method was developed for the simultaneous determination of both passively (propranolol, carbamazepine, acyclovir, and hydrochlorothiazide and actively transported drugs (vinblastine and verapamil. Separation was achieved on a C18 column with step-gradient elution (acetonitrile and aqueous solution of ammonium acetate, pH 3.0 at a flow rate of 1.0 mL/min and UV detection at 275 nm during the total run time of 35 min. The method was validated and found to be specific, linear, precise, and accurate. This chromatographic system can be readily used on a routine basis and its utilization can be extended to other permeability models. The results obtained in the Caco-2 bi-directional transport experiments confirmed the validity of the assay, given that high and low permeability profiles were identified, and P-glycoprotein functionality was established.

  20. Quality evaluation of Houttuynia cordata Thunb. by high performance liquid chromatography with photodiode-array detection (HPLC-DAD).

    Science.gov (United States)

    Yang, Zhan-nan; Sun, Yi-ming; Luo, Shi-qiong; Chen, Jin-wu; Chen, Jin-wu; Yu, Zheng-wen; Sun, Min

    2014-03-01

    A new, validated method, developed for the simultaneous determination of 16 phenolics (chlorogenic acid, scopoletin, vitexin, rutin, afzelin, isoquercitrin, narirutin, kaempferitrin, quercitrin, quercetin, kaempferol, chrysosplenol D, vitexicarpin, 5-hydroxy-3,3',4',7-tetramethoxy flavonoids, 5-hydroxy-3,4',6,7-tetramethoxy flavonoids and kaempferol-3,7,4'-trimethyl ether) in Houttuynia cordata Thunb. was successfully applied to 35 batches of samples collected from different regions or at different times and their total antioxidant activities (TAAs) were investigated. The aim was to develop a quality control method to simultaneously determine the major active components in H. cordata. The HPLC-DAD method was performed using a reverse-phase C18 column with a gradient elution system (acetonitrile-methanol-water) and simultaneous detection at 345 nm. Linear behaviors of method for all the analytes were observed with linear regression relationship (r(2)>0.999) at the concentration ranges investigated. The recoveries of the 16 phenolics ranged from 98.93% to 101.26%. The samples analyzed were differentiated and classified based on the contents of the 16 characteristic compounds and the TAA using hierarchical clustering analysis (HCA) and principal component analysis (PCA). The results analyzed showed that similar chemical profiles and TAAs were divided into the same group. There was some evidence that active compounds, although they varied significantly, may possess uniform anti-oxidant activities and have potentially synergistic effects.

  1. Morphology of open bite.

    Science.gov (United States)

    Krey, Karl-Friedrich; Dannhauer, Karl-Heinz; Hierl, Thomas

    2015-05-01

    The purpose of this work was to define and illustrate the skeletal morphology of open-bite patients against the background of sagittal jaw relationships on the basis of lateral cephalograms. Lateral cephalograms of 197 untreated adults were analyzed in dental imaging software (Onyx Ceph 3™; Image Instruments, Chemnitz, Germany). Four groups were formed based on vertical (Index scores) and sagittal (individualized ANB values) parameters. Ninety-nine patients were defined as the control group due to their neutral sagittal and vertical relationships. The remaining patients were found by their vertical relationships to represent open-bite cases and were divided by their sagittal relationships into three study groups: neutral (Class I, n = 34), distal (Class II, n = 26), and mesial (Class III, n = 38). A geometric morphometric approach was used to analyze the x,y-coordinates of 28 skeletal landmarks on each cephalogram. Relative size was captured based on centroid size (CS). The shape-determining factors in the groups were compared by permutation testing after Procrustes transformation, and intergroup differences were visualized in the form of thin-plate splines. While size (CS) was significantly increased in the Class III group, the other two groups were not different from the control group. After Procrustes transformation, characteristic and invariably significant (p common that the mandibular ramus is compressed, but marked differences are seen in terms of vertical development of the maxilla. This differentiated view of open-bite cases should be taken into consideration during individual etiology assessment and treatment planning.

  2. Characterization of bioactive compounds of Annona cherimola L. leaves using a combined approach based on HPLC-ESI-TOF-MS and NMR.

    Science.gov (United States)

    Díaz-de-Cerio, Elixabet; Aguilera-Saez, Luis Manuel; Gómez-Caravaca, Ana María; Verardo, Vito; Fernández-Gutiérrez, Alberto; Fernández, Ignacio; Arráez-Román, David

    2018-06-01

    Annona cherimola Mill. (cherimoya) has widely been used as food crop. The leaves of this tree possess several health benefits, which are, in general, attributed mainly to its bioactive composition. However, literature concerning a comprehensive characterization based on a combined approach, which consists of nuclear magnetic resonance (NMR) and high-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-TOF-MS), from these leaves is scarce. Thus, the aim of this work was to study the polar profile of full extracts of cherimoya leaves by using these tools. Thus, a total of 77 compounds have been characterized, 12 of which were identified by both techniques. Briefly, 23 compounds were classified as amino acids, organic acids, carbohydrates, cholines, phenolic acid derivatives, and flavonoids by NMR, while 66 metabolites were divided into sugars, amino acids, phenolic acids and derivatives, flavonoids, phenylpropanoids, and other polar compounds by HPLC-TOF-MS. It is worth mentioning that different solvent mixtures were tested and the total phenolic content in the extracts quantified (TPC via HPLC-TOF-MS). The tendency observed was EtOH/water 80/20 (v/v) (17.0 ± 0.2 mg TPC/g leaf dry weight (d.w.)) ≥ acetone/water 70/30 (v/v) (16.1 ± 0.7 mg TPC/g leaf d.w.) > EtOH/water 70/30 (v/v) (14.0 ± 0.3 mg TPC/g leaf d.w.) > acetone/water 80/20 (v/v) (13.5 ± 0.4 mg TPC/g leaf d.w.). Importantly, flavonoids derivatives were between 63 and 76% of the TPC in those extracts. Major compounds were sucrose, glucose (α and β), and proline, and chlorogenic acid and rutin for NMR and HPLC-TOF-MS, respectively. Graphical abstract The combined use of LC-HRMS and NMR is a potential synergic combination for a comprehensive metabolite composition of cherimoya leaves.

  3. Analysis of molecular species of triacylglycerols from vegetable oils containing fatty acids with non-methylene-interrupted double bonds, by HPLC in the silver-ion mode

    Energy Technology Data Exchange (ETDEWEB)

    Joh, Y.; Kim, S. [Dong A Univ., Pusan (Korea, Republic of)

    1998-10-20

    The possibilities for application of silver ion HPLC to analysis of the triacylglycerols containing conjugate trienoic acids and {Delta}{sup 5}-polymethylene-interrupted acids and proportions of triacylglycerol fractions obtained by silver-ion HPLC from the seed oil of Momordica charantia double bonds were examined, respectively. The triacylglycerols of seed oils containing conjugate trienoic acids such as {alpha}-eleostearic acid (C{sub 18:3 9c,11t,13t}) and punicic acid (C{sub 18:3} {sub 9c,11t,13c}) were resolved by silver-ion HPLC. Fractions were fractionated on the basis of the number and configuration of double bonds in the species, and the elution profile is quite different from that of the species comprising exclusively saturated and unsaturated fatty acids with methylene-interrupted double bonds ; for instance, the species (DT(c2)) composed of one dienoic acid and two conjugate trienoic acids eluted much earlier than the species (D{sub 2}T{sub c}) composed of two dienoic acids and one conjugate trienoic acid, in spite of having larger number of double bonds. This means that the interaction of conjugate double bonds with silver ions is weaker than that of methylene-interrupted double bonds, presumably because of the delocalization of {pi}-electrons in conjugate double bonds. In this instance, the strength of interaction of a conjugate trienoic double bond system with silver ions seemed to be between that of methylene-interrupted dienoic and monoenoic double bond systems. Triacylglycerols of the seeds of Ginkgo biloba have been resolved by HPLC in the silver-ion mode according to the number and position of double bonds. In this instance, the strength of interaction between the {pi}-electrons of double bonds in the fatty acyl residues and silver ions is in the order; C{sub 18:3{omega}3}>C(20:3){Delta}{sup 5,11,14}C{sub 18:3}{Delta}{sup 5,9,12}>= C{sub 18:2{omega}6}>C{sub 18:2}{Delta}{sup 5,9}>C{sub 18:1{omega}9}>C{sub 18:1ome= ga7}. 49 refs., 2 figs., 2 tabs.

  4. A novel HPLC-ESI-Q-ToF approach for the determination of fatty acids and acylglycerols in food samples.

    Science.gov (United States)

    La Nasa, Jacopo; Degano, Ilaria; Brandolini, Leonardo; Modugno, Francesca; Bonaduce, Ilaria

    2018-07-12

    We propose a new analytical method using reverse phase High performance liquid chromatography (HPLC) coupled through an electrospray source with a tandem quadrupole-time-of-flight (ESI-Q-ToF) mass spectrometric detector for the full characterization and quantitation of the different classes of fatty acids and acylglycerols in lipid samples in a single chromatographic run. In this work, we optimized the derivatization reaction for free fatty acids with 2-hydrazinoquinoline, which is a low-cost approach, using a full factorial design. This reaction does not involve transesterification, thus enabling the free fatty acids to be separated and successfully quantified in the presence of mono-, di- and triacylglycerols without altering the whole glyceride profile. This new analytical method provides a full profile of fatty acids, mono-, di- and triglycerides within a relatively short chromatographic run (less than 40 min), with low operating back-pressure (less than 110 bar). The derivatization of the free fatty acids allows their detection in positive mode, with limits of detection in the range of 0.2-1.9 ng/g, and a dynamic range of two orders of magnitude. The figures of merit of the procedure are competitive with respect to the literature. The method was validated by characterizing two different types of olive oils. Free fatty acid content was quantified, and the results are consistent with literature data. The method was applied to the characterization of cow milk and an infant formula, after the precipitation of proteins and phospholipids, and proved suitable for the detection of short chain fatty acids, free fatty acids and glycerides highlighting differences in the composition of the two milks. The proposed procedure improves the current methods for the analysis of acylglyceride based materials, such as olive oil, and proved promising for the characterization of lipids in complex matrices, such as milk. Copyright © 2018 Elsevier B.V. All rights reserved.

  5. Targeting high-performance liquid chromatography-high-resolution mass spectrometry-solid-phase extraction-nuclear magnetic resonance analysis with high-resolution radical scavenging profiles - bioactive secondary metabolites from the endophytic fungus Penicillium namyslowskii

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Nyberg, Nils; Tejesvi, Mysore V.

    2013-01-01

    The high-resolution radical scavenging profile of an extract of the endophytic fungus Penicillium namyslowskii was used to target analysis by high-performance liquid chromatography-high-resolution mass spectrometry-solid-phase extraction-nuclear magnetic resonance spectroscopy, i.e., HPLC...... NMR probe designed for 1.7-mm NMR tubes. To further explore the potential of the above HPLC-HRMS-SPE-NMR platform for analysis of endophytic extracts, six peaks displaying no radical scavenging activity were also analyzed. This allowed unambiguous identification of six metabolites, i...... and griseofulvin, directly from crude extract via HPLC-HRMS-SPE-NMR. Dechlorodehydrogriseofulvin was reported for the first time from nature....

