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Sample records for rapid liquid chromatographic

  1. A rapid hydrophilic interaction liquid chromatographic determination of glimepiride in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    Si Zhou

    2017-09-01

    Full Text Available Glimepiride is one of the most widely prescribed antidiabetic drugs and contains both hydrophobic and hydrophilic functional groups in its molecules, and thus could be analyzed by either reversed-phase high performance liquid chromatography (HPLC or hydrophilic interaction liquid chromatography (HILIC. In the literature, however, only reversed-phase HPLC has been reported. In this study, a simple, rapid and accurate hydrophilic interaction liquid chromatographic method was developed for the determination of glimepiride in pharmaceutical formulations. The analytical method comprised a fast ultrasound-assisted extraction with acetonitrile as a solvent followed by HILIC separation and quantification using a Waters Spherisorb S5NH2 hydrophilic column with a mobile phase consisting of acetonitrile and aqueous acetate buffer (5.0 mM. The retention time of glimepiride increased slightly with decrease of mobile phase pH value from 6.8 to 5.8 and of acetonitrile content from 60% to 40%, indicating that both hydrophilic, ionic, and hydrophobic interactions were involved in the HILIC retention and elution mechanisms. Quantitation was carried out with a mobile phase of 40% acetonitrile and 60% aqueous acetate buffer (5.0 mM at pH 6.3, by relating the peak area of glimepiride to that of the internal standard, with a detection limit of 15.0 μg/L. UV light absorption responses at 228 nm were linear over a wide concentration range from 50.0 μg/L to 6.00 mg/L. The recoveries of the standard added to pharmaceutical tablet samples were 99.4–103.0% for glimepiride, and the relative standard deviation for the analyte was less than 1.0%. This method has been successfully applied to determine the glimepiride contents in pharmaceutical formulations.

  2. Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

    Science.gov (United States)

    Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

    2017-04-15

    A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Dual liquid and gas chromatograph system

    Science.gov (United States)

    Gay, D.D.

    A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  4. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  5. SIMULTANEOUS ANALYSIS OF AZIDOTHYMIDINE AND ITS MONOPHOSPHATE, DIPHOSPHATE AND TRIPHOSPHATE DERIVATIVES IN BIOLOGICAL-FLUIDS, TISSUE AND CULTURED-CELLS BY A RAPID HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC METHOD

    NARCIS (Netherlands)

    MOLEMA, G; JANSEN, RW; Visser, Jan; MEIJER, DKF

    1992-01-01

    A rapid high-performance liquid chromatographic (HPLC) method for the simultaneous analysis of the antiviral drug azidothymidine (AZT), AZT monophosphate, AZT diphosphate and AZT triphosphate, with ultraviolet detection in the nanomolar range, is described. Determination of these compounds in vitro

  6. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop and validate a simple, efficient and reliable Liquid chromatographic-mass spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs, ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  7. Liquid chromatographic analysis of phenobarbitone, ethosuximide ...

    African Journals Online (AJOL)

    A liquid chromatographic method for the simultaneous assay of four anticonvulsant drugs, phenobarbitone, ethosuximide, phenytoin and carbamazepine on a polystyrene-divinyl benzene column is described. The method was developed by the systematic study of different types of co-polymer materials, type and ...

  8. Validated high performance liquid chromatographic (HPLC) method ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-22

    Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

  9. Quantification of rifampicin in human plasma and cerebrospinal fluid by a highly sensitive and rapid liquid chromatographic-tandem mass spectrometric method.

    Science.gov (United States)

    Srivastava, Abhishek; Waterhouse, David; Ardrey, Alison; Ward, Stephen A

    2012-11-01

    A highly sensitive and rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed to measure the levels of the antitubercular drug rifampicin (RIF) in human plasma and cerebrospinal fluid (CSF). The analyte and internal standard (IS) were isolated from plasma and CSF by a simple organic solvent based precipitation of proteins followed by centrifugation. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring (MRM) mode. The assay was linear in the concentration range 25-6400 ng/mL with intra- and inter-day precision of <7% and <8%, respectively. The validated method was applied to the study of RIF pharmacokinetics in human CSF and plasma over 25 h period after a 10 mg/kg oral dose. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Decomposition of pilocarpine eye drops assessed by a highly efficient high pressure liquid chromatographic method

    NARCIS (Netherlands)

    Kuks, P. F.; Weekers, L. E.; Goldhoorn, P. B.

    1990-01-01

    A rapid high-resolution high pressure liquid chromatographic method was developed for assaying pilocarpine. Pilocarpine in ophthalmic solutions decomposes fairly rapidly to give isopilocarpine, pilocarpic acid and isopilocarpic acid. The quality of an ophthalmic solution can be assessed by assaying

  11. High Performance Liquid Chromatographic Method for Determination of Dipyridamole in Human Plasma

    Directory of Open Access Journals (Sweden)

    DAVOOD BEIGI BAND ARAB ADI

    1999-08-01

    Full Text Available A simple, rapid and specific high-performance liquid chromatographic procedure is reported for"nquantitative determination of dipyridamole in human -plasma. The assay uses a reversed-phase"nhigh-performance liquid chromatographic (HPLC and UV detection at 280nm and has a limit"nof detection of approximately 5ng/mL. The mobile phase consists of MeOH-H20 (60:40"nadjusted to pH 3.3. Dipyridamole was extracted from plasma by back-extraction procedure, with"npropranolol as the internal standard. The reproducibility of the method is satisfactory

  12. Liquid chromatographic determination of sennosides in Cassia angustifolia leaves.

    Science.gov (United States)

    Srivastava, Alpuna; Pandey, Richa; Verma, Ram K; Gupta, Madan M

    2006-01-01

    A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanol-water (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 microm, 125 x 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 microg/mL). Detection limits were 10 microg/mL for sennoside B and 35 microg/mL for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 microg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

  13. A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

    Science.gov (United States)

    Dawson, V.K.

    1982-01-01

    The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

  14. Sensitive high performance liquid chromatographic method for the ...

    African Journals Online (AJOL)

    A new simple, sensitive, cost-effective and reproducible high performance liquid chromatographic (HPLC) method for the determination of proguanil (PG) and its metabolites, cycloguanil (CG) and 4-chlorophenylbiguanide (4-CPB) in urine and plasma is described. The extraction procedure is a simple three-step process ...

  15. Development and Validation of a Liquid Chromatographic Method ...

    African Journals Online (AJOL)

    A liquid chromatographic method for the simultaneous determination of six human immunodeficiency virus (HIV) protease inhibitors, indinavir, saquinavir, ritonavir, amprenavir, nelfinavir and lopinavir, was developed and validated. Optimal separation was achieved on a PLRP-S 100 Å, 250 x 4.6 mm I.D. column maintained ...

  16. High performance liquid chromatographic determination of ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-08

    ) high performance liquid chromatography (HPLC) grade .... applications. These are important requirements if the reagent is to be applicable to on-line pre or post column derivatisation in a possible automation of the analytical.

  17. Rapid validated liquid chromatographic method coupled with ...

    African Journals Online (AJOL)

    NTB in human plasma, and thus can be applied efficiently for the analysis of clinical samples containing. NTB. Keywords: ... permits the analysis of a lot of clinical samples containing NTB in a ... from Milli-Q plus purification system, Millipore, ... Fifty microliter of CBP working standard solution ... Percentage relative error (%.

  18. Micro-column plasma emission liquid chromatograph. [Patent application

    Science.gov (United States)

    Gay, D.D.

    1982-08-12

    In a direct current plasma emission spectrometer for use in combination with a microcolumn liquid chromatograph, an improved plasma source unit is claimed. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

  19. Chiral ionic liquids in chromatographic and electrophoretic separations.

    Science.gov (United States)

    Kapnissi-Christodoulou, Constantina P; Stavrou, Ioannis J; Mavroudi, Maria C

    2014-10-10

    This report provides an overview of the application of chiral ionic liquids (CILs) in separation technology, and particularly in capillary electrophoresis and both gas and liquid chromatography. There is a large number of CILs that have been synthesized and designed as chiral agents. However, only a few have successfully been applied in separation technology. Even though this application of CILs is still in its early stages, the scientific interest is increasing dramatically. This article is focused on the use of CILs as chiral selectors, background electrolyte additives, chiral ligands and chiral stationary phases in electrophoretic and chromatographic techniques. Different examples of CILs, which contain either a chiral cation, a chiral anion or both, are presented in this review article, and their major advantages along with their potential applications in chiral electrophoretic and chromatographic recognition are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Determination of hexachlorocyclohexane pesticide residues in wool fat by a combined high-performance liquid chromatographic-gas-liquid chromatographic method

    International Nuclear Information System (INIS)

    Ali, S.L.

    1978-01-01

    Beta- and gamma-hexachlorocyclohexane residues were determined in twelve wool fat samples by using a combined high-performance liquid chromatographic (HPLC)-gas-liquid chromatographic (GLC) method. After extraction and chromatographic clean-up on a silca-gel column, the sample was further purified by HPLC on a reversed-phase C-18 column with methanol as the mobile phase. The final determination was effected by GLC with a 1-mCi nickel-63 electron-capture detector. The analytical method was checked by addition of carbon-14-labelled lindane and measurement of the radioactivity in a liquid scintillation counter. (Auth.)

  1. High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

    Science.gov (United States)

    Weinberger, R; Mann, B; Posluszny, J

    1980-04-01

    A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

  2. High-performance liquid chromatographic method for guanylhydrazone compounds.

    Science.gov (United States)

    Cerami, C; Zhang, X; Ulrich, P; Bianchi, M; Tracey, K J; Berger, B J

    1996-01-12

    A high-performance liquid chromatographic method has been developed for a series of aromatic guanylhydrazones that have demonstrated therapeutic potential as anti-inflammatory agents. The compounds were separated using octadecyl or diisopropyloctyl reversed-phase columns, with an acetonitrile gradient in water containing heptane sulfonate, tetramethylammonium chloride, and phosphoric acid. The method was used to reliably quantify levels of analyte as low as 785 ng/ml, and the detector response was linear to at least 50 micrograms/ml using a 100 microliters injection volume. The assay system was used to determine the basic pharmacokinetics of a lead compound, CNI-1493, from serum concentrations following a single intravenous injection in rats.

  3. Liquid chromatographic separation of zalcitabine and its stereoisomers.

    Science.gov (United States)

    Scypinski, S; Ross, A J

    1994-10-01

    A liquid chromatographic method capable of separating and quantitating the stereoisomers of zalcitabine has been developed and validated. The separation was achieved with an Astec Cyclobond I--RSP column and a mobile phase of 0.25% triethylamine in water adjusted to a pH of 6.5 with glacial acetic acid. All enantiomers were found to exhibit a linear response in the range of 0.1-10% in the presence of 100% zalcitabine. Precision of analysis was found to be less than 1.5% at a level of 1% relative to zalcitabine. The limit of detection for two of the three enantiomeric impurities was determined to be 0.05% relative to zalcitabine. The detection limit for the third was found to be 0.1%. This method was successfully applied to the analysis of reference standards and several production scale batches. All of these materials were found to be stereochemically pure to a level of 99.8% or better.

  4. Comprehensive two-dimensional liquid chromatographic analysis of poloxamers.

    Science.gov (United States)

    Malik, Muhammad Imran; Lee, Sanghoon; Chang, Taihyun

    2016-04-15

    Poloxamers are low molar mass triblock copolymers of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO), having number of applications as non-ionic surfactants. Comprehensive one and two-dimensional liquid chromatographic (LC) analysis of these materials is proposed in this study. The separation of oligomers of both types (PEO and PPO) is demonstrated for several commercial poloxamers. This is accomplished at the critical conditions for one of the block while interaction for the other block. Reversed phase LC at CAP of PEO allowed for oligomeric separation of triblock copolymers with regard to PPO block whereas normal phase LC at CAP of PPO renders oligomeric separation with respect to PEO block. The oligomeric separation with regard to PEO and PPO are coupled online (comprehensive 2D-LC) to reveal two-dimensional contour plots by unconventional 2D IC×IC (interaction chromatography) coupling. The study provides chemical composition mapping of both PEO and PPO, equivalent to combined molar mass and chemical composition mapping for several commercial poloxamers. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. High performance liquid chromatographic determination of glucosamine in rat plasma.

    Science.gov (United States)

    Aghazadeh-Habashi, Ali; Sattari, Saeed; Pasutto, Franco; Jamali, Fakhreddin

    2002-01-01

    A high performance liquid chromatographic method was developed for the determination of glucosamine (GlcN) in rat plasma. Internal standard, galactosamine, was added to 100 micro L of plasma containing GlcN followed by precipitation of plasma proteins with acetonitrile. Evaporation of the decanted supernatant solution was accelerated by the addition of methanol. GlcN was derivatized by addition of a solution containing 1-naphthyl isothiocyanate. Sample cleanup included passage through an anion exchange cartridge. Analysis was accomplished by injection of 0.1 mL of the sample solution into an isocratic HPLC system consisting of a C18 column, a mobile phase of acetonitrile: water: acetic acid: triethylamine (4.5: 95.5:0.1:0.05), a flow rate of 0.9 mL/min, and a UV detector set at 254 nm. Galactosamine and GlcN appeared 26 and 29 min post-injection, respectively. The assay was linear over the range of 1.25-400 micro g/mL (CV<10%) with a detection limit of 0.63 microg/mL and a limit of quantification of 1.25 microg/mL. The method was applied to the determination of GlcN in rat plasma after oral administration of 350 mg/kg of GlcN hydrochloride. The present assay is specific, sensitive, precise, and accurate and is suitable for pharmacokinetic studies.

  6. High-pressure liquid chromatographic assay of Bay n 7133 in human serum.

    OpenAIRE

    Fasching, C E; Hughes, C E; Hector, R F; Peterson, L R

    1984-01-01

    A high-pressure liquid chromatographic method that includes a Sep-Pak (Waters Associates, Inc., Milford , Mass.) preparation of human serum was employed for the quantitative assay of Bay n 7133. Drug levels of 0.1 to 20 micrograms/ml could be detected. No interference from amphotericin B was found in the chromatographic analysis of Bay n 7133.

  7. Rapid differentiation of rocky mountain spotted fever from chickenpox, measles, and enterovirus infections and bacterial meningitis by frequency-pulsed electron capture gas-liquid chromatographic analysis of sera.

    Science.gov (United States)

    Brooks, J B; McDade, J E; Alley, C C

    1981-01-01

    Normal sera and sera from patients with Rocky Mountain spotted fever, chickenpox, enterovirus infections, measles, and Neisseria meningitidis infections were extracted with organic solvents under acidic and basic conditions and then derivatized with trichloroethanol or heptafluorobutyric anhydride-ethanol to form electron-capturing derivatives of organic acids, alcohols, and amines. The derivatives were analyzed by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). There were unique differences in the FPEC-GLC profiles of sera obtained from patients with these respective diseases. With Rocky Mountain spotted fever patients, typical profiles were detected as early as 1 day after onset of disease and before antibody could be detected in the serum. Rapid diagnosis of Rocky Mountain spotted fever by FPEC-GLC could permit early and effective therapy, thus preventing many deaths from this disease. PMID:7276147

  8. Reverse-Phase High-Performance Liquid Chromatographic Separation of Methylated and Non-Methylated Nucleic Acid Bases

    OpenAIRE

    Madyastha, Prema; Rao, Pratima; Deobagkar, DN; Madyastha, KM

    1983-01-01

    A high-performance liquid chromatographic sepration method is described for the detection of 5-methylcytosine and 6-methyladenine in nucleic acid ext. The bases were sepd. on a Waters $C18 \\mu$ Bondapak column with a water: methanol acetic acid system. Effluents were monitored by UV absorption at 254 nm. The bases were estd. by peak heights which are proportional to the amts. of the individual bases. The method is rapid, sensitive, easy to perform and reproducible.

  9. Liquid chromatographic determination of seven antioxidants in dry food.

    Science.gov (United States)

    Page, B D; Charbonneau, C F

    1989-01-01

    The liquid chromatographic determinative step of the official method for propyl gallate, trihydroxybutyrophenone, tert-butylhydroquinone, nordihydroguaiaretic acid, butylated hydroxyanisole (BHA), 3,5-di-tert-butyl-4-hydroxymethylphenol, and butylated hydroxytoluene (BHT) in fats and oils has been applied to their determination in a number of dry foods. A representative sample (10 g) is homogenized first with hexane (25 mL), then with 5 mL added water, and finally with 75 mL added acetonitrile. The hexane and acetonitrile are decanted, filtered, and separated; the hexane and rehydrated food are reextracted with 2 additional portions of acetonitrile, and the combined acetonitrile extracts are concentrated and diluted to 10 mL. An aliquot is analyzed as described in the official method, using a 150 x 4.6 mm 5 microns C-18 column. The need for rehydration to maximize the recovery of BHA and other antioxidants from marketplace dry food samples such as potato flakes, dry coffee whiteners, and dessert topping mixes was demonstrated. Rehydration was not required for cheese snacks, breakfast cereals, cake mixes, and some other foods. The need for rehydration should be determined by analyzing other foods with and without the addition of water. Potato and corn chips, popcorn and cheese snacks, breakfast cereals, dry beverage mixes, rice, potato flakes, french fried potatoes, and cake mixes were spiked with the above antioxidants at 10-50 ppm. Overall recoveries ranged from 64.3 to 105.6% and repeatabilities ranged from 0.7 to 10.8%. A total of 109 samples of the above foods were analyzed, and 64% contained detectable (greater than 1-2 ppm) antioxidants, mainly BHA and BHT.

  10. High-performance liquid chromatographic analysis of methadone hydrochloride oral solution.

    Science.gov (United States)

    Beasley, T H; Ziegler, H W

    1977-12-01

    A direct and rapid high-performance liquid chromatographic assay for methadone hydrochloride in a flavored oral solution dosage form is described. A syrup sample, one part diluted with three parts of water, is introduced onto a column packed with octadecylsilane bonded on 10 micrometer porous silica gel (reversed phase). A formic acid-ammonium formate-buffered mobile phase is linear programmed with acetonitrile. The absorbance is monitored continuously at 280 or 254 nm, using a flow-through, UV, double-beam photometer. An aqueous methadone hydrochloride solution is used for external standardization. The relative standard deviation was not more than 1.0%. Drug recovery from a syrup base was better than 99.8%.