  6. Application of ABTS radical cation for selective on-line detection of radical scavengers in HPLC eluates

    NARCIS (Netherlands)

    Koleva, [No Value; Niederlander, HAG; van Beek, TA

    2001-01-01

    The radical cation 2,2 ' -azinobis-(3 -ethylbenzothiazoline-6-sulfonate), (ABTS(.+)) was utilized in an on-line HPLC method for the detection of radical scavengers in complex matrixes. The HPLC-separated analytes react postcolumn with the preformed ABTS(.+), and the induced bleaching is detected as

  7. Competitive Nitration of Benzene-Fluorobenzene and Benzene-Toluene Mixtures: Orientation and Reactivity Studies Using HPLC

    Science.gov (United States)

    Blankespoor, Ronald L.; Hogendoorn, Stephanie; Pearson, Andrea

    2007-01-01

    The reactivity and orientation effects of a substituent are analyzed by using HPLC to determine the competitive nitration of the benzene-toluene and benzene-fluorobenzene mixtures. The results have shown that HPLC is an excellent instrumental method to use in analyzing these mixtures.

  8. The first use of a HPLC system at a Louisiana Sugarcane Factory: What it can do for you

    Science.gov (United States)

    Alma Plantation sugarcane factory established and operated the first High Performance Liquid Chromatography (HPLC) system in Louisiana in 2015. Although many HPLC systems exist, the factory opted for a ThermoFisherTM ion chromatography (anion exchange) system with integrated pulsed amperometric det...

  9. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Characterisation of oligosaccharides in vegetables by HPLC and MALDI-TOF MS

    Czech Academy of Sciences Publication Activity Database

    Štikarovská, M.; Chmelík, Josef

    96(S), - (2002), s. S189-S191 ISSN 0009-2770. [Meeting of Chemistry & Life /2./. Brno, 10.09.2002-11.09.2002] Institutional research plan: CEZ:AV0Z4031919 Keywords : oligosaccharides * HPLC * MALDI-TOF-MS Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.336, year: 2002

  11. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasawa, Koji, E-mail: koji180@pharm.showa-u.ac.jp; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-02-15

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H{sub 2}O{sub 2} and O{sub 2}{sup −} generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  12. Quantitative HPLC analysis of some marker compounds of hydroalcoholic extracts of Piper aduncum L

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Laura C.P.; Nunomura, Sergio M. [Instituto Nacional de Pesquisas da Amazonia (INPA), Manaus, AM (Brazil). Coordenacao de Pesquisas em Produtos Naturais]. E-mail: smnunomu@inpa.gov.br; Mause, Robert [Siema Eco Essencias da Amazonia Ltda., Manaus, AM (Brazil)

    2005-11-15

    High performance liquid chromatography is one of the major analytical techniques used in the quality control of phytotherapics. This work describes a HPLC method used to determine the major components present in different hydroalcoholic extracts of aerial parts of Piper aduncum. (author)

  13. A Decomposition Model for HPLC-DAD Data Set and Its Solution by Particle Swarm Optimization

    Directory of Open Access Journals (Sweden)

    Lizhi Cui

    2014-01-01

    Full Text Available This paper proposes a separation method, based on the model of Generalized Reference Curve Measurement and the algorithm of Particle Swarm Optimization (GRCM-PSO, for the High Performance Liquid Chromatography with Diode Array Detection (HPLC-DAD data set. Firstly, initial parameters are generated to construct reference curves for the chromatogram peaks of the compounds based on its physical principle. Then, a General Reference Curve Measurement (GRCM model is designed to transform these parameters to scalar values, which indicate the fitness for all parameters. Thirdly, rough solutions are found by searching individual target for every parameter, and reinitialization only around these rough solutions is executed. Then, the Particle Swarm Optimization (PSO algorithm is adopted to obtain the optimal parameters by minimizing the fitness of these new parameters given by the GRCM model. Finally, spectra for the compounds are estimated based on the optimal parameters and the HPLC-DAD data set. Through simulations and experiments, following conclusions are drawn: (1 the GRCM-PSO method can separate the chromatogram peaks and spectra from the HPLC-DAD data set without knowing the number of the compounds in advance even when severe overlap and white noise exist; (2 the GRCM-PSO method is able to handle the real HPLC-DAD data set.

  14. Two Validated HPLC Methods for the Quantification of Alizarin and other Anthraquinones in Rubia tinctorum Cultivars

    NARCIS (Netherlands)

    Derksen, G.C.H.; Lelyveld, G.P.; Beek, van T.A.; Capelle, A.; Groot, de Æ.

    2004-01-01

    Direct and indirect HPLC-UV methods for the quantitative determination of anthraquinones in dried madder root have been developed, validated and compared. In the direct method, madder root was extracted twice with refluxing ethanol-water. This method allowed the determination of the two major native

  15. A simple method for HPLC retention time prediction: linear calibration using two reference substances.

    Science.gov (United States)

    Sun, Lei; Jin, Hong-Yu; Tian, Run-Tao; Wang, Ming-Juan; Liu, Li-Na; Ye, Liu-Ping; Zuo, Tian-Tian; Ma, Shuang-Cheng

    2017-01-01

    Analysis of related substances in pharmaceutical chemicals and multi-components in traditional Chinese medicines needs bulk of reference substances to identify the chromatographic peaks accurately. But the reference substances are costly. Thus, the relative retention (RR) method has been widely adopted in pharmacopoeias and literatures for characterizing HPLC behaviors of those reference substances unavailable. The problem is it is difficult to reproduce the RR on different columns due to the error between measured retention time (t R ) and predicted t R in some cases. Therefore, it is useful to develop an alternative and simple method for prediction of t R accurately. In the present study, based on the thermodynamic theory of HPLC, a method named linear calibration using two reference substances (LCTRS) was proposed. The method includes three steps, procedure of two points prediction, procedure of validation by multiple points regression and sequential matching. The t R of compounds on a HPLC column can be calculated by standard retention time and linear relationship. The method was validated in two medicines on 30 columns. It was demonstrated that, LCTRS method is simple, but more accurate and more robust on different HPLC columns than RR method. Hence quality standards using LCTRS method are easy to reproduce in different laboratories with lower cost of reference substances.

  16. Apparent loss of urinary albumin during long-term frozen storage : HPLC vs immunonephelometry

    NARCIS (Netherlands)

    Brinkman, Jacoline W.; De Zeeuw, Dick; Lambers Heerspink, Hiddo J.; Gansevoort, Ronald T.; Kema, Ido P.; de Jong, Paul E.; Bakker, Stephan J. L.

    Background: Urinary albumin detection by immuno-nephelometry is decreased by -30% in samples that have been frozen at -20 degrees C. An HPLC method for assessment of urinary albumin that detects immunoreactive and immunochemically nonreactive albumin has been introduced as an alternative to

  17. Quantitative HPLC analysis of some marker compounds of hydroalcoholic extracts of Piper aduncum L

    International Nuclear Information System (INIS)

    Oliveira, Laura C.P.; Nunomura, Sergio M.

    2005-01-01

    High performance liquid chromatography is one of the major analytical techniques used in the quality control of phytotherapics. This work describes a HPLC method used to determine the major components present in different hydroalcoholic extracts of aerial parts of Piper aduncum. (author)

  18. Ellagitannin composition of blackberry as determined by HPLC-ESI-MS and MALDI-TOF-MS.

    Science.gov (United States)

    Hager, Tiffany J; Howard, Luke R; Liyanage, Rohana; Lay, Jackson O; Prior, Ronald L

    2008-02-13

    Blackberries ( Rubus sp.) were evaluated by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF-MS) to identify the ellagitannins present in flesh, torus (receptacle tissue), and seeds. Most ellagitannins were present (or detectable) only in seed tissues. Ellagitannins identified by HPLC-ESI-MS in the seeds included pedunculagin, casuarictin/potentillin, castalagin/vescalagin, lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D. For several of the ellagitannins, isomeric separation was also obtained. The MALDI-TOF-MS analysis was primarily utilized to evaluate and identify high molecular mass (>1000 Da) ellagitannins. The MALDI analysis verified the presence of the ellagitannins identified by HPLC-ESI-MS including lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D, but the analysis also indicated the presence of several other compounds that were most likely ellagitannins based on the patterns observed in the masses (i.e., loss or addition of a gallic acid moiety to a known ellagitannin). This study determined the presence of several possible isomeric forms of ellagitannins previously unidentified in fruit and presents a possible analytical HPLC method for the analysis of the major ellagitannins present in the fruit.

  19. A NEW HPLC METHOD FOR SEPARATION OF PHYTOPLANKTON PIGMENTS IN NATURAL SAMPLES

    Science.gov (United States)

    A new high-performance liquid chromatographic (HPLC) method was developed to analyze, in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a reverse-phase amide C16 (RP-amide C16) column and an elution gradient o...

  20. An optimized method for automated analysis of algal pigments by HPLC

    NARCIS (Netherlands)

    van Leeuwe, M. A.; Villerius, L. A.; Roggeveld, J.; Visser, R. J. W.; Stefels, J.

    2006-01-01

    A recent development in algal pigment analysis by high-performance liquid chromatography (HPLC) is the application of automation. An optimization of a complete sampling and analysis protocol applied specifically in automation has not yet been performed. In this paper we show that automation can only

  1. Melanin determination by high performance liquid chromatography (HPLC) for K. marxianus

    Science.gov (United States)

    Ultraviolet light (UV) mutated K. marxianus was found to turn dark brown during a growth assay. This brown color was hypothesized to be melanin overproduction influenced by the UV exposure. Cell cultures were oxidized and HPLC analyzed to determine melanin concentrations. The resulting melanin con...

  2. Simultaneous analysis of 17 diuretics in dietary supplements by HPLC and LC-MS/MS.

    Science.gov (United States)

    Woo, H; Kim, J W; Han, K M; Lee, J H; Hwang, I S; Lee, J H; Kim, J; Kweon, S J; Cho, S; Chae, K R; Han, S Y; Kim, J

    2013-01-01

    In order to test health foods for illegally added diuretics for weight loss, we developed simple, rapid, selective, and sensitive methods using HPLC and LC-MS/MS for the simultaneous analysis of 17 diuretics in dietary supplements. HPLC conditions were set with a Capcell-pak C18, using a mobile phase consisting of gradient conditions, UV detection at 254 nm and validated for linearity (r(2)> 0.999), precision (CV ≤ 3%), recoveries (90.4-102.8%) and reproducibility. Identification and quantification of 17 diuretics were accomplished by ion-spray LC-MS/MS using multiple reaction monitoring (MRM). The chromatographic separation was carried out under the reversed-phase mechanism on an HSS-T3 column. The LC-MS/MS method was validated for linearity (r(2)> 0.99) and precision (CV Diuretics were not detected in all samples. Extraction recovery was also investigated and the extraction recoveries in different formulations were from 88% to 110% and from 81% to 116% using HPLC and LC-MS/MS, respectively. There was no significant difference in recoveries in the type of dietary supplements. Based on this result, the developed methods to monitor illegal drug adulterations in dietary supplements using HPLC and LC-MS/MS are simple, fast and reliable. Therefore, it is applicable to routine drug-adulteration screening.