  11. High-performance liquid chromatographic quantitation of desmosine plus isodesmosine in elastin and whole tissue hydrolysates

    International Nuclear Information System (INIS)

    Soskel, N.T.

    1987-01-01

    Quantitation of desmosine and isodesmosine, the major crosslinks in elastin, has been of interest because of their uniqueness and use as markers of that protein. Accurate measurement of these crosslinks may allow determination of elastin degradation in vivo and elastin content in tissues, obviating lengthy extraction procedures. We have developed a method of quantitating desmosine plus isodesmosine in hydrolysates of tissue and insoluble elastin using high-performance liquid chromatographic separation and absorbance detection that is rapid (21-35 min) and sensitive (accurate linearity from 100 pmol to 5 nmol). This method has been used to quantitate desmosines in elastin from bovine nuchal ligament and lung and in whole aorta from hamsters. The ability to completely separate [ 3 H]lysine from desmosine plus isodesmosine allows the method to be used to study incorporation of lysine into crosslinks in elastin

  12. Performance characteristics of bioassay, radioenzymatic assay, homogeneous enzyme immunoassay, and high-performance liquid chromatographic determination of serum gentamicin

    International Nuclear Information System (INIS)

    Delaney, C.J.; Opheim, K.E.; Smith, A.L.; Plorde, J.J.

    1982-01-01

    We compared the accuracy, precision, and between-method error of the microbiological assay, the radioenzymatic assay, the homogeneous enzyme immunoassay, and the high-performance liquid chromatographic assay for the quantitation of gentamicin in serum. Precision and accuracy were evaluated by reference samples prepared to contain 0.0 to 32.7 micrograms of gentamicin per ml. Correlations between the methods utilized patient sera with gentamicin concentrations ranging from 0.6 to 13.3 micrograms/ml. All methods were reliable within acceptable limits for routine clinical use; intermethod correlation coefficients exceeded 0.96. Relative to the microbiological assay, the alternative methods offer the advantage of rapid analysis. The elapsed times for acquiring data on a set of 10 specimens under routine operating conditions were 0.5 h by the enzyme immunoassay, 4 h by the radioenzymatic assay, 5 h by the high-performance liquid chromatographic assay, and 10 h by the microbiological assay

  13. Liquid chromatographic determination with fluorescence detection of B6 vitamers and riboflavin in milk and pharmaceuticals

    International Nuclear Information System (INIS)

    Gatti, R.; Gioia, M.G.

    2005-01-01

    A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B 6 vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B 2 in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B 6 and Vitamin B 2 in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol

  14. Rapid on-site sensing aflatoxin B1 in food and feed via a chromatographic time-resolved fluoroimmunoassay.

    Directory of Open Access Journals (Sweden)

    Zhaowei Zhang

    Full Text Available Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1. In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring.

  15. Rapid on-site sensing aflatoxin B1 in food and feed via a chromatographic time-resolved fluoroimmunoassay.

    Science.gov (United States)

    Zhang, Zhaowei; Tang, Xiaoqian; Wang, Du; Zhang, Qi; Li, Peiwu; Ding, Xiaoxia

    2015-01-01

    Aflatoxin B1 poses grave threats to food and feed safety due to its strong carcinogenesis and toxicity, thus requiring ultrasensitive rapid on-site determination. Herein, a portable immunosensor based on chromatographic time-resolved fluoroimmunoassay was developed for sensitive and on-site determination of aflatoxin B1 in food and feed samples. Chromatographic time-resolved fluoroimmunoassay offered a magnified positive signal and low signal-to-noise ratio in time-resolved mode due to the absence of noise interference caused by excitation light sources. Compared with the immunosensing performance in previous studies, this platform demonstrated a wider dynamic range of 0.2-60 μg/kg, lower limit of detection from 0.06 to 0.12 µg/kg, and considerable recovery from 80.5% to 116.7% for different food and feed sample matrices. It was found to be little cross-reactivity with other aflatoxins (B2, G1, G2, and M1). In the case of determination of aflatoxin B1 in peanuts, corn, soy sauce, vegetable oil, and mouse feed, excellent agreement was found when compared with aflatoxin B1 determination via the conversational high-performance liquid chromatography method. The chromatographic time-resolved fluoroimmunoassay affords a powerful alternative for rapid on-site determination of aflatoxin B1 and holds a promise for food safety in consideration of practical food safety and environmental monitoring.

  16. Measurement Uncertainty of Liquid Chromatographic Analyses Visualized by Ishikawa Diagrams

    OpenAIRE

    Meyer, Veronika R.

    2017-01-01

    Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncer...

  17. Liquid chromatographic-tandem mass spectrometric assay for ...

    African Journals Online (AJOL)

    Methods: Blood and urine samples were obtained from healthy volunteers who admitted to not being on any medications. The investigated analytes were chromatographically separated on a C18 column (Luna®-PFP 100Å column, 50 mm × 2.0 mm i.d., 3.0 μm) with the aid of a mobile phase containing A; acetonitrile (ACN) ...

  18. Development of Direct Reversed-Phase High Performance liquid chromatographic method for quantitative determination of gabapentin in pharmaceutical dosage

    International Nuclear Information System (INIS)

    Hassan, W.; Zaman, B.; Rahman, S.; Rahman, A.U.; Ali, N.; Mohammadzai, I.U.

    2012-01-01

    The objective of the present work was to develop and validate a rapid analytical method for quantitative determination of Gabapentin in pharmaceutical dosage tablets and capsules. An accurate, simple, and sensitive reversed-phase high performance liquid chromatographic (HPLC) method, UV detection at 215 nm and flow rate at 1.0 ml/min has been developed. Isocratic elution was used instead of gradient elution to reduce the time and cost of serial analysis. The mobile phase was a mixture of water and methanol (HPLC grade). The retention time (Rt) of Gabapentin was 4.681 +- 0.013 minutes. Recovery, Precision, accuracy, and linearity were determined for the stated method. The calibration curve was linear and the correlation coefficient was 0.9996. There was no chromatographic interference from other excipients present in dosage form. The method was validated appropriately and successfully used for determination of Gabapentin in Pharmaceutical formulations. (author)

  19. Measurement uncertainty of liquid chromatographic analyses visualized by Ishikawa diagrams.

    Science.gov (United States)

    Meyer, Veronika R

    2003-09-01

    Ishikawa, or cause-and-effect diagrams, help to visualize the parameters that influence a chromatographic analysis. Therefore, they facilitate the set up of the uncertainty budget of the analysis, which can then be expressed in mathematical form. If the uncertainty is calculated as the Gaussian sum of all uncertainty parameters, it is necessary to quantitate them all, a task that is usually not practical. The other possible approach is to use the intermediate precision as a base for the uncertainty calculation. In this case, it is at least necessary to consider the uncertainty of the purity of the reference material in addition to the precision data. The Ishikawa diagram is then very simple, and so is the uncertainty calculation. This advantage is given by the loss of information about the parameters that influence the measurement uncertainty.

  20. High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

    Science.gov (United States)

    A reverse-phase high performance liquid chromatographic (RP-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 RP-C16-Amide column and a ternary gradient system consistin...

  1. The combination of the liquid chromatograph with the nuclear magnetic resonance spectrometer

    International Nuclear Information System (INIS)

    Scott, R.P.W.

    1986-01-01

    The association of the liquid chromatograph with the NMR spectrometer would be a very powerful analytical system for the separation and identification of unknown mixtures. There are, however, some serious difficulties involved with the association of these two techniques. The historical development of NMR chromatography is outlined and some problems are discussed. (Auth.)

  2. Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

    OpenAIRE

    Hassib, Sonia T.; Farag, Awatef E.; Elkady, Ehab F.

    2011-01-01

    Simple, accurate and precise reversed-phase liquid chromatographic (LC) and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS) and trimethoprim (TMP) in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm) based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9):acetonitrile:water (25:100:50, v/v/v) at a flow rate of 1...

  3. Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

    Science.gov (United States)

    Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

    2014-01-01

    Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

  4. The development of a high performance liquid chromatograph with a sensitive on-stream radioactivity monitor for the analysis of 3H- and 14C-labelled gibberellins

    International Nuclear Information System (INIS)

    Reeve, D.R.; Yokota, T.; Nash, L.; Crozier, A.

    1976-01-01

    The development of a high performance liquid chromatograph for the separation of gibberellins is described. The system combines high efficiency, peak capacity, and sample capacity with rapid speed of analysis. In addition, the construction details of a sensitive on-stream radioactivity monitor are outlined. The overall versatility of the chromatograph has been demonstrated by the separation of a range of 3 H- and 14 C-labelled gibberellins and gibberellin precursors. The system also has considerable potential for the analysis of abscisic acid and acidic and neutral indoles. (author)

  5. Liquid chromatographic method for determining the concentration of bisazir in water

    Science.gov (United States)

    Scholefield, Ronald J.; Slaght, Karen S.; Allen, John L.

    1997-01-01

    Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys (Petromyzon marinus) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-N-methylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a C18 column, a mobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

  6. Liquid chromatographic determination of pioglitazone in pharmaceuticals, serum and urine samples

    International Nuclear Information System (INIS)

    Abro, K.; Memon, N.; Bhanger, M.I.; Mahesar, S.A.; Parveen, S.

    2011-01-01

    A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC) with UV detection (221 nm) has been developed for the determination of the anti-hyper glycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine) after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith Performance RP-18e (10 4.6mm) column using mobile phase composition of acetonitrile: mixed phosphate buffer (pH 2.5; 10mM) (30:70, v/v) with a flow rate of 2.0mL/min. The total run time was 2 min. under optimized conditions. The calibration curve was found to be linear in the range of 1-10 mu g mL/sup -1/ with regression coefficient of 0.9996, and the lower limit of detection 72 ng/20 mu L injection. The method has been validated for the system suitability, linearity, precision and accuracy, limits of detection, specificity, stability and robustness. The %recovery of Pioglitazone in pharmaceutical formulations was found to be 104.7%. The assay has been applied successfully to the pharmaceutical Tablet samples and biological fluids (serum and urine) of healthy volunteers. (author)

  7. Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

    Directory of Open Access Journals (Sweden)

    Kranti P. Musmade

    2014-01-01

    Full Text Available A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC method with UV detection has been developed and validated for quantification of naringin (NAR in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1. The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity.

  8. Comparative in vitro assessment of tolterodine tartrate tablets by high performance liquid chromatographic (HPLC

    Directory of Open Access Journals (Sweden)

    Hossein Danafar

    2016-06-01

    Full Text Available Tolterodine tartrate, is a new, potent and competitive muscarinic receptor antagonist in clinical development for the treatment of urge incontinence and other symptoms of unstable bladder. The purpose of this study is to establish a reliable and quick method for the assignment of tolterodine tartrate by high performance liquid chromatography with ultraviolet detection (HPLC-UV. A rapid  and  sensitive  high  performance  liquid  chromatographic  (HPLC  method  has  been developed  for  determination  of  tolterodine tartrate.  Mobile phase was composed of phosphate acetate 0.1 M (pH 2.5-acetonitrile (50:50 v/v with a flow rate of 1.2 ml/min. The eluted peaks were detected by a UV detector was set at wavelength of 285 nm. The method was validated in the range of tolterodine tartrate concentrations from 10 to 100 µg/ml. The limits of detection (LOD and quantitation (LOQ of the method were 5 and 10 µg/ml, respectively. The average drug recovery was 98.20 % throughout the linear concentration range. The average within-run and between-run accuracy values of 98.56 % and 99.11 % respectively. Statistical  assessment  of  various  in  vitro  dissolution  parameters  and  assay  results was  also  conducted  to  establish  if  there were  any significant difference among them. The validated HPLC method has been used successfully to study tolterodine tartrate.

  9. High-performance liquid chromatographic radioenzymatic assay for plasma catecyholamines

    International Nuclear Information System (INIS)

    Klaniecki, T.S.; Corder, C.N.; McDonald, R.H. Jr.; Feldman, J.A.

    1977-01-01

    A new assay method for plasma catecholamimes (CA) requiring only 50 μl has been developed, which uses high performance liquid chromatography (HPLC). The norepinephrine (NE), dopamine (D), and epinephrine (E) compounds found in plasma are radioactively o-methylated with S-[methyl- 3 H]-adenosyl-L-methionine ( 3 H-SAM) 3 H-SAM by the reaction of catechol-o-methyl transferase (COMT). The reaction is terminated and a standard mixture of nonradioactive o-methylated analogues of NE, D, and E is added to act as a carrier. Following separation by HPLC, the D,L-normetanephrine (NMN), 3-methoxy-4-hydroxyphenylethyl-amine or 3-methoxytyramine (3-MOT), and metanephrine (MN) radioactive peaks are collected which represent NE, D, and E, respectively. Then MNM and MN are oxidized to vanillin, and 3-MOT is acetylated. The products are subsequently separated by solvent extraction. This is necessary in order to avoid high radioactive blanks and to allow quantitation of the radioactivity by liquid scintillation spectrometry. The mean supine levels of NE, D, and E in normal subjects were respectively 182, 33, and 87 pg/ml of plasma. Similar assays on patients with pheochromocytoma revealed 797, 80, and 470 pg/ml

  10. Liquid chromatographic separation of terpenoid pigments in foods and food products.

    Science.gov (United States)

    Cserháti, T; Forgács, E

    2001-11-30

    The newest achievements in the use of various liquid chromatographic techniques such as adsorption and reversed-phase thin-layer chromatography and HPLC employed for the separation and quantitative determination of terpenoid-based color substances in foods and food products are reviewed. The techniques applied for the analysis of individual pigments and pigments classes are surveyed and critically evaluated. Future trends in the separation and identification of pigments in foods and food products are delineated.

  11. Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

    Science.gov (United States)

    Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

    2013-11-01

    A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. High-performance liquid-chromatographic separation of subcomponents of antimycin-A

    Science.gov (United States)

    Abidi, S.L.

    1988-01-01

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  13. Liquid chromatographic determination of saccharin in beverages and desserts: complementary collaborative study.

    Science.gov (United States)

    Sjöberg, A M

    1988-01-01

    A complementary collaborative study was conducted on a liquid chromatographic method for determination of saccharin in accordance with the latest international recommendations. One industrial and 6 official food control laboratories analyzed 3 samples of a juice, a soft drink, and a dessert at concentration levels of 26-90 mg/L, 33-73 mg/L, and 56-147 mg/kg, respectively. Blind duplicates and a blank were supplied for each type of material at each concentration level. The beverage was chromatographed directly and the dessert was extracted with ethanol before chromatography. Average recoveries were 95-107%. The reproducibility relative standard deviations were 6.4-7.3% for the juice, 9.2-20.6% for the soft drink, and 13.4-16.2% for the dessert. The outlier percentage was 14.3%. The results were compared with those of an earlier collaborative study by Nordic laboratories and with general collaborative results obtained by AOAC.

  14. Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

    Science.gov (United States)

    Simonaitis, R A; Cail, R S

    1975-09-01

    A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

  15. Stereospecific high-performance liquid chromatographic assay of sotalol in plasma.

    Science.gov (United States)

    Carr, R A; Foster, R T; Bhanji, N H

    1991-09-01

    A convenient high-performance liquid chromatographic (HPLC) assay was developed for determination of sotalol (STL) enantiomers in plasma. Following addition of the internal standard (IS; racemic atenolol), enantiomers of STL and IS were extracted using ethyl acetate. After evaporation of the organic layer, samples were derivatized with a solution of S-(+)-1-(1-naphthyl)ethyl isocyanate (NEIC). The resulting diastereomers were chromatographed with normal-phase HPLC with chloroform:hexane:methanol [65:33:2 (v/v)] as the mobile phase at a flow rate of 2 ml/min. The fluorescence detection wavelength was set at 220 nm for excitation with no emission filter. The suitability of the assay for pharmacokinetic studies was determined by measuring STL enantiomers in the plasma of a healthy subject after administration of a single 160-mg oral, racemic dose of STL.

  16. Rapid planar chromatographic analysis of 25 water-soluble dyes used as food additives.

    Science.gov (United States)

    Morlock, Gertrud E; Oellig, Claudia

    2009-01-01

    A rapid planar chromatographic method for identification and quantification of 25 water-soluble dyes in food was developed. In a horizontal developing chamber, the chromatographic separation on silica gel 60F254 high-performance thin-layer chromatography plates took 12 min for 40 runs in parallel, using 8 mL ethyl acetate-methanol-water-acetic acid (65 + 23 + 11 + 1, v/v/v/v) mobile phase up to a migration distance of 50 mm. However, the total analysis time, inclusive of application and evaluation, took 60 min for 40 runs. Thus, the overall time/run can be calculated as 1.5 min with a solvent consumption of 200 microL. A sample throughput of 1000 runs/8 h day can be reached by switching between the working stations (application, development, and evaluation) in a 20 min interval, which triples the analysis throughput. Densitometry was performed by absorption measurement using the multiwavelength scan mode in the UV and visible ranges. Repeatabilities [relative standard deviation (RSD), 4 determinations] at the first or second calibration level showed precisions of mostly or = 0.9987) and RSD values ( or = 0.9996). If necessary for confirmation, online mass spectra were recorded within a minute.

  17. Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

    Science.gov (United States)

    Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2008-10-31

    A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

  18. Diagnosis of rinderpest in Tanzania by a rapid chromatographic strip-test.

    Science.gov (United States)

    Wambura, P N; Moshy, D W; Mbise, A N; Mollel, G O; Taylor, W P; Anderson, J; Bruning, A

    2000-06-01

    A simple chromatographic strip-test based on Clearview technology, is under development as a pen-side test for the detection of rinderpest antigen in eye swabs taken from cattle in the field. An outbreak of rinderpest occurred in the northern zone of Tanzania from late February to June 1997. The affected cattle exhibited very mild clinical signs, which made clinical diagnosis difficult. One hundred and seven eye swabs were collected from cattle suspected of infection with rinderpest. These were tested in the field using a prototype of the pen-side test and 13 (12.15%) of the samples were found to be positive for the presence of rinderpest antigen. These were confirmed by ICE. The positive cases were predominantly found in the Ngorongoro district. This demonstrates the usefulness of such a simple, rapid pen-side diagnostic assay, particularly when clinically 'mild' strains of rinderpest are present.