  3. Recent developments in HPLC analysis of β-blockers in biological samples.

    Science.gov (United States)

    Saleem, Kishwar; Ali, Imran; Kulsum, Umma; Aboul-Enein, Hassan Y

    2013-09-01

    β-Adrenergic blockers represent a very important class of drugs that are used worldwide for treating various cardiac diseases. The present article describes the state-of-the art of analyses of β-adrenergic blockers using high-performance liquid chromatography (HPLC). Sample preparation techniques such as liquid-liquid extraction, solid-phase extraction and solid-phase microextraction have been discussed, which are essential prior to HPLC analysis. Additionally, applications of liquid chromatography coupled with tandem mass spectrometry are included. HPLC methods have been reported to include 0.6-26 min as the run times and 0.01 ng/mL to 25 µg/mL as detection limits. The most commonly used columns were C18 with various buffers as the mobile phases, along with various organic modifiers. The optimization of HPLC conditions has been discussed. It has been observed that the reported methods are quite satisfactory for the analyses of β-adrenergic blockers in biological samples. Future perspectives in the hyphenation of solid-phase microextraction-nano-liquid chromatography-tandem mass spectrometry have also been highlighted to achieve detections at nanogram and picogram levels. The present article is very useful for academicians, scientists, drug and pharmaceutical personnel and government regulatory authorities.

  4. 2D-HPLC and MALDI-TOF/TOF analysis of barley proteins glycated during brewing

    Czech Academy of Sciences Publication Activity Database

    Petry-Podgorska, Inga; Žídková, Jitka; Flodrová, Dana; Bobálová, Janette

    2010-01-01

    Roč. 878, č. 30 (2010), s. 3143-3148 ISSN 1570-0232 R&D Projects: GA MŠk 1M0570 Institutional research plan: CEZ:AV0Z40310501 Keywords : 2D-HPLC * MALDI-TOF/TOF mass spectrometry * barley Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.971, year: 2010

  5. Determination of epirubicin and its metabolite epirubicinol in saliva and plasma by HPLC

    NARCIS (Netherlands)

    Dodde, WIW; Maring, JG; Hendriks, G; Wachters, FM; Groen, HJM; de Vries, EGE; Uges, DRA

    We present a high-performance liquid chromatography (HPLC) method suitable for the analysis of epirubicin and its metabolite epirubicinol in saliva and plasma. Preparation of saliva and plasma samples was performed by extraction of analytes with a chloroform: 2-propanol mixture (6:1, vol/vol) and

  6. Determination of organic acids evolution during apple cider fermentation using an improved HPLC analysis method

    NARCIS (Netherlands)

    Zhang, H.; Zhou, F.; Ji, B.; Nout, M.J.R.; Fang, Q.; Zhang, Z.

    2008-01-01

    An efficient method for analyzing ten organic acids in food, namely citric, pyruvic, malic, lactic, succinic, formic, acetic, adipic, propionic and butyric acids, using HPLC was developed. Boric acid was added into the mobile phase to separate lactic and succinic acids, and a post-column buffer

  7. Screening natural antioxidants in peanut shell using DPPH-HPLC-DAD-TOF/MS methods.

    Science.gov (United States)

    Qiu, Jiying; Chen, Leilei; Zhu, Qingjun; Wang, Daijie; Wang, Wenliang; Sun, Xin; Liu, Xiaoyong; Du, Fangling

    2012-12-15

    Peanut shell, a byproduct in oil production, is rich in natural antioxidants. Here, a rapid and efficient method using DPPH-HPLC-DAD-TOF/MS was used for the first time to screen antioxidants in peanut shell. The method is based on the hypothesis that upon reaction with 1, 1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced or disappeared, and the identity confirmation could be achieved by HPLC-DAD-TOF/MS technique. With this method, three compounds possessing potential antioxidant activities were found abundantly in the methanolic extract of peanut shell. They were identified as 5,7-dihydroxychromone, eriodictyol, and luteolin. The contents of these compounds were 0.59, 0.92, and 2.36 mg/g, respectively, and luteolin possessed the strongest radical scavenging capacity. DPPH-HPLC-DAD-TOF/MS assay facilitated rapid identification and determination of natural antioxidants in peanut shell, which may be helpful for value-added utilization of peanut processing byproducts. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Simultaneous HPLC quantitative analysis of mangostin derivatives in Tetragonula pagdeni propolis extracts

    Directory of Open Access Journals (Sweden)

    Sumet Kongkiatpaiboon

    2016-04-01

    Full Text Available Propolis has been used as indigenous medicine for curing numerous maladies. The one that is of ethnopharmacological use is stingless bee propolis from Tetragonula pagdeni. A simultaneous high-performance liquid chromatography (HPLC investigation was developed and validated to determine the contents of bioactive compounds: 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin. HPLC analysis was effectively performed using a Hypersil BDS C18 column, with the gradient elution of methanol–0.2% formic acid and a flow rate of 1 ml/min, at 25 °C and detected at 245 nm. Parameters for the validation included accuracy, precision, linearity, and limits of quantitation and detection. The developed HPLC technique was precise, with lower than 2% relative standard deviation. The recovery values of 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin in the extracts were 99.98%, 99.97%, 98.98% and 99.19%, respectively. The average contents of these mixtures in the propolis extracts collected from different seasons were 0.127%, 1.008%, 0.323% and 2.703% (w/w, respectively. The developed HPLC technique was suitable and practical for the simultaneous analysis of these mangostin derivatives in T. pagdeni propolis and would be a valuable guidance for the standardization of its pharmaceutical products.

  9. HPLC-photodiode array detection analysis of curcuminoids in Curcuma species indigenous to Indonesia

    NARCIS (Netherlands)

    Bos, Rein; Windono, Tri; Woerdenbag, Herman J.; Boersma, Ykelien L.; Koulman, Albert; Kayser, Oliver

    An optimized HPLC method with photodiode array detection was developed and applied to analyse the curcuminoids curcumin, demethoxycurcumin, and bis-demethoxycurcumin in rhizomes of Curcuma mangga Val &. v. Zijp, C. heyneana Val. & v. Zijp, C. aeruginosa Roxb. and C. soloensis Val. (Zingiberaceae),

  10. Determination of acetylsalicylic acid and salicylic acid in foods, using HPLC with fluorescence detection.

    NARCIS (Netherlands)

    Venema, D.P.; Hollman, P.C.H.; Janssen, P.L.T.M.K.; Katan, M.B.

    1996-01-01

    We developed a specific and sensitive HPLC method with fluorescence detection for the determination of free acetylsalicylic acid, free salicylic acid, and free salicylic acid plus salicylic acid after alkaline hydrolysis (free-plus-bound) in foods. Acetylsalicylic acid was detected after postcolumn

  11. Application of HPLC capacity coefficients to characterize the sorption of polycyclic aromatic compounds to humic acid

    DEFF Research Database (Denmark)

    Nielsen, T.; Helweg, C.; Siigur, K.

    1997-01-01

    The sorption coefficients to humic acid of 46 PAC having a wide range in polarity were compared with the capacity coefficients of the PAC to a non-polar HPLC column material (ODS) and a polar one (Diol). It is shown that polar interactions contribute to the sorption of polar PAC in addition...

  12. Determination of Trace Level Triclosan in Water by Online Preconcentration and HPLC-UV Diode Array

    Science.gov (United States)

    An online high performance liquid chromatography (HPLC) method for the detection and quantification of trace levels of triclosan in water is discussed. Triclosan, an anti-bacterial agent, and related compounds have been shown to reach municipal waste waters through the disposal ...

  13. Time-resolved SAXS measurements facilitated by online HPLC buffer exchange

    DEFF Research Database (Denmark)

    Jensen, Malene Hillerup; Toft, Katrine Nørgaard; David, Gabriel

    2010-01-01

    continuous or stopped flow. In this paper a method for obtaining TR-SAXS data from systems where the reaction is triggered by removal of a species is presented. This method is based on fast buffer exchange over a short desalting column facilitated by an online HPLC (high-performance liquid chromatography...

  14. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    International Nuclear Information System (INIS)

    Karasawa, Koji; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-01-01

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H_2O_2 and O_2"− generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  15. SEPARATION OF OCTYLPHENOL POLYETHER ALCOHOLS SURFACTANTS BY CAPILLARY COLUMN SFC AND HPLC

    Science.gov (United States)

    Separation of nonionic octylphenol polyether alcohols (OPA) by supercritical fluid chromatography (SFC) and HPLC is described. Using a density programming and a 50-μm i.d. capillary column, a total of 18 group oligomers was separated. The effects of the operating parameters, such...

  16. An introduction of HPLC to check contamination in the adsorption of uranium from sea water

    International Nuclear Information System (INIS)

    Takai, Nobuharu; Senoo, Manabu; Sugasaka, Kazuhiko; Katoh, Shunsaku; Ouchi, Hideyoshi; Itagaki, Takaharu.

    1984-01-01

    Seawater contains many inorganic ions and many organic substances, and they are adsorbed by adsorbents as well as uranium, and some of which are released into solution when desorbed. An examination was carried out on the substances contained in desorption solution using HPLC to confirm the desorption behavior of contaminants. The instruments used for the test were Hitachi HPLC Model 638 and the prototype spectrophotometer with 32 wave lengths, and the signals from the spectrophotometer are transmitted to a microcomputer through I/O. The test was carried out at National Industrial Institute of Shikoku using the desorption solution obtained from the composite adsorbent of carbon titanium and amidoxime resin by the treatment with acid and alkali. As preliminary test, desorption behavior was detected with the HPLC on the samples of various desorption solutions with a detector of fixed wave length at various wave lengths. Another test was carried out using the prototype with 32 wave lengths to check the function of the system. Desorption solution was tested with the HPLC with the detector of multi-wave lengths. From the experimental results, it was found that the contaminants contained in acid desorption solution were largely different from those contained in sodium carbonate desorption solution. (Yoshitake, I.)

  17. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

  18. Analysis of several irdoid and indole precursors of terpenoid indole alkaloids with a single HPLC run

    DEFF Research Database (Denmark)

    Dagnino, Denise; Schripsema, Jan; Verpoorte, Robert

    1996-01-01

    An isocratic HPLC system is described which allows the separation of the iridoid and indole precursors of terpenoid indole alkaloids, which are present in a single crude extract. The system consists of a column of LiChrospher 60 RP select B 5 my, 250x4 mm (Merck) with an eluent of 1 % formic acid...

  19. A first step towards miniaturized HPLC systems in analytical routine laboratories

    NARCIS (Netherlands)

    Straten, van M.A.; Vermeer, E.A.; Claessens, H.A.

    1996-01-01

    This article shows that the first step towards the miniaturization of HPLC systems can be made without any, or only slight, modification to conventional equipment. Minor (less expensive) equipment modifications, particularly the use of micro-detector cells, allow the routine use of 3.2- and 2.1-mm

  20. Using HPLC-Mass Spectrometry to Teach Proteomics Concepts with Problem-Based Techniques

    Science.gov (United States)

    Short, Michael; Short, Anne; Vankempen, Rachel; Seymour, Michael; Burnatowska-Hledin, Maria

    2010-01-01

    Practical instruction of proteomics concepts was provided using high-performance liquid chromatography coupled with a mass selective detection system (HPLC-MS) for the analysis of simulated protein digests. The samples were prepared from selected dipeptides in order to facilitate the mass spectral identification. As part of the prelaboratory…

  1. Discrimination of Polish unifloral honeys using overall PTR-MS and HPLC fingerprints combined with chemometrics

    NARCIS (Netherlands)

    Kus, P.M.; Ruth, van S.M.

    2015-01-01

    A total of 62 honey samples of six floral origins (rapeseed, lime, heather, cornflower, buckwheat and black locust) were analysed by means of proton transfer reaction mass spectrometry (PTR-MS) and HPLC-DAD. The data were evaluated by principal component analysis and k-nearest neighbours

  2. Fluorescence detection of flavonols in HPLC by postcolumn chelation with aluminum

    NARCIS (Netherlands)

    Hollman, Peter C H; Van Trijp, J. M P; Buysman, Michel N C P

    1996-01-01

    Flavonols are dietary antioxidants which may prevent coronary heart disease. To be able to study absorption of flavonols in humans, we developed a postcolumn derivatization with aluminum for HPLC with fluorescence detection. Variables governing postcolumn chelation, such as water content, buffer,

  3. Comparison of calorimetric and HPLC methods in measuring nitrate content of meat products: An economic evaluation

    Directory of Open Access Journals (Sweden)

    M moradi

    2014-02-01

    Full Text Available Nitrate is a flavors compound, color stabilizer and growth inhibitor of anaerobic microorganisms in meat products. High concentration of nitrate in food can cause methaemoglobinaemia and is recognized as carcinogenic. Therefore, accurate determination of nitrate is crucial to ensure consumers’ health. Regularly, nitrate is estimated by colorimetric and HPLC methods. In measurement of nitrate, the efficiency, accuracy, speed and amount of material are important from economical point of view. In this study, the cost of initial investment, staff, consumable material and equipments used by the two methods were calculated and finally Net Present Value (NPV was estimated for each of them. The rate of interest was considered from 4 until 30%. According to the results the amount of initial investment, annual cost of staff and consumable materials for colorimetric method were determined as 274000000, 379080000 and 214289130 Rials, respectively. These costs for HPLC method were 342000000, 252720000 and 7633080 Rials, respectively. NPV in minimum and maximum rates of interest (4 and 30% for colorimetric method were 8368344000 and 2242330000 Rials and for HPLC method were estimated at 4035848000 and 1207544000 Rials. As a consequence, HPLC is more economical and could be recommended for the routine measurement of nitrate in of food safety laboratories.

  4. Uncertainty budget for final assay of a pharmaceutical product based on RP-HPLC

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Anglov, Thomas; Byrialsen, Kirsten

    2003-01-01

    ). The reported example illustrates the estimation of uncertainty for the final determination of a protein concentration by HPLC using UV detection, using the approach described by EURACHEM/CITAC. The combined standard uncertainty for a protein concentration of 2400 mumol/L was estimated to be 14 mumol/L. All...

  5. Determination of Trace Elements in Uranium by HPLC-ID-ICP-MS: NTNFC Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Manard, Benjamin Thomas [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Wylie, Ernest Miller II [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Xu, Ning [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tandon, Lav [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-10-19

    This report covers the FY 16 effort for the HPLC-ID-ICP-MS methodology 1) sub-method validation for the group I&II elements, 2) sub-method stood-up and validation for REE, 3) sub-method development for the transition element, and 4) completion of a comprehensive SOP for three families of elements.

  6. Determination of the sugar content in fruit flavoured drinks by HPLC ...

    African Journals Online (AJOL)

    The remaining 3 fruit flavoured drinks indicated the presence of glucose and sucrose only. The sugar content of some of the drinks calls for caution in children's diet especially with the rise in obesity and dental erosion in tooth enamel associated with sugar sweetened beverages or drinks. Keywords: HPLC; Fruit drinks, ...

  7. Morphology of a Wetland Stream

    Science.gov (United States)

    Jurmu; Andrle

    1997-11-01

    / Little attention has been paid to wetland stream morphology in the geomorphological and environmental literature, and in the recently expanding wetland reconstruction field, stream design has been based primarily on stream morphologies typical of nonwetland alluvial environments. Field investigation of a wetland reach of Roaring Brook, Stafford, Connecticut, USA, revealed several significant differences between the morphology of this stream and the typical morphology of nonwetland alluvial streams. Six morphological features of the study reach were examined: bankfull flow, meanders, pools and riffles, thalweg location, straight reaches, and cross-sectional shape. It was found that bankfull flow definitions originating from streams in nonwetland environments did not apply. Unusual features observed in the wetland reach include tight bends and a large axial wavelength to width ratio. A lengthy straight reach exists that exceeds what is typically found in nonwetland alluvial streams. The lack of convex bank point bars in the bends, a greater channel width at riffle locations, an unusual thalweg location, and small form ratios (a deep and narrow channel) were also differences identified. Further study is needed on wetland streams of various regions to determine if differences in morphology between alluvial and wetland environments can be applied in order to improve future designs of wetland channels.KEY WORDS: Stream morphology; Wetland restoration; Wetland creation; Bankfull; Pools and riffles; Meanders; Thalweg

  8. Killer whale morphology - Variation in morphology of killer whale ecotypes

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — We are using elliptic Fourier analysis to determine the patterns of variation in morphology of dorsal fin shape, saddle patch shape, and eye patch shape of resident,...

  9. Profiling of Centella asiatica (L.) urban extract

    International Nuclear Information System (INIS)

    Zainol, N.A.; Voo, S.C.; Sarmidi, M.R.; Aziz, R.A.

    2008-01-01

    Centella Asiatica is one of those phyto chemical that has been consume for hundreds years and it is claimed that the plant possess various healing effect and antioxidant properties. For many years, a lot of commercial and medicinal researches have been focusing their resources on this plant. Hence, the profiling of this plant is vital. This study was done to investigate the behaviour of active components in two different accessions commercially grown in Johore Bahru. Research procedures were carried out according to the modified method utilizing TLC and HPLC analysis method. The findings suggested that in different parts of Centella Asiatica contain different amount of phytochemicals. The highest concentration of phytochemicals was found in the second accession that was asiaticoside (2.56 μg/ ml), madecasoside (5.30 μg/ ml) and asiatic acids (3421.60 μg/ ml). Leaves contain a higher concentration of those phytochemicals relative to the petioles and the roots. (author)

  10. Evaluation of processing effects on anthocyanin content and colour modifications of blueberry (Vaccinium spp.) extracts: Comparison between HPLC-DAD and CIELAB analyses.

    Science.gov (United States)

    Cesa, Stefania; Carradori, Simone; Bellagamba, Giuseppe; Locatelli, Marcello; Casadei, Maria Antonietta; Masci, Alessandra; Paolicelli, Patrizia

    2017-10-01

    Colour is the first organoleptic property that consumers appreciate of a foodstuff. In blueberry (Vaccinium spp.) fruits, the anthocyanins are the principal pigments determining the colour as well as many of the beneficial effects attributed to this functional food. Commercial blueberry-derived products represent important sources of these healthy molecules all year round. In this study, blueberries were produced into purees comparing two homogenization methods and further heated following different thermal treatments. All the supernatants of the homogenates were monitored for pH. Then, the hydroalcoholic extracts of the same samples were characterized by CIELAB and HPLC-DAD analyses. These analytical techniques provide complementary information on fruit pigments content as a whole and on quali-quantitative profile of the single bioactive colorants. These data could be very interesting to know the best manufacturing procedure to prepare blueberry-derived products, well accepted by the consumers, while maintaining their healthy properties unaltered. Copyright © 2017. Published by Elsevier Ltd.

  11. Alkaloid and polyphenol analysis by HPLC in green and black tea powders and their potential use as additives in ruminant diets

    Science.gov (United States)

    Ramdani, Diky; Chaudhry, Abdul S.; Seal, Chris J.

    2018-02-01

    We used HPLC to examine the bioactive compounds such as alkaloids and polyphenols in green and black tea powders and their use as potential additives in ruminant diets. Caffeine was the highest alkaloid in both green and black teas. Green tea had significantly higher concentrations of alkaloids and catechins but lower theaflavins than black tea. Epigallocatechin gallate, epicatechin gallate and epigallocatechin were the major catechins in green tea while theaflavin-3, 3'-digallate and theaflavin-3-gallate were the major theaflavins in black tea. Tea powders in ruminant diets decreased in vitro rumen ammonia and methane production without affecting volatile fatty acid profiles and the degradability of the diets. The tea powders containing variable amounts of alkaloids, catechins and theaflavins can potentially be used to decrease rumen ammonia and methane productions without any detrimental effect on rumen functions in vitro and perhaps ruminant productive efficiency.

  12. [Pharmacokinetics of (-)-clausenamide and its major metabolite 6-hydroxyl-clausenamide in beagle dogs by HPLC/MS].

    Science.gov (United States)

    Song, Min; Qian, Wen; Hang, Tai-Jun; Zhang, Zheng-Xing

    2005-10-01

    To establish a sensitive and accurate method to study the pharmacokinetics of (-)-clausenamide [(-)-clau] and its major metabolite 6-hydroxyl-clausenamide (6-OH-clau) in the plasma of the Beagle dog. (-)-Clau was orally administered to six Beagle dogs at the dose of 30 mg x kg(-1), venous blood from front leg was sampled and plasma was separated for analysis. After extraction with ethyl acetate, the plasma samples were analyzed by HPLC/MS and the mobile phase was a mixture of methanol-water-acetic acid (60: 40: 0. 8) at the flow rate of 1.0 mL x min(-1). The API-ES positive ion SIM detection was carried out for the detection of both (-)-clau ([M + H] (+), m/z 298 ) and 6-OH-clau ([M + H - H2 O](+), m/z 296) with glipzide (glip) ([M + H](+), m/z 446) as internal standard. The pharmacokinetic parameters were calculated by 3P97 software. There was good linear relationship ( r > 0. 999) between the SIM responses and the concentrations for (-)-clau and 6-OH-clau at the range from 1.0 to 200 ng x mL(-1) and 0.2 to 40.0 ng x mL(-1), respectively. The absolute recovery was greater than 85%. The plasma concentration-time curves of (-)-clau and 6-OH-clau were both best fitted to a two-compartment model. The C(max) of (-)-clau and 6-OH-clau were (21 +/- 10) ng x mL(-1) and (3.9 +/- 2.2) ng x mL(-1), T(max) were (0.8 +/- 0.5) h and (1.3 +/- 0.5) h, T 1/2 alpha were (0.9 +/- 0.6) hand (1.4 +/- 0.6) h, T 1/2 beta were (19 +/- 23) hand (13 +/- 12) h, AUC(0-24 h) were (69 +/- 14) h x ng x mL(-1) and (12 +/- 7) h x ng x mL(-1) respectively. The established HPLC/MS method was sensitive and specific for the determination of (-)-clau. It was shown that the absorption and first phase elimination of (-)-clau were very quick in Beagle dogs, but the terminal elimination was very slow. The plasma concentration profile of its major metabolite 6-OH-clau was similar to (-)-clau and the AUC was relatively small in comparison with (-)-clau.