  19. Development and validation of micellar liquid chromatographic methods for the determination of antibiotics in different matrixes.

    Science.gov (United States)

    Rambla-Alegre, Maria; Esteve-Romero, Josep; Carda-Broch, Samuel

    2011-01-01

    Antibiotics are the most important bioactive and chemotherapeutic compounds to be produced by microbiological synthesis, and they have proved their worth in a variety of fields, such as medicinal chemistry, agriculture, and the food industry. Interest in antibiotics has grown in parallel with an increasingly high degree of productivity in the field of analytical applications. Therefore, it is necessary to develop chromatographic procedures capable of determining various drugs simultaneously in the shortest possible time. Micellar liquid chromatography (MLC) is an RP-HPLC technique that offers advantages over conventional HPLC as far as sample preparation, selectivity, and versatility are concerned. Its main advantage is that samples can be injected directly into the chromatographic system with no previous preparation step. This paper mainly focuses on the results of the authors' own recent research and reports the chromatographic conditions for determination of various antibiotics (penicillins, quinolones, and sulfonamides) in different matrixes (pharmaceuticals, biological fluids, and food). The work of other authors on MLC-based antibiotic determination has been included.

  20. A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

    Science.gov (United States)

    Gartzke, J; Jäger, H; Vins, I

    1991-01-01

    A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

  1. Sorption and chromatographic techniques for processing liquid waste of nuclear fuel cycle

    International Nuclear Information System (INIS)

    Gelis, V.M.; Milyutin, V.V.; Chuveleva, E.A.; Maslova, G.B.; Kudryavtseva, S.P.; Firsova, L.A.; Kozlitin, E.A.

    2000-01-01

    In the spent nuclear fuel processing procedures the significant quantity of high level liquid waste containing long-lived high toxic radionuclides of cesium, strontium, promethium, americium, curium, etc. is generated. Separation of those radionuclides from the waste not merely simplifies the further safe waste handling but also reduces the waste processing operation costs due to the market value of certain individual radionuclide preparations. Recovery and separation of high grade pure long-lived radionuclide preparations is frequently performed by means of chromatographic techniques. (authors)

  2. High-pressure liquid chromatographic determination of chlorphenesin carbamate and the beta-isomeric carbamate.

    Science.gov (United States)

    Beyer, W F

    1976-12-01

    A high-pressure liquid chromatographic assay was developed for the determination of chlorphenesin carbamate and its beta-isomeric carbamate. A single 4-mm i.d. X 30-cm column, prepacked with 10 micrometer fully porous silica gel particles, is used with 3% methanol in 50% water-saturated butyl chloride as the mobile phase. The procedure separates chlorphenesin carbamate from several possible impurities in addition to the beta-isomeric carbamate. The assay was applied to bulk drug and compressed tablets. The relative standard deviations for the assays of chlorphenesin carbamate and the beta-isomer are approximately 1 and 2%, respectively.

  3. Total cholesterol in serum determined by isotope dilution/mass spectrometry, with liquid-chromatographic separation

    International Nuclear Information System (INIS)

    Takatsu, Akiko; Nishi, Sueo

    1988-01-01

    We describe an accurate, precise method for determination of total serum cholesterol by isotope dilution/mass spectrometry (IDMS) with liquid chromatographic separation. After adding [3,4- 13 C] cholesterol to serum and hydrolyzing the cholesterol esters, we extract the total cholesterol. High-performance liquid chromatography (HPLC) is used to separate the extracted cholesterol for measurement by electron-impact mass spectrometry with use of a direct-insertion device. To evaluate the specificity and the accuracy of this method, we also studied the conventional IDMS method, which involves converting cholesterol to the trimethylsilyl ether and assay by gas chromatography-mass spectrometry with use of a capillary column. The coefficient of variation for the HPLC method was a little larger than for the conventional method, but mean values by each method agreed within 1% for all sera tested. (author)

  4. Direct chromatographic methods for the rapid determination of homogentisic acid in strawberry tree (Arbutus unedo L.) honey.

    Science.gov (United States)

    Scanu, Roberta; Spano, Nadia; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino; Tapparo, Andrea

    2005-10-07

    Two rapid and direct chromatographic methods based on reverse phase-high performance liquid chromatography (RP-HPLC) and ion chromatography (IC) were developed for the determination of homogentisic acid (HA) in honey. This is the marker of the botanic origin of strawberry tree honey. The methods were validated and tested using 22 samples from Sardinia, Italy. The IC method is faster than the RP-HPLC one (6 min versus 13 min of total run), but it is slightly less sensitive (the limit of detection (LOD), is 26 mg kg(-1) versus 15 mg kg(-1)) and reproducible (relative standard deviation, RSD, of 10.4 and 4.4%, respectively). The whole dataset of validation parameters allows both the proposed methods to be considered as bias-free (by recovery tests, comparison of analytical results of the two independent methods and analysis of a synthetic sample) and precise (both the techniques show a repeatability better than 2% repeatability in the range between 70 and 600 mg kg(-1)).

  5. Characterization of Chinese rice wine taste attributes using liquid chromatographic analysis, sensory evaluation, and an electronic tongue.

    Science.gov (United States)

    Yu, HaiYan; Zhao, Jie; Li, Fenghua; Tian, Huaixiang; Ma, Xia

    2015-08-01

    To evaluate the taste characteristics of Chinese rice wine, wine samples sourced from different vintage years were analyzed using liquid chromatographic analysis, sensory evaluation, and an electronic tongue. Six organic acids and seventeen amino acids were measured using high performance liquid chromatography (HPLC). Five monosaccharides were measured using anion-exchange chromatography. The global taste attributes were analyzed using an electronic tongue (E-tongue). The correlations between the 28 taste-active compounds and the sensory attributes, and the correlations between the E-tongue response and the sensory attributes were established via partial least square discriminant analysis (PLSDA). E-tongue response data combined with linear discriminant analysis (LDA) were used to discriminate the Chinese rice wine samples sourced from different vintage years. Sensory evaluation indicated significant differences in the Chinese rice wine samples sourced from 2003, 2005, 2008, and 2010 vintage years in the sensory attributes of harmony and mellow. The PLSDA model for the taste-active compounds and the sensory attributes showed that proline, fucose, arabinose, lactic acid, glutamic acid, arginine, isoleucine, valine, threonine, and lysine had an influence on the taste characteristic of Chinese rice wine. The Chinese rice wine samples were all correctly classified using the E-tongue and LDA. The electronic tongue was an effective tool for rapid discrimination of Chinese rice wine. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

    Directory of Open Access Journals (Sweden)

    Sonia T. Hassib

    2011-12-01

    Full Text Available Simple, accurate and precise reversed-phase liquid chromatographic (LC and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS and trimethoprim (TMP in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9:acetonitrile:water (25:100:50, v/v/v at a flow rate of 1.6 ml min−1 with UV detection at 210 nm for ERS and 280 nm for TMP. Besides, two spectrophotometric methods were applied after reaction with perchloric acid (12 M which gives a colored product with ERS. Then, the spectral interference between the colored product of ERS and TMP was resolved by either ratio spectra derivative spectrophotometry in the first spectrophotometric method or chemometric techniques, namely classical least-squares (CLS, principal component regression (PCR and partial least-squares regression (PLS in the second spectrophotometric method. The results were statistically compared using one-way analysis of variance (ANOVA. The methods developed were satisfactorily applied to the analysis of the pharmaceutical preparation containing the two drugs and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

  7. A Selective High Performance Liquid Chromatographic Method to Follow the Hydrolytic Degradation of Nicardipine Hydrochloride

    Directory of Open Access Journals (Sweden)

    K. E. Ibrahim

    2010-01-01

    Full Text Available A simple, stability indicating, reverse phase high performance liquid chromatographic method was developed and validated for determination of nicardipine hydrochloride (NC in the presence of its degradation products. The chromatographic separation was performed on Hypersil, BDS-C18, 30 cm × 3.9 mm id, at ambient temperature with UV-detection at 254 nm. A mixture of 20% (v/v aqueous 0.01 M sodium acetate∕acetic acid buffer (pH 4.5 and 80% acetonitrile was used as the mobile phase at a flow rate of 1.5 mL min-1, losartan was used as internal standard. The calibration curve is linear over the concentration range 5-40 μg mL-1, with a regression coefficient of 0.9984 and the % recovery was 99.78±0.17. The method was used to investigate the kinetics of alkaline, acids induced degradation, effect of buffer concentration and temperature. The degradation followed first-order kinetics. The rate constant, half-life time, and activation energy were calculated

  8. Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

    Science.gov (United States)

    Mullett, Wayne M

    2007-03-10

    The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

  9. Covalently coating dextran on macroporous polyglycidyl methacrylate microsphere enabled rapid protein chromatographic separation

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Rongyue; Li, Qiang; Li, Juan; Zhou, Weiqing; Ye, Peili; Gao, Yang; Ma, Guanghui, E-mail: ghma@home.ipe.ac.cn; Su, Zhiguo