  13. Activity behavior of a HPLC column including α-chymotrypsin immobilized monosized-porous particles

    International Nuclear Information System (INIS)

    Bilici, Z.; Camli, S.T.; Unsal, E.; Tuncel, A.

    2004-01-01

    In this study, a polymer-based, α-chymotrypsin (CT) immobilized HPLC column was prepared as a potential material for affinity-HPLC and chiral separation applications. Monosized-macroporous particles were synthesized as the support material by a relatively new polymerization protocol, the so-called, 'modified seeded polymerization'. The particles were obtained in the form of styrene-glycidyl methacrylate- divinylbenzene terpolymer approximately 11 μm in size. The particles were treated with aqueous ammonia to have primary amine groups on the porous surface. The amine functionalized particles were reacted by glutaraldehyde and the enzyme, CT, was covalently attached. CT carrying monosized-porous particles were slurry packed into the HPLC column 50 mmx4.6 mm in size. Since the activity behavior of immobilized CT played an important role in the enantiomeric separations performed by similar columns, the enzymatic activity behavior of the column produced by our protocol was determined. For this purpose, HPLC column was used as a packed bed reactor and the enzymatic reaction was continuously followed by measuring the absorbance of the output flow by the UV-detector of HPLC. S-shaped absorbance-time curves were obtained by monitoring the reactor output both in dynamic and steady-state periods. The columns with relatively lower immobilized enzyme content were more sensitive to the changes in the operating conditions and responded with more appreciable substrate conversion changes. The maximum reaction rate of the immobilized enzyme was estimated as approximately 25% of the free one by the mathematical model describing the activity behavior of the column. No significant loss was observed in the activity of the immobilized enzyme during the course of the experiments

  14. Determination of Bortezomib in API Samples Using HPLC: Assessment of Enantiomeric and Diastereomeric Impurities.

    Science.gov (United States)

    Kamalzadeh, Zahra; Babanezhad, Esmaeil; Ghaffari, Solmaz; Mohseni Ezhiyeh, Alireza; Mohammadnejad, Mahdieh; Naghibfar, Mehdi; Bararjanian, Morteza; Attar, Hossein

    2017-08-01

    A new, normal phase high performance liquid chromatography (NP-HPLC) method was developed for separation of Bortezomib (BZB) enantiomers and quantitative determination of (1S,2R)-enantiomer of BZB in active pharmaceutical ingredient (API) samples. The developed method was validated based on International Conference on Harmonisation (ICH) guidelines and it was proved to be accurate, precise and robust. The obtained resolution (RS) between the enantiomers was more than 2. The calibration curve for (1S,2R)-enantiomer was found to be linear in the concentration range of 0.24-5.36 mg/L with regression coefficient (R2) of 0.9998. Additionally, the limit of detection (LOD) and limit of quantification (LOQ) were 0.052 and 0.16 mg/L, respectively. Also, in this study, a precise, sensitive and robust gradient reversed-phase HPLC (RP-HPLC) method was developed and validated for determination of BZB in API samples. The detector response was linear over the concentration range of 0.26-1110.5 mg/L. The values of R2, LOD and LOQ were 0.9999, 0.084 and 0.25 mg/L, respectively. For both NP-HPLC and RP-HPLC methods, all of the RSD (%) values obtained in the precision study were 2,000 and RS > 2.0. The performance of two common integration methods of valley to valley and drop perpendicular for drawing the baseline between two adjacent peaks were investigated for the determination of diastereomeric impurity (Imp-D) in the BZB-API samples. The results showed that the valley to valley method outperform the drop perpendicular method for calculation of Imp-D peak areas. Therefore, valley to valley method was chosen for peak integration. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. Morphology and Structures of Nearby Dwarf Galaxies

    Science.gov (United States)

    Seo, Mira; Ann, HongBae

    2015-08-01

    We performed an analysis of the structure of nearby dwarf galaxies based on a 2-dimensional decomposition of galaxy images using GALFIT. The present sample consists of ~1,100 dwarf galaxies with redshift less than z = 0.01, which is is derived from the morphology catalog of the Visually classified galaxies in the local universe (Ann, Seo, and Ha 2015). In this catalog, dwarf galaxies are divided into 5 subtypes: dS0, dE, dSph, dEbc, dEblue with distinction of the presence of nucleation in dE, dSph, and dS0. We found that dSph and dEblue galaxies are fainter than other subtypes of dwarf galaxies. In most cases, single component, represented by the Sersic profile with n=1~1.5, well describes the luminosity distribution of dwarf galaxies in the present sample. However, a significant fraction of dS0, dEbc, and dEbue galaxies show sub-structures such as spiral arms and rings. We will discuss the morphology dependent evolutionary history of the local dwarf galaxies.

  16. Dendritic surface morphology of palladium hydride produced by electrolytic deposition

    International Nuclear Information System (INIS)

    Julin, Peng; Bursill, L.A.

    1990-01-01

    Conventional and high-resolution electron microscopic studies of electrolytically-deposited palladium hydride reveal a fascinating variety of surface profile morphologies. The observations provide direct information concerning the surface structure of palladium electrodes and the mechanism of electrolytic deposition of palladium black. Both classical electrochemical mechanisms and recent 'modified diffusion-limited-aggregation' computer simulations are discussed in comparison with the experimental results. 13 refs., 9 figs

  17. [The 40th anniversary of RAMS institute of human morphology].

    Science.gov (United States)

    Kakturskiĭ, L V; Shakhlamov, V A

    2002-01-01

    Institute of Human Morphology of Russian Academy of Medical Sciences was established in 1961 and united efforts of morphologists of various profile--pathologists, cytologists, embryologists. The role of outstanding Russian morphologists and the first Institute heads is shown. Basic achievements in four research fields are characterized: in geographic pathology; structural basis of immune homeostasis in health and pathology; pathologic anatomy and pathogenesis of basic human diseases; human morpho- and embriogenesis in health and disease.

  18. Profile: Asian Americans

    Science.gov (United States)

    ... and Data > Minority Population Profiles > Asian American Profile: Asian Americans Asian American Profile (Map of the US with the top 10 states displaying the largest Asian American population according to the Census Bureau) CA - ...

  19. Online extraction-high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry for rapid flavonoid profiling of Fructus aurantii immaturus.

    Science.gov (United States)

    Tong, Runna; Peng, Mijun; Tong, Chaoying; Guo, Keke; Shi, Shuyun

    2018-03-01

    Chemical profiling of natural products by high performance liquid chromatography (HPLC) was critical for understanding of their clinical bioactivities, and sample pretreatment steps have been considered as a bottleneck for analysis. Currently, concerted efforts have been made to develop sample pretreatment methods with high efficiency, low solvent and time consumptions. Here, a simple and efficient online extraction (OLE) strategy coupled with HPLC-diode array detector-quadrupole time-of-flight tandem mass spectrometry (HPLC-DAD-QTOF-MS/MS) was developed for rapid chemical profiling. For OLE strategy, guard column inserted with ground sample (2 mg) instead of sample loop was connected with manual injection valve, in which components were directly extracted and transferred to HPLC-DAD-QTOF-MS/MS system only by mobile phase without any extra time, solvent, instrument and operation. By comparison with offline heat-reflux extraction for Fructus aurantii immaturus (Zhishi), OLE strategy presented higher extraction efficiency perhaps because of the high pressure and gradient elution mode. A total of eighteen flavonoids were detected according to their retention times, UV spectra, exact mass, and fragmentation ions in MS/MS spectra, and compound 9, natsudaidain-3-O-glucoside, was discovered in Zhishi for the first time. It is concluded that the developed OLE-HPLC-DAD-QTOF-MS/MS system offers new perspectives for rapid chemical profiling of natural products. Copyright © 2018. Published by Elsevier B.V.

  20. The chemotaxonomic classification of Rhodiola plants and its correlation with morphological characteristics and genetic taxonomy.

    Science.gov (United States)

    Liu, Zhenli; Liu, Yuanyan; Liu, Chunsheng; Song, Zhiqian; Li, Qing; Zha, Qinglin; Lu, Cheng; Wang, Chun; Ning, Zhangchi; Zhang, Yuxin; Tian, Cheng; Lu, Aiping

    2013-07-12

    Rhodiola plants are used as a natural remedy in the western world and as a traditional herbal medicine in China, and are valued for their ability to enhance human resistance to stress or fatigue and to promote longevity. Due to the morphological similarities among different species, the identification of the genus remains somewhat controversial, which may affect their safety and effectiveness in clinical use. In this paper, 47 Rhodiola samples of seven species were collected from thirteen local provinces of China. They were identified by their morphological characteristics and genetic and phytochemical taxonomies. Eight bioactive chemotaxonomic markers from four chemical classes (phenylpropanoids, phenylethanol derivatives, flavonoids and phenolic acids) were determined to evaluate and distinguish the chemotaxonomy of Rhodiola samples using an HPLC-DAD/UV method. Hierarchical cluster analysis (HCA) and principal component analysis (PCA) were applied to compare the two classification methods between genetic and phytochemical taxonomy. The established chemotaxonomic classification could be effectively used for Rhodiola species identification.

  1. Estimation of the limit of detection with a bootstrap-derived standard error by a partly non-parametric approach. Application to HPLC drug assays

    DEFF Research Database (Denmark)

    Linnet, Kristian

    2005-01-01

    Bootstrap, HPLC, limit of blank, limit of detection, non-parametric statistics, type I and II errors......Bootstrap, HPLC, limit of blank, limit of detection, non-parametric statistics, type I and II errors...

  2. Determination of 9 Carcinogenic Dyes by HPLC-DAD%HPLC-DAD法检测染料产品中9种致癌染料

    Institute of Scientific and Technical Information of China (English)

    吕双; 季浩; 蒲爱军; 王勇

    2016-01-01

    本文建立了测定染料产品中9种致癌染料的高效液相色谱-二极管阵列检测器分析方法(HPLC-DAD).各类染料经溶解或萃取后,通过Symmetry Shield RP-18色谱柱分离后进入DAD检测器,采用外标法对9种致癌染料进行定性和定量分析.

  3. Morphologic Subtypes of Hepatocellular Carcinoma.

    Science.gov (United States)

    Torbenson, Michael S

    2017-06-01

    Hepatocellular carcinomas can be further divided into distinct subtypes that provide important clinical information and biological insights. These subtypes are distinct from growth patterns and are on based on morphologic and molecular findings. There are 12 reasonably well-defined subtypes as well as 6 provisional subtypes, together making up 35% of all hepatocellular carcinomas. These subtypes are discussed, with an emphasis on their definitions and the key morphologic findings. Copyright © 2017 Elsevier Inc. All rights reserved.

  4. Mitochondrial morphology and cardiovascular disease

    OpenAIRE

    Ong, Sang-Bing; Hausenloy, Derek J.

    2010-01-01

    Mitochondria are dynamic and are able to interchange their morphology between elongated interconnected mitochondrial networks and a fragmented disconnected arrangement by the processes of mitochondrial fusion and fission, respectively. Changes in mitochondrial morphology are regulated by the mitochondrial fusion proteins (mitofusins 1 and 2, and optic atrophy 1) and the mitochondrial fission proteins (dynamin-related peptide 1 and mitochondrial fission protein 1) and have been implicated in a...

  5. Analysis of Wheat Prolamins, the Causative Agents of Celiac Sprue, Using Reversed Phase High Performance Liquid Chromatography (RP-HPLC and Matrix-Assisted Laser Desorption Ionization Time of Flight Mass Spectrometry (MALDI-TOF-MS

    Directory of Open Access Journals (Sweden)

    Jaime H. Mejías

    2014-04-01

    Full Text Available Wheat prolamins, commonly known as “gluten”, are a complex mixture of 71–78 proteins, which constitute ~80% of the proteins in the wheat grains and supply 50% of the global dietary protein demand. Prolamins are also responsible for numerous gluten-induced disorders and determine the unique visco-elastic properties of the wheat dough. These properties necessitate the reliable determination of the prolamin composition in wheat grains and their derived products. Therefore, this study examined the impact of HPLC conditions, including column type, column temperature, flow rate, and the gradient of polar and non-polar solvents in the mobile phase, to improve the analytical resolution of prolamins. The following conditions were found optimal for analyses: column temperature 60 °C, flow rate 1.0 mL/min and an elution gradient of 20%–60% of 0.1% trifluoroacetic acid + acetonitrile in 60 min. For further improvement of resolution, gliadin and glutenin extracts were analyzed using MALDI-TOF-MS in combination with HPLC fractionation. Two semi-quantitative methods, densitometry of stained polyacrylamide gels and HPLC, were used to determine relative prolamin quantities and the correspondence between the methods was established. The combinatorial gluten analyses approach developed during the present study was used to analyze prolamin profiles of wheat transformants expressing DEMETER silencing artificial microRNA, and the results are discussed.

  6. Sella turcica morphology and the pituitary gland--a new contribution to craniofacial diagnostics based on histology and neuroradiology

    DEFF Research Database (Denmark)

    Kjær, Inger

    2012-01-01

    histological analyses of human prenatal material and profile radiographic analyses of human postnatal material, supplemented in a few cases with neuroradiology. Prenatal and postnatal results are compared. Similarities between prenatal and postnatal deviations in sella turcica morphology were demonstrated...

  7. The parachute morphology as equilibrium morphology of vesicle-polymer hybrids?

    NARCIS (Netherlands)

    Jung, M.; Hubert, D.H.W.; Herk, van A.M.; German, A.L.

    2000-01-01

    Polymerisation in vesicles leads to novel polymer colloid morphologies. Two morphologies are currently reported: the triple-shell and the parachute morphology. The termodynamic analysis of these two morphologies, presented here, stresses the importance of considering interfacial energies between

  8. Study of HPLC/ICP-MS coupling for the As speciation; Estudo de um acoplamento de HPLC/ICP-MS para a especiacao do As

    Energy Technology Data Exchange (ETDEWEB)

    Cortez, Bruna C.G.; Oliveira, Arno Heeren de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: brunacortez2004@yahoo.com.br; heeren@nuclear.ufmg.br

    2005-07-01

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (As{sup III}) is more toxic than arsenate (As{sup V}). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  9. Quality Evaluation and Chemical Markers Screening of Salvia miltiorrhiza Bge. (Danshen Based on HPLC Fingerprints and HPLC-MSn Coupled with Chemometrics

    Directory of Open Access Journals (Sweden)

    Wenyi Liang

    2017-03-01

    Full Text Available Danshen, the dried root of Salvia miltiorrhiza Bge., is a widely used commercially available herbal drug, and unstable quality of different samples is a current issue. This study focused on a comprehensive and systematic method combining fingerprints and chemical identification with chemometrics for discrimination and quality assessment of Danshen samples. Twenty-five samples were analyzed by HPLC-PAD and HPLC-MSn. Forty-nine components were identified and characteristic fragmentation regularities were summarized for further interpretation of bioactive components. Chemometric analysis was employed to differentiate samples and clarify the quality differences of Danshen including hierarchical cluster analysis, principal component analysis, and partial least squares discriminant analysis. Consistent results were that the samples were divided into three categories which reflected the difference in quality of Danshen samples. By analyzing the reasons for sample classification, it was revealed that the processing method had a more obvious impact on sample classification than the geographical origin, it induced the different content of bioactive compounds and finally lead to different qualities. Cryptotanshinone, trijuganone B, and 15,16-dihydrotanshinone I were screened out as markers to distinguish samples by different processing methods. The developed strategy could provide a reference for evaluation and discrimination of other traditional herbal medicines.

  10. Role of beach morphology in wave overtopping hazard assessment

    Science.gov (United States)

    Phillips, Benjamin; Brown, Jennifer; Bidlot, Jean-Raymond; Plater, Andrew

    2017-04-01

    Understanding the role of beach morphology in controlling wave overtopping volume will further minimise uncertainties in flood risk assessments at coastal locations defended by engineered structures worldwide. XBeach is used to model wave overtopping volume for a 1:200 yr joint probability distribution of waves and water levels with measured, pre- and post-storm beach profiles. The simulation with measured bathymetry is repeated with and without morphological evolution enabled during the modelled storm event. This research assesses the role of morphology in controlling wave overtopping volumes for hazardous events that meet the typical design level of coastal defence structures. Results show disabling storm-driven morphology under-represents modelled wave overtopping volumes by up to 39% under high Hs conditions, and has a greater impact on the wave overtopping rate than the variability applied within the boundary conditions due to the range of wave-water level combinations that meet the 1:200 yr joint probability criterion. Accounting for morphology in flood modelling is therefore critical for accurately predicting wave overtopping volumes and the resulting flood hazard and to assess economic losses.

  11. Analysis on Protein Profile and Amino Acid of Edible Bird's Nest (Collocalia Fuchiphaga) From Painan

    OpenAIRE

    Elfita, Lina

    2014-01-01

    This study was aimed to analyze protein profile and amino acid composition of bird nest from Painan, Pesisir Selatan Distric, West Sumatra. Protein analysis was performed by Sodium Dodecyl Sulphate Polyacrilamide Gel Electrophoresis (SDS-PAGE), meanwhile High Performance Liquid Chromatography (HPLC) was used for analysis of amino acid. Analysis on water extract of bird nest by SDS-PAGE showed six bands which correspond to molecular protein which had molecular weight of 147.2; 142.6; 133.4; 73...

  12. Amino Acid Profile as a Feasible Tool for Determination of the Authenticity of Fruit Juices

    OpenAIRE

    Mostafa Asadpoor; Masoud Ansarin; Mahboob Nemati

    2014-01-01

    Purpose: Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. Methods: The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA). Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the...

  13. HPLC assay for 2-(3-aminopropylamino)ethanethiol (WR-1065) in plasma

    International Nuclear Information System (INIS)

    McGovern, E.P.; Swynnerton, N.F.; Steele, P.D.; Mangold, D.J.

    1984-01-01

    A high pressure liquid chromatography (HPLC) plasma assay for WR-1065 is described which is both precise and accurate throughout the concentration range from 1 to 500 μg/mL of plasma. The analyte is separated by HPLC and detected with a thiol specific electrochemical transducer cell. The detector response is linear over the ranges 1 to 10 μg/mL, 10 to 100 μg/mL, and 100 to 500 μg/mL. The absolute retention times for WR-1065 and WT-1729 are 9 and 12 minutes, respectively. The assay uses 100 μL of plasma and requires a total chromatography cycle time of 40 minutes. The method has been found suitable for the determination of WR-1065 in plasma from a beagle dog after i.v. administration of S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721)

  14. Development of an HPLC post-column antioxidant assay for Solidago canadensis radical scavengers.

    Science.gov (United States)

    Marksa, Mindaugas; Radušienė, Jolita; Jakštas, Valdas; Ivanauskas, Liudas; Marksienė, Rūta

    2016-01-01

    The aim of this work was to modify and validate the post-column high-performance liquid chromatography (HPLC)-ABTS and DPPH methods for evaluating the antioxidant activity of the methanolic extracts of Solidago canadensis (Canadian goldenrod) leaves and flowers. Separation of the analytes was performed via the HPLC-PDA method on a YMC analytical column using a gradient elution program. Three compounds with antioxidant properties - chlorogenic acid, rutin and isoquercitrin - and two unidentified antioxidants were established. The research showed that the coil temperature regimes and loop length combinations influence the optimised post-column assay method for detecting the antioxidant activity of goldenrod radical scavengers. Investigations established that the temperature in the reaction coil was a substantial factor contributing to the signal strength of the analytes after reacting with the DPPH and ABTS radicals.

  15. Study of the electrooxidation of ethanol on hydrophobic electrodes by DEMS and HPLC

    International Nuclear Information System (INIS)

    Gonzalez Pereira, M.; Davila Jimenez, M.; Elizalde, M.P.; Manzo-Robledo, A.; Alonso-Vante, N.

    2004-01-01

    The electrochemical oxidation of ethanol in alkaline solution has been studied on Cu-PVC electrode and Ni/Cu-PVC composite electrodes modified by ruthenium nanoparticles. The techniques used were cyclic voltammetry (CV), steady-state potentiostatic method, on line differential electrochemical mass spectrometry (DEMS), and high-performance liquid chromatography (HPLC). The chemical products: acetaldehyde and acetic acid were detected measuring the proper mass charge (m/z) ratios. These products were also confirmed by HPLC. The surface modification of composite electrodes by ruthenium nanoparticles promotes the formation of acetaldehyde. As shown by DEMS, the surface modification shifts the onset potential for oxygen evolution reaction on the Cu-PVC composite electrode towards more anodic values

  16. Targeted natural product isolation guided by HPLC-SPE-NMR: Constituents of Hubertia species

    DEFF Research Database (Denmark)

    Sprogoe, K.; Staek, D.; Jager, A.K.

    2007-01-01

    -hydroxyphenyl)acetyl]quinic acid (3), was performed. Finally, targeted isolation of 1 was achieved by SPE fractionation and preparative HPLC, followed by evaluation of its antioxidant and antimicrobial activity. In contrast to chlorogenic acid and 3,5-di-O-caffeoylquinic acid, which act as antioxidants...... full or partial identification of all major extract constituents and demonstrated the presence of unusual quinic acid derivatives containing the (1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl residue that exhibit strongly coupled ABXY patterns, the parameters of which were obtained by spin simulations....... Using homo- and heteronuclear 2D NMR data acquired in the HPLC-SPE-NMR mode, complete structure determination of three new natural products, i.e., 3,5-di-O-caffeoyl-4-O-[(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl]quini c acid (1), its 2-hydroxy derivative (2), and 3,5-di-O-caffeoyl-4-O-[(4...