    2012-12-01

    Protein denaturation and nonspecific adsorption on polymer media as a chromatographic support have been a problem which needs to be overcome. Macroporous poly(glycidyl methacrylate-divinylbezene) (PGMA-DVB) microspheres prepared in this study were firstly covalently coated with dextran through a three-step method. The dextran was firstly adsorbed onto the microspheres and then covalently bound to the PGMA-DVB microsphere through ether bonds which were formed by hydroxyl group reacting with epoxy group at the presence of 4-(Dimethylamino) pyridine. Finally, the coating dextran layer was crosslinked by ethylene glycol diglycidyl ether to form the continuous network coating. The coated microspheres were characterized by Fourier transform infrared spectra, scanning electron microscope, mercury porosimetry measurements, laser scanning confocal microscope, and protein adsorption experiments. Results showed that PGMA-DVB microspheres coated with dextran successfully maintained the macroporous structure and high permeability. The backpressure was only 1.69 MPa at a high flow rate of 2891 cm/h. Consequently, the hydrophilicity and biocompatibility of modified microspheres were greatly improved, and the contact angle decreased from 184 Degree-Sign to 13 Degree-Sign , and nonspecific adsorption of proteins was decreased to little or none. The clad dextran coating with large amounts of hydroxyl group was easily derived to be various functional groups. The derived media have great potential applications in rapid protein chromatography. - Highlights: Black-Right-Pointing-Pointer Macroporous PGMA-DVB microspheres were covalently coated with dextran. Black-Right-Pointing-Pointer The hydrophilicity of the coated microspheres was significantly improved. Black-Right-Pointing-Pointer The irreversible adsorption of proteins was reduced to zero. Black-Right-Pointing-Pointer The coated microspheres can maintain the macropore structure. Black-Right-Pointing-Pointer The coated microspheres

  10. Covalently coating dextran on macroporous polyglycidyl methacrylate microsphere enabled rapid protein chromatographic separation

    International Nuclear Information System (INIS)

    Zhang, Rongyue; Li, Qiang; Li, Juan; Zhou, Weiqing; Ye, Peili; Gao, Yang; Ma, Guanghui; Su, Zhiguo

    2012-01-01

    Protein denaturation and nonspecific adsorption on polymer media as a chromatographic support have been a problem which needs to be overcome. Macroporous poly(glycidyl methacrylate–divinylbezene) (PGMA–DVB) microspheres prepared in this study were firstly covalently coated with dextran through a three-step method. The dextran was firstly adsorbed onto the microspheres and then covalently bound to the PGMA–DVB microsphere through ether bonds which were formed by hydroxyl group reacting with epoxy group at the presence of 4-(Dimethylamino) pyridine. Finally, the coating dextran layer was crosslinked by ethylene glycol diglycidyl ether to form the continuous network coating. The coated microspheres were characterized by Fourier transform infrared spectra, scanning electron microscope, mercury porosimetry measurements, laser scanning confocal microscope, and protein adsorption experiments. Results showed that PGMA–DVB microspheres coated with dextran successfully maintained the macroporous structure and high permeability. The backpressure was only 1.69 MPa at a high flow rate of 2891 cm/h. Consequently, the hydrophilicity and biocompatibility of modified microspheres were greatly improved, and the contact angle decreased from 184° to 13°, and nonspecific adsorption of proteins was decreased to little or none. The clad dextran coating with large amounts of hydroxyl group was easily derived to be various functional groups. The derived media have great potential applications in rapid protein chromatography. - Highlights: ► Macroporous PGMA–DVB microspheres were covalently coated with dextran. ► The hydrophilicity of the coated microspheres was significantly improved. ► The irreversible adsorption of proteins was reduced to zero. ► The coated microspheres can maintain the macropore structure. ► The coated microspheres were applied to rapid protein separation.

  11. Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

    International Nuclear Information System (INIS)

    Fraley, D.M.; Yates, D.; Manahan, S.E.

    1979-01-01

    Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

  12. Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

    Science.gov (United States)

    Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

    1986-07-01

    This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

  13. High-performance liquid chromatographic analysis of anthraquinone compounds in the Laurera benguelensis

    Science.gov (United States)

    Manojlović, N.; Marković, Z.; Gritsanapan, W.; Boonpragob, K.

    2009-09-01

    A high-performance liquid chromatographic (HPLC) method has been developed for the characterization of anthraquinone metabolites in extracts of the lichen Laurera benguelensis. With this method four anthraquinone derivatives 1,8-dihydroxy-3-methoxy-6-methylanthraquinone, 1,8-dihydroxy-3-formyl-6-methoxyanthraquinone, 1,8-dihydroxy-3-hydroxymethyl-6-methoxy-anthraquinone and 1,3,8-trihyroxy-6-methylanthraquinone can be analyzed. Components of lichen were detected by characteristic ultraviolet spectra and relative retention times. This is first report of phytochemical analysis of L. benguelensis. Importance of this research is in recognizing some new source (lichen and its extracts) as a natural emplacement of antioxidants because oxidation with free radicals or autooxidation is big problem for preservation of food products.

  14. [Reversed-phase high-performance liquid chromatograph--application to serum aluminium monitoring].

    Science.gov (United States)

    Hoshino, H; Kaneko, E

    1996-01-01

    High-Performance Liquid Chromatography (HPLC) with the reversed-phase partition mode separation (including ion-pair one) towards metal chelate compounds prepared in an off-line fashion (precolumn chelation) is most versatile in terms of high sensitivity with base-line flatness, unique selectivity and cost effectiveness. The extraordinary toughness to the complicated matrices encountered in clinical testing is exemplified by the successful application to the aluminium monitoring of human serum samples. The A1 chelate with 2,2'-dihydroxyazobenzene is efficiently chromatographed on a LiChroCART RP-18 column using an aqueous methanol eluent (63.6 wt%) containing tetrabutylammonium bromide as an ion-pair agent. The serum concentration level of A1 down to 6 micrograms dm-3 is readily monitored without influences from iron, chyle and haemolysis.

  15. Liquid-chromatographic determination of sarafloxacin residues in channel catfish muscle-tissue

    Science.gov (United States)

    Meinertz, J.R.; Dawson, V.K.; Gingerich, W.H.; Cheng, B.; Tubergen, M.M.

    1994-01-01

    A liquid chromatographic method is described for the determination of sarafloxacin hydrochloride residues i n channel catfish (ictalurus punctatus) fillets. Sarafloxacin was extracted from fillet tissue with acetonitrile=water (1 + 1). The extract was centrifuged and the supernatant was partitioned with hexane. The aqueous fraction was filtered through a 0.45 Mum filter and evaporated to dryness. The sample was redissolved with 20% acetonitrile-methanol (3 + 2) and 80% trifluoroacetic acid (0.1%), Centrifuged, and filtered to remove proteins. Samples were analyzed by chromatography with gradient elution on a c18 column and with fluorescence detection (excitation at 280 nm and emission above 389 nm). Mean recoveries ranged from 85.4 To 104%, and relative standard deviations ranged from 1.06 To 5.58% In samples spiked at concentrations of 10.0-863.8 Ng/g. The method detection limit for sarafloxacin was 1.4 Ng/g.

  16. A simple subcritical chromatographic test for an extended ODS high performance liquid chromatography column classification.

    Science.gov (United States)

    Lesellier, Eric; Tchapla, Alain

    2005-12-23

    This paper describes a new test designed in subcritical fluid chromatography (SFC) to compare the commercial C18 stationary phase properties. This test provides, from a single analysis of carotenoid pigments, the absolute hydrophobicity, the silanol activity and the steric separation factor of the ODS stationary phases. Both the choice of the analytical conditions and the validation of the information obtained from the chromatographic measurements are detailed. Correlations of the carotenoid test results with results obtained from other tests (Tanaka, Engelhard, Sander and Wise) performed both in SFC and HPLC are discussed. Two separation factors, calculated from the retention of carotenoid pigments used as probe, allowed to draw a first classification diagram. Columns, which present identical chromatographic behaviors are located in the same area on this diagram. This location can be related to the stationary phase properties: endcapping treatments, bonding density, linkage functionality, specific area or silica pore diameter. From the first classification, eight groups of columns are distinguished. One group of polymer coated silica, three groups of polymeric octadecyl phases, depending on the pore size and the endcapping treatment, and four groups of monomeric stationary phases. An additional classification of the four monomeric groups allows the comparison of these stationary phases inside each group by using the total hydrophobicity. One hundred and twenty-nine columns were analysed by this simple and rapid test, which allows a comparison of columns with the aim of helping along their choice in HPLC.