  17. Dual-mode gradient HPLC procedure for the simultaneous determination of chloroquine and proguanil.

    Science.gov (United States)

    Paci, A; Caire-Maurisier, A-M; Rieutord, A; Brion, F; Clair, P

    2002-01-01

    In order to assay the antipaludic capsule of the Service de Santé des Armées (SSA), that contains two antimalarial drugs, i.e. chloroquine sulfate (CQS, cp1) and proguanil hydrochloride (PGH, cp5), a HPLC procedure was developed. A reversed-phase ion-pair high-performance liquid chromatography (HPLC) method with an ultraviolet detection at 254 nm was set up and validated. Elution system includes programming of both organic concentration and flow-rate known as 'dual-mode gradient'. This method allows the simultaneous determination of both active compounds and separation of four process related substances. The method is simple, rapid, selective and accurate, and the precision is good with an inter- and intra-assay of <2%. The sensitivity is particularly suitable for pharmaceutical quality control.

  18. [Comparison between colorimetry and HPLC on the stability test of roxithromycin].

    Science.gov (United States)

    Wei, Z P; Mao, S R; Bi, D Z

    2000-11-01

    To compare the stability of roxithromycin in solutions of different pH. Roxithromycin solutions of different pH were prepared with water, simulate intestinal fluid (SIF) and simulate gastric fluid (SGF) shown to be the stability of these solutions were tested by colorimetry and HPLC. Roxithromycin was stable in water, SGF and SIF determined by colorimetry. However, it was found to be stable only in water and SIF but unstable in SGF as determined by HPLC. Roxithromycin is unstable in acidic medium like SGF. The metabolite of roxithromycin showed unfavorable interference on the assay of roxithromycin when colorimetry was used. Colorimetry can not be used for the determination and assay of roxithromycin in acidic solution like SGF.

  19. Stability Indicating RP-HPLC Method for Simultaneous Determination of Aspirin and Clopidrogel in Dosage Form

    International Nuclear Information System (INIS)

    Mohd Gousuddin; Sengupta, P.; Tripathi, V.D.; Das, A.

    2016-01-01

    Stability-indicating High Performance Liquid Chromatographic (HPLC) method was developed for simultaneous Aspirin and Clopidogrel, A Phenomenex Gemini C-18, 5 μm column having 250 mm x 4.6 mm i.d. in isocratic mode, with mobile phase containing buffer solution 0.3 % orthophosphoric acid : acetonitrile (65:35, v/v). The flow rate was 1 ml/ min and effluents were monitored at 266 nm. For linearity seven points calibration curve were obtained in a concentration range from 0.030-0.120 mg/ ml for aspirin and 0.015-0.060 mg/ ml for clopidogrel with correlation coefficient 0.9999. In the present study stability indicating HPLC method for the combination was tested by degrading the drugs together under various stress conditions like acid hydrolysis, base hydrolysis, oxidation, thermal and photolytic stress which is recommended by ICH guideline. (author)

  20. Simultaneous Determination of Lactulose and Lactose in Conserved Milk by HPLC-RID

    Directory of Open Access Journals (Sweden)

    Michelle Fernandes Silveira

    2015-01-01

    Full Text Available Heat treatment is applied to dairy products to ensure microbiological quality and increase the shelf life. However, a suitable control of this process is necessary to guarantee nutritional and sensory quality. The aim of this study is to adapt the high performance liquid chromatography (HPLC method for determination of lactulose and lactose content in commercial samples of UHT and sweetened condensed milk. The HPLC method used showed a good resolution of the analytes evaluated. The analyzed UHT milk samples presented levels for lactulose in accordance with the limit recommended by the International Dairy Federation. There was no significant variation in lactulose concentration for sweetened condensed milk samples. However, one sweetened condensed milk sample showed lactose level lower than the established values (10–12%.

  1. Authentication and distinction of Shenmai injection with HPLC fingerprint analysis assisted by pattern recognition techniques

    Directory of Open Access Journals (Sweden)

    Xue-Feng Lu

    2012-10-01

    Full Text Available In this paper, the feasibility and advantages of employing high performance liquid chromatographic (HPLC fingerprints combined with pattern recognition techniques for quality control of Shenmai injection were investigated and demonstrated. The Similarity Evaluation System was employed to evaluate the similarities of samples of Shenmai injection, and the HPLC generated chromatographic data were analyzed using hierarchical clustering analysis (HCA and soft independent modeling of class analogy (SIMCA. Consistent results were obtained to show that the authentic samples and the blended samples were successfully classified by SIMCA, which could be applied to accurate discrimination and quality control of Shenmai injection. Furthermore, samples could also be grouped in accordance with manufacturers. Our results revealed that the developed method has potential perspective for the original discrimination and quality control of Shenmai injection. Keywords: Shenmai injection, High performance liquid chromatography, Fingerprint, Pattern recognition

  2. Effective method for the detection of piroxicam in human plasma using HPLC.

    Science.gov (United States)

    Calvo, Adriana Maria; Prado, Mariel Tavares de Oliveira; Dionísio, Thiago José; Marques, Maria Paula; Brozoski, Daniel Thomas; Lanchote, Vera Lúcia; Faria, Flávio Augusto Cardoso; Santos, Carlos Ferreira

    2016-05-20

    Non-steroidal anti-inflammatory drugs (NSAIDs) are widely used by the general population to alleviate inflammation and pain after oral surgeries. Piroxicam is among the most commonly used NSAIDs and excels in controlling pain, swelling, trismus and other common symptoms of inflammation. This study aimed to evaluate different concentrations of piroxicam and its major metabolite, 5'-hydroxypiroxicam, in human plasma samples over time using high performance liquid chromatography (HPLC) after liquid-liquid extraction. Briefly, 10 volunteers participated in this study after approval by the Ethics Committee of Bauru School of Dentistry, Universidade de São Paulo - USP, Brazil. Volunteers received a single dose oral of piroxicam (20 mg) and had blood collected at various times following an established protocol. The methodology of liquid-liquid extraction was effective for determining concentrations of piroxicam in plasma using HPLC in 10 out of 10 volunteers while 5'-hydroxypiroxicam was only detected in 2 out of 10 volunteers.

  3. Separation of Alkyne Enantiomers by Chiral Column HPLC Analysis of Their Cobalt-Complexes

    Directory of Open Access Journals (Sweden)

    Qiaoyun Liu

    2017-03-01

    Full Text Available Separation of the enantiomers of new chiral alkynes in strategic syntheses and bioorthogonal studies is always problematic. The chiral column high-performance liquid chromatography (HPLC method in general could not be directly used to resolve such substrates, since the differentiation of the alkyne segment with the other alkane/alkene segment is not significant in the stationary phase, and the alkyne group is not a good UV chromophore. Usually, a pre-column derivatization reaction with a tedious workup procedure is needed. Making use of easily-prepared stable alkyne-cobalt-complexes, we developed a simple and general method by analyzing the in situ generated cobalt-complex of chiral alkynes using chiral column HPLC. This new method is especially suitable for the alkynes without chromophores and other derivable groups.

  4. Analysis of 2-ethylhexyl-p-methoxycinnamate in sunscreen products by HPLC and Raman spectroscopy.

    Science.gov (United States)

    Cheng, J; Li, Y S; L Roberts, R; Walker, G

    1997-10-01

    The analyses of 2-ethylhexyl-p-methoxycinnamate (EHMC) using HPLC and Raman spectroscopy have been undertaken and compared. EHMC, which is one of the most widely used sunscreen agents in suncare products in the US, exhibits a strong Raman signal. This signal clearly appears in both ethanol solutions of EHMC as well as in commercial sunscreen lotions containing this sun screen agent. A method for the direct detection and analysis of EHMC has been developed using Raman spectroscopy. This was accomplished by correlating the Raman intensities with the HPLC assays for a series of prototype suncare formulations. Based upon this information, it would be possible to employ Raman spectroscopy as an in-process control method in the commercial production of suncare products containing EHMC. The possibility of applying surface-enhanced Raman scattering for trace analysis was discussed.

  5. Experimental Studies of quantitative evaluation using HPLC and safety of Bee Venom Acupuncture

    Directory of Open Access Journals (Sweden)

    Seong Bong Jang

    2006-02-01

    Full Text Available Objectives : This study was conducted to carry out quantitative evaluation and safety of Bee Venom Acupuncture. Methods : Content analysis was done using HPLC, measurement of , and histological observations were made on the skin and muscles. Results : 1. According to HPLC analysis, each BVA-1 contained approximately , and BVA-2 contained approximately . But the volume of coating was so minute, slight difference exists between each needle. 2. LD50 of mouse with BVA-1 was 16 counts and this is equivalent to 640 needles/kg, making Bee Venom Acupuncture safe treatment apparatus. 3. Regardless of the number of needles, there was no sign of blood stasis or inflammation detected on the skin and muscle tissues. Conclusion : Above results indicate that the Bee Venom Acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

  6. Chromatographic characterization of 99mTc-EHDP complexes by HPLC and GPC

    International Nuclear Information System (INIS)

    Groot, G.J. de.

    1991-01-01

    Technetium-99m is a radioactive element and can be used in medical diagnostics. There are several technetium-99m complexes all having a specific preference for different organs. The aim of this thesis is to contribute to the identification of these complexes by analyzing them by the high performance liquid chromatography (HPLC) and the gel permeation chromatography (GPC) separation method. The first method separates with respect to the charge, the second one separates with respect to the size of the complexes. The HPLC method makes it possible to study the changes in the composition of the complex as a function of time. This kind of study is described in this thesis. Another part of this thesis describes the realization of a automated separation system. The advantages of the system compared to commercial available systems is that this system is less expensive and better suitable for measuring radioactive signals with a low intensity. (R.B.). 142 refs.; 30 figs.; 9 tabs

  7. Isolation and HPLC method development of azafrin from Alectra parasitica var. chitrakutensis.

    Science.gov (United States)

    Agrawal, Poonam; Laddha, Kirti; Tiwari, Ashok

    2014-01-01

    This study was undertaken to isolate and quantify azafrin in Alectra parasitica (Scrophulariaceae) rhizomes. A simple method for the isolation of carotenoid, azafrin, involves solvent extraction of the dried rhizome powder using a single solvent and further purification by recrystallisation. The structure of the compound was elucidated and confirmed by thin-layer chromatography, infrared spectroscopy, mass spectroscopy and nuclear magnetic resonance spectral analysis. A specific and rapid reversed-phase high-performance liquid chromatography (HPLC) method was developed for the analysis of azafrin. The method was validated for accuracy, precision, linearity and specificity. Validation revealed that the method is specific, accurate, precise, reliable and reproducible. The proposed HPLC method can be used for the identification and quantitative analysis of azafrin in A. parasitica rhizomes.

  8. Study of the electrooxidation of ethanol on hydrophobic electrodes by DEMS and HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez Pereira, M.; Davila Jimenez, M.; Elizalde, M.P.; Manzo-Robledo, A.; Alonso-Vante, N

    2004-09-15

    The electrochemical oxidation of ethanol in alkaline solution has been studied on Cu-PVC electrode and Ni/Cu-PVC composite electrodes modified by ruthenium nanoparticles. The techniques used were cyclic voltammetry (CV), steady-state potentiostatic method, on line differential electrochemical mass spectrometry (DEMS), and high-performance liquid chromatography (HPLC). The chemical products: acetaldehyde and acetic acid were detected measuring the proper mass charge (m/z) ratios. These products were also confirmed by HPLC. The surface modification of composite electrodes by ruthenium nanoparticles promotes the formation of acetaldehyde. As shown by DEMS, the surface modification shifts the onset potential for oxygen evolution reaction on the Cu-PVC composite electrode towards more anodic values.

  9. Discrimination of Black Ball-point Pen Inks by High Performance Liquid Chromatography (HPLC)

    International Nuclear Information System (INIS)

    Mohamed Izzharif Abdul Halim; Norashikin Saim; Rozita Osman; Halila Jasmani; Nurul Nadhirah Zainal Abidin

    2013-01-01

    In this study, thirteen types of black ball-point pen inks of three major brands were analyzed using high performance liquid chromatography (HPLC). Separation of the ink components was achieved using Bondapak C-18 column with gradient elution using water, ethanol and ethyl acetate. The chromatographic data obtained at wavelength 254.8 nm was analyzed using agglomerative hierarchical clustering (AHC) and principle component analysis (PCA). AHC was able to group the inks into three clusters. This result was supported by PCA, whereby distinct separation of the three different brands was achieved. Therefore, HPLC in combination with chemometric methods may be a valuable tool for the analysis of black ball-point pen inks for forensic purposes. (author)

  10. Automated injection of a radioactive sample for preparative HPLC with feedback control

    International Nuclear Information System (INIS)

    Iwata, Ren; Yamazaki, Shigeki

    1990-01-01

    The injection of a radioactive reaction mixture into a preparative HPLC column has been automated with computer control for rapid purification of routinely prepared positron emitting radiopharmaceuticals. Using pneumatic valves, a motor-driven pump and a liquid level sensor, two intelligent injection methods for the automation were compared with regard to efficient and rapid sample loading into a 2 mL loop of the 6-way valve. One, a precise but rather slow method, was demonstrated to be suitable for purification of 18 F-radiopharmaceuticals, while the other, due to its rapid operation, was more suitable for 11 C-radiopharmaceuticals. A sample volume of approx 0.5 mL can be injected onto a preparative HPLC column with over 90% efficiency with the present automated system. (author)

  11. The use of dihexyldithiocarbamate in reverse-phase HPLC of metal chelates

    Science.gov (United States)

    Fatimah, S. S.; Bahti, H. H.; Hastiawan, I.; Permanasari, A.

    2018-05-01

    Dialkyldithiocarbamates have long been used as chelating agents in reverse-phase HPLC of transition metals. In the previous study, an alkyl homolog of this type of ligand, namely dihexyldithiocarbamate (DHDTC), was synthesized and characterized. The use of this particular ligand in the revese-phase HPLC of some selected transition metal ions is now reported for the first time. The mobile phase comprising of the flow rate and of the detection, in the separation of the metal chelates of Cd (II), Fe (III), Cu (II), and Co (III), were investigated on a C-18 column. The results showed that dihexylditiocarbamate could be used for separating Cd (II), Fe(III), Cu(II), and Co(III). Therefore, it could be used in simultaneous analysis.

  12. [Determination of aristolochic acid A in Guanxinsuhe preparations by RP-HPLC].

    Science.gov (United States)

    Li, Lin; Gao, Hui-Min; Wang, Zhi-Min; Wang, Wei-Hao

    2006-01-01

    To establish a determination method of aristolochic acid A in Guanxisuhe preparations by RP-HPLC. The instrument used was Hewlett-Packard 1100 HPLC with a Alltech C18 column (4.6 mm x 250 mm, 5 microm). The mobile phase was methanol-water-acetic acid (68: 32:1) and the flow rate was 1.0 mL x min(-1). The UV detection wavelength was 390 nm and the column temperature was at 35 degrees C. The extracted solvent for the preparations was methanol solution contained 10% formic acid. The calibration curve was linear (r = 0.999 9) within the range of 0.119-1.89 microg for aristolochic acid A. The average recovery 99.0%, RSD 0.63%. The method with good linear relationship was convenient, quick, accurate, and suitable for the quality control of the aristolochic acid A in Guanxinsuhe and other traditional Chinese medicines containing aristolochic acid A.

  13. Analysis of D3-,4-,5-phosphorylated phosphoinositides using HPLC.

    Science.gov (United States)

    Munnik, Teun

    2013-01-01

    Detection of polyphosphoinositides (PPIs) is difficult due to their low chemical abundancy. This problem is further complicated by the fact that PPIs are present as various, distinct isomers, which are difficult, if not impossible, to separate by conventional thin layer chromatography (TLC) systems. PPIs in plants include PtdIns3P, PtdIns4P, PtdIns5P, PtdIns(3,5)P 2, and PtdIns(4,5)P 2. Here, a protocol is described analyzing plant PPIs using (32)P-orthophosphorus pre-labeled material. After extraction, lipids are deacylated and the resulting glycerophosphoinositol polyphosphates (GroPInsPs) separated by HPLC using a strong anion-exchange column and a shallow salt gradient. Alternatively, PPIs are first separated by TLC, the lipids reisolated, deacylated, and the GroPInsPs then separated by HPLC.

  14. [Simultaneous determination of eight kinds of conjunct bile acids in human bile by R-HPLC].

    Science.gov (United States)

    Dai, Z; Tan, G; Qian, K; Chen, X

    1997-01-01

    A method for the simultaneous determination of eight kinds of conjunct bile acids in human bile was developed by HPLC. They were separated on a YWG-C18 (3 microns) column at 30 degrees C, with methanol/water (65/35, V/V, pH3.0) as mobile phase, and detection wavelength at UV 210 nm. The linear ranges were 50-1,000 microns.ml-1, the recoveries were 91.2%-108.6%. The biles of 30 cases with cholelithiasis cholecystolithiasis and 20 cases without gallstone were detected by HPLC. The results showed that the constitution of bile acids was different between patients with cholelithiasis cholecystolithiasis and patients without gallstone.

  15. Eruptive viscosity and volcano morphology

    International Nuclear Information System (INIS)

    Posin, S.B.; Greeley, R.

    1988-01-01

    Terrestrial central volcanoes formed predominantly from lava flows were classified as shields, stratovolcanoes, and domes. Shield volcanoes tend to be large in areal extent, have convex slopes, and are characterized by their resemblance to inverted hellenic war shields. Stratovolcanoes have concave slopes, whereas domes are smaller and have gentle convex slopes near the vent that increase near the perimeter. In addition to these differences in morphology, several other variations were observed. The most important is composition: shield volcanoes tend to be basaltic, stratovolcanoes tend to be andesitic, and domes tend to be dacitic. However, important exceptions include Fuji, Pico, Mayon, Izalco, and Fuego which have stratovolcano morphologies but are composed of basaltic lavas. Similarly, Ribkwo is a Kenyan shield volcano composed of trachyte and Suswa and Kilombe are shields composed of phonolite. These exceptions indicate that eruptive conditions, rather than composition, may be the primary factors that determine volcano morphology. The objective of this study is to determine the relationships, if any, between eruptive conditions (viscosity, erupted volume, and effusion rate) and effusive volcano morphology. Moreover, it is the goal of this study to incorporate these relationships into a model to predict the eruptive conditions of extraterrestrial (Martian) volcanoes based on their morphology

  16. Characterization of plasma protein binding dissociation with online SPE-HPLC

    OpenAIRE

    Li, Ping; Fan, Yiran; Wang, Yunlong; Lu, Yaxin; Yin, Zheng

    2015-01-01

    A novel parameter of relative recovery (Rre) was defined and determined by online SPE-HPLC to characterize plasma protein binding (PPB) kinetics of highly plasma binding drugs. The proportional relationship of Rre with koff of PPB has been established with a new SPE model. A rapid, easy to use method could potentially be used to categorize PK properties of the drug candidates in the decision process of drug discovery and development.

  17. Validation for The Quantification of Andrographolide Isolated from Andrographis paniculata Nees Plant Using HPLC

    OpenAIRE

    Yandi Syukri; Agung Endro Nugroho; Ronny Martien; Endang Lukitaningsih

    2015-01-01

    The aim of study was to develop quantitative analysis of isolated andrographolide from Andrographis paniculata and different solvent for prelimenary studies to preperation Self Nano Emulsifying Drug Delivery System (SNEDDS) using HPLC. The separation was acquired on Sunfire C18 column with an isocratic mixture of methanol and water at a ratio of 6:4, v/v as a mobile phase. The method to determine the content of isolated andrographolide showed an adequate precision, with a RSD smaller than 1%....

  18. Identification and Quantitation of Asparagine and Citrulline Using High-Performance Liquid Chromatography (HPLC)

    OpenAIRE

    Bai, Cheng; Reilly, Charles C.; Wood, Bruce W.

    2007-01-01

    High-performance liquid chromatography (HPLC) analysis was used for identification of two problematic ureides, asparagine and citrulline. We report here a technique that takes advantage of the predictable delay in retention time of the co-asparagine/citrulline peak to enable both qualitative and quantitative analysis of asparagine and citrulline using the Platinum EPS reverse-phase C18 column (Alltech Associates). Asparagine alone is eluted earlier than citrulline alone, but when both of them...

  19. Assessment of radiochemical purity of [{sup 18}F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z., E-mail: radiofarmacoscdtn@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Producao de Radiofarmacos

    2011-07-01

    The quality control of [{sup 18}F]fludeoxyglucose ({sup 18}FDG) has received attention due to its increasing clinical use. Although the quality requirements of {sup 18}FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of {sup 18}FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. {sup 18}FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of {sup 18}FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of {sup 18}FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of {sup 18}FDG, considering operational conditions of our laboratory. (author)

  20. HPLC/DAD Intercomparison on Phytoplankton Pigments (HIP-1, HIP-2, HIP-3 and HIP-4)

    OpenAIRE

    CANUTI Elisabetta; RAS Josephine; GRUNG Merete; ROTTGERS Rudiger; COSTA GOELA Priscilla; ARTUSO Florinda; CATALDI Dario

    2016-01-01

    From 2009 to 2015, in the context of the MERIS (Medium Resolution Imaging Spectrometer) validation activities, the JRC Marine Optical Laboratory organised four HPLC Intercomparison exercises for Phytoplankton Pigment measurements (HIP-1, HIP-2, HIP-3 and HIP-4), involving seven European accredited and reference laboratories. The objectives of these intercomparison exercises were: creating a reference community at European level for phytoplankton pigment analysis capable of supporting satel...