  17. Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

    National Research Council Canada - National Science Library

    Parris, N. A

    1976-01-01

    Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

  18. Abnormal tyrosine and phenylalanine metabolism in patients with tyrosyluria and phenylketonuria; gas-liquid chromatographic analysis of urinary metabolites

    NARCIS (Netherlands)

    Wadman, S.K.; Heiden, C. van der; Ketting, D.; Sprang, F.J. van

    Gas-liquid chromatographic methods have been developed for the analysis of: urinary phenylalanine metabolites (I) in patients with phenylketonuria, tyrosine metabolites (II) in patients with a disturbed tyrosine metabolism at the level of p-hydroxyphenylpyruvate hydroxylase, and homogentisic acid in

  19. Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

    Science.gov (United States)

    Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

    2000-11-01

    Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

  20. Characterization of crude oils and petroleum products: (I Elution liquid chromatographic separation and gas chromatographic analysis of crude oils and petroleum products

    Directory of Open Access Journals (Sweden)

    E.O. Odebunmi

    2002-12-01

    Full Text Available Some physical and chemical properties of samples of light, medium and heavy Nigerian crude oils and petroleum products including gasoline, kerosene and engine oil have been measured and are reported in this paper. The crude oils and petroleum products have also been characterized by fractional distillation and elution liquid chromatography. The fractions obtained from elution liquid chromatography were analyzed using gas chromatography (GC. The GC fractions were identified by comparing the retention time of peaks in the unknown samples with those of components of calibration standard mixtures. The importance of the physico-chemical properties and the significance of the fractional distillation and chromatographic separation methods to industrial process operations have been discussed.

  1. [Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up].

    Science.gov (United States)

    Zhang, Chunyu; Wang, Hui; Zhang, Xiaohui; Ma, Zhongqiang; Deng, Wanmei; Hu, Ke; Ding, Mingyu

    2011-12-01

    A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm x 4.6 mm, 5 microm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25 - 13.4 microg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n = 3) of 0.3% - 5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

  2. An improved high-performance liquid chromatographic method for simultaneous determination of tocopherols, tocotrienols and γ-oryzanol in rice.

    Science.gov (United States)

    Huang, Shao-Hua; Ng, Lean-Teik

    2011-07-22

    An improved normal phase high performance liquid chromatographic (NP-HPLC) method was developed for simultaneous quantification of eight vitamin E isomers (α-, β-, γ- and δ-tocopherols and α-, β-, γ- and δ-tocotrienols) and γ-oryzanol in rice. A complete separation of all compounds was achieved within 25 min using an Inertsil CN-3, SIL-100A 5 μM (4.6 mm × 250 mm) column and an isocratic elution system of hexane/isopropanol/ethylacetate/acetic acid (97.6:0.8:0.8:0.8, v/v/v/v) at a flow rate varying from 0.7 to 1.5 mL min(-1). A linear correlation coefficient (r(2)>0.99) and high reproducibility were obtained at concentrations ranging 0.05-10 μg mL(-1) for vitamin E isomers and 0.5-500 μg mL(-1) for γ-oryzanol. This method proved to be rapid, accurate and reproducible. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Precolumn derivatization followed by liquid chromatographic separation and determination of tramiprosate in rat plasma by fluorescence detector: application to pharmacokinetics.

    Science.gov (United States)

    Rao, R Nageswara; Maurya, Pawan K; Shinde, Dhananjay D; Khalid, Sara

    2011-05-15

    Alzheimer disease (AD) is characterized pathologically by extracellular amyloid deposits composed of amyloid β (Aβ) protein. A simple and rapid method using HPLC with fluorescence detector was developed and validated for determination of tramiprosate in rat plasma. Pre-column derivatization of the deproteinized rat plasma was carried out using o-phthaldialdehyde (OPA) as a fluorescent reagent in presence of 3-mercaptopropionic acid. The liquid chromatographic separation was achieved on a Kromasil C18 column using methanol:acetonitrile: 20 mM phosphate buffer pH 7.5 (8.0:17.5:74.5 v/v/v) as a mobile phase in an isocratic elution mode. The eluents were monitored by a fluorescence detector set at 330 and 450 nm of excitation and emission wavelength respectively. Vigabatrin was used as an internal standard. The method was linear within the range 30.0-1000.0 ng/mL. Design of experiments (DOE) was used to evaluate the robustness of the method. The developed method was applied to study the pharmacokinetics of tramiprosate in rats. Copyright © 2011. Published by Elsevier B.V.

  4. Simple and sensitive high performance liquid chromatographic method for the simultaneous quantitation of the phenylalanine in human plasma

    Directory of Open Access Journals (Sweden)

    Hossein Danafar

    2015-09-01

    Full Text Available Phenylalanine (Phe is the most reliable indicator for the diagnosis of phenylketonuria (PKU. The purpose of this study is to establish a reliable and quick method for the assignment of Phe in peripheral capillary blood from newborns and children by high performance liquid chromatography with ultraviolet detection (HPLC-UV. PKU is an inborn error of metabolism characterized by the inability of the body to use Phe. A rapid and sensitive high performance liquid chromatographic (HPLC method has been developed for determination of Phe in plasma. The method uses a protein precipitation step with sulfosalicilic acid for sample preparation by separation on a Nova-pack C18 column using sodium acetate buffer and acetonitrile (94: 6 v/v adjusted to pH 6.5 with glacial acetic acid. The eluted peaks detected by a UV detector was set at wavelength of 215 nm. The method was validated in the range of Phe concentrations from 0.1 to 20 µg/ml. The limits of detection (LOD and quantitation (LOQ of the method were 0.05 and 0.1 µg/ml, respectively. The average drug recovery from plasma was 88.60 percent throughout the linear concentration range., with the average within-run and between-run accuracy values of 103.3 and 115.350, respectively. The method is quick, easy, very steady and precise for the screen, assignment, and evaluation of Phe in human plasma by HPLC, which is particularly a useful way for screening and diagnosis of PKU and monitoring of a diet therapy.

  5. Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

    Directory of Open Access Journals (Sweden)

    Mei-Liang Chin-Chen

    2012-01-01

    Full Text Available A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS, Brij-35 and N-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v-pentanol-0.01’M NaH2PO4 buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999, limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp., and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp., with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

  6. Ion-pair high performance liquid chromatographic retention behavior of salicylic acid and its derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Lee, K.W.; Chung, Y.S. [Chungbuk National University, Cheongju (Korea); Oh, S.K. [Handok Pharmaceuticals Co. Ltd., Chungbuk (Korea)

    1999-06-01

    The ion-pair high performance liquid chromatographic elution behavior of salicylic acid and its derivatives was studied with measuring capacity factor, k', changing the concentration of ion-pairing reagent (tetrabutylammonium chloride, TBACl) in mobile phase. As a result, it was found that k' of the samples increase at pH 7.2 as the TBACl concentration increase. The derivatives of salicylic acid were separated each other at an optimum mobile phase condition which was found from the observation of the retention behavior. The optimum mobile phase condition was methanol solution(MeOH:H{sub 2}O 30:70) containing 20 mM TBACl for the determination of salicylic acid and methanol solution (MeOH:H{sub 2}O 20:80) containing 40 mM TBACl for p-aminosalicylic acid at pH 7.2. The method has been applied for the analysis of the contents of salicylic acid derivatives in an aspirin tablet and a tuberculosis curing agent. 8 refs., 4 figs., 2 tabs.

  7. Liquid chromatographic determination of urinary 2-thiothiazolidine-4-carboxylic acid, a biomarker of carbon disulphide exposure.

    Science.gov (United States)

    Lee, B L; Yang, X F; New, A L; Ong, C N

    1995-06-23

    An effective gradient high-performance liquid chromatographic method for baseline separation of urinary 2-thiothiazolidine-4-carboxylic acid (TTCA), with photodiode array detection at 271 nm was described. o-Methylhippuric acid was used as an internal standard (I.S.). A 1-ml urine sample was saturated with 300 mg of sodium sulphate, acidified with 100 microliters of 6 M hydrochloric acid, extracted twice with 2 ml of diethyl ether, and after evaporation, the residue was taken up in 1 ml of 0.1% (v/v) phosphoric acid. The two mobile phases used for gradient elution were: (A) 10 mM ammonium dihydrogenphosphate (pH 3.5) and (B) same concentration of buffer but containing 20% (v/v) of methanol (pH 4.8). The flow-rate was set at 1.0 ml/min. TTCA and I.S. were detected at 2.2 and 9.1 min, respectively. The method was validated with urine samples collected from normal subjects and workers occupationally exposed to carbon disulphide. The present method enables the detection of urinary TTCA at a concentration of 0.025 mg/l. Analytical recovery and reproducibility generally exceeded 90%. The proposed method is considered more sensitive, specific and reliable than other existing methods.

  8. Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar

    Directory of Open Access Journals (Sweden)

    Emilia Sawicki

    2016-08-01

    Full Text Available Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are substrates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chromatographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

  9. Liquid chromatographic determination of oxytetracycline in edible fish fillets from six species of fish

    Science.gov (United States)

    Meinertz, J.R.; Stehly, G.R.; Gingerich, W.H.

    1998-01-01

    The approved use of oxytetracycline (OTC) in U.S. Aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100, 1000, and 5000 ng/g. In tissues fortified with OTC at 100, 1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily integratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.

  10. Peak distortion in the column liquid chromatographic determination of omeprazole dissolved in borax buffer.

    Science.gov (United States)

    Arvidsson, T; Collijn, E; Tivert, A M; Rosén, L

    1991-11-22

    Injection of a sample containing omeprazole dissolved in borax buffer (pH 9.2) into a reversed-phase liquid chromatographic system consisting of a mixture of acetonitrile and phosphate buffer (pH 7.6) as the mobile phase and a C18 surface-modified silica as the solid phase resulted under special conditions in split peaks of omeprazole. The degree of peak split and the retention time of omeprazole varied with the concentration of borax in the sample solution and the ionic strength of the mobile phase buffer as well as with the column used. Borax is eluted from the column in a broad zone starting from the void volume of the column. The retention is probably due to the presence of polyborate ions. The size of the zone varies with the concentration of borax in the sample injected. In the borax zone the pH is increased compared with the pH of the mobile phase, and when omeprazole (a weak acid) is co-eluting in the borax zone its retention is affected. In the front part and in the back part of the borax zone, pH gradients are formed, and these gradients can induce the peak splitting. When the dissolving medium is changed to a phosphate buffer or an ammonium buffer at pH 9 no peak distortion of omeprazole is observed.

  11. Liquid chromatographic and ultraviolet spectrophotometric determination of bevantolol and hydrochlorothiazide in feeds.

    Science.gov (United States)

    Spurlock, C H; Schneider, H G

    1984-01-01

    Separate assay methods have been developed for the 2 components of an 80 + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol-water-acetic acid (60 + 40 + 1) containing 0. 005M octane-sulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% +/- 4.3 RSD and at 2.0 mg/g, 101.5% +/- 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% +/- 2.7 RSD and 99.0% +/- 3.5 RSD, respectively, using the method as described.

  12. Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

    Science.gov (United States)

    Barker, S A; Long, A R

    1994-01-01

    The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

  13. Gas--liquid chromatographic determination of total inorganic iodine in milk

    International Nuclear Information System (INIS)

    Bakker, H.J.

    1977-01-01

    Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively

  14. Improved Chromatographic Bioavailability Estimations

    National Research Council Canada - National Science Library

    Dorsey, John

    1996-01-01

    .... Since the inception of reversed phase liquid chromatography there have been many attempts to correlate chromatographic retention with bioavailability and the most often used bulk measure, the octanol...

  15. Liquid chromatographic determination of polyphenenols in czech beers during brewing proces

    Directory of Open Access Journals (Sweden)

    Chunsriimyatav Ganbaatar

    2015-05-01

    Full Text Available High performance liquid chromatographic (HPLC/UV method was adapted for simultaneous determination of seven polyphenols, including derivatives of benzoic (gallic and vanillic acids and cinnamic acids (p-coumaric, ferulic and sinapic acids, flavan-3-ols (catechin and flavonols (rutin in worts and beers at the various stages of the brewing process. Based on the semi-quantitative HPLC analysis, total polyphenols chromatographic index (TPCI was in the ranges of 5.18 - 19.4 mg/L and 7.37 - 20.7 mg/L for all worts and beers, respectively. The HPLC analyses showed that relatively high levels of (+-catechin and gallic acid were in all the worts and the beers, while the values were much lower for ferulic acid, rutin, vanillic acid, sinapic acid and p-coumaric acid. Polyphenols with relatively high concentrations, that were detected in all tested worts and beers, were gallic acid (1.29 - 4.75 mg/L resp. 2.59 - 4.97 mg/L, (+-catechin (1.66 - 7.95 mg/L resp. 4.70 - 10.0 mg/L and ferulic acid (0.41 - 4.53 mg/L resp. 1.05 - 2.87 mg/L. On the other side, the sinapic acid (0.72 - 1.59 mg/L resp. 0.72 - 2.5 mg/L, rutin (1.17 - 2.03 mg/L resp. 1.16 - 2.85 mg/L, p-coumaric acid (ND - 4.73 mg/L resp. ND - 1.44 mg/L and vanillic acid (ND - 1.52 mg/L resp. 0.75 - 1.81 mg/L were detected in lowest concentrations. In both, worts and beers investigated in this study, the changes in the contents of individual polyphenols were not uniform. In the case of some polyphenols, a decrease in the content was observed after boiling the worts with hops or after the main fermentation until maturation and filtration, but with some polyphenols, the concentrations were constant until the end of the process or even increased.

  16. Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis

    OpenAIRE

    Kshirsagar, Parthraj R.; Hegde, Harsha; Pai, Sandeep R.

    2016-01-01

    Background and Aim: This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. Materials and Methods: One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at ?4?C. Results: Contaminant peak was detected in methanol stored in polypropylene m...

  17. Investigating the Effect of Column Geometry on Separation Efficiency using 3D Printed Liquid Chromatographic Columns Containing Polymer Monolithic Phases.

    Science.gov (United States)

    Gupta, Vipul; Beirne, Stephen; Nesterenko, Pavel N; Paull, Brett

    2018-01-16

    Effect of column geometry on the liquid chromatographic separations using 3D printed liquid chromatographic columns with in-column polymerized monoliths has been studied. Three different liquid chromatographic columns were designed and 3D printed in titanium as 2D serpentine, 3D spiral, and 3D serpentine columns, of equal length and i.d. Successful in-column thermal polymerization of mechanically stable poly(BuMA-co-EDMA) monoliths was achieved within each design without any significant structural differences between phases. Van Deemter plots indicated higher efficiencies for the 3D serpentine chromatographic columns with higher aspect ratio turns at higher linear velocities and smaller analysis times as compared to their counterpart columns with lower aspect ratio turns. Computational fluid dynamic simulations of a basic monolithic structure indicated 44%, 90%, 100%, and 118% higher flow through narrow channels in the curved monolithic configuration as compared to the straight monolithic configuration at linear velocities of 1, 2.5, 5, and 10 mm s -1 , respectively. Isocratic RPLC separations with the 3D serpentine column resulted in an average 23% and 245% (8 solutes) increase in the number of theoretical plates as compared to the 3D spiral and 2D serpentine columns, respectively. Gradient RPLC separations with the 3D serpentine column resulted in an average 15% and 82% (8 solutes) increase in the peak capacity as compared to the 3D spiral and 2D serpentine columns, respectively. Use of the 3D serpentine column at a higher flow rate, as compared to the 3D spiral column, provided a 58% reduction in the analysis time and 74% increase in the peak capacity for the isocratic separations of the small molecules and the gradient separations of proteins, respectively.

  18. Liquid chromatographic determination of para-toluenesulfonamide in edible fillet tissues from three species of fish

    Science.gov (United States)

    Meinertz, J.R.; Schmidt, L.J.; Stehly, G.R.; Gingerich, W.H.

    1999-01-01

    Chloramine-T (N-sodium-N-chloro-p-toluene-sulfonamide) is a candidate therapeutic drug for treating bacterial gill disease, a predominant disease of a variety of fish species. Research has been initiated to obtain the U.S. Food and Drug Administration's (FDA) approval for the use of chloramine-T on a variety of fish species. An attribute of a therapeutic aquaculture drug that must be characterized before the FDA approves its use is depletion of the drug's marker residue (the drug's parent compound or metabolite of highest concentration in an edible tissue). Para-Toluenesulfonamide (p-TSA) is the primary degradation product and marker residue for chloramine-T in rainbow trout. To conduct residue depletion studies for chloramine-T in fish, a robust analytical method sensitive and specific for p-TSA residues in edible fillet tissue from a variety of fish was required. Homogenized fillet tissues from rainbow trout (Oncorhynchus mykiss), walleye (Stizostedion vitreum), and channel catfish (Ictalurus punctatus) were fortified at nominal p-TSA concentrations of 17, 67, 200, 333, and 1000 ng/g. Samples were analyzed by isocratic reversed-phase liquid chromatography (LC) with absorbance detection at 226 nm. Mean recoveries of p-TSA ranged from 77 to 93.17%; relative standard deviations ranged from 1.5 to 14%; method quantitation limits ranged from 13 to 18 ng/g; and method detection limits ranged from 3.8 to 5.2 ng/g. The LC parameters produced p-TSA peaks without coelution of endogenous compounds and excluded chromatographic interference from at least 20 chemicals and drugs of potential use in aquaculture.

  19. Liquid chromatographic determination of CPZEN-45, a novel anti-tubercular drug, in biological samples.

    Science.gov (United States)

    Hanif, S N M; Hickey, A J; Garcia-Contreras, L

    2014-01-01

    CPZEN-45 is a new drug candidate being considered for the treatment of tuberculosis (TB). The aim of this study was to develop and validate a reverse-phase high-performance liquid chromatographic (HPLC) method suitable to determine CPZEN-45 concentrations in biological samples. CPZEN-45 was extracted from biological fluids and tissues (plasma, lung and spleen from guinea pig) by sequential extraction with acetonitrile and quantified by a Waters HPLC Alliance System coupled with a ZORBAX Bonus-RP column, guard column and UV detection at 263nm. The mobile phase was 20:80 acetonitrile:ultrapure-water with 0.05% TFA. The CPZEN-45 peak was eluted at 5.1min with no interference from the inherent peaks of plasma, bronchoalveolar lavage (BAL), lung or spleen tissues. Recovery of CPZEN-45 from biological samples was >96% of the spiked amount. The limit of detection was 0.05μg/ml and the limit of quantitation was 0.29μg/ml which was more than 5 and 21 times lower than the reported minimal inhibitory concentration of CPZEN-45 (MIC=1.56μg/ml for Mycobacterium tuberculosis and 6.25μg/ml for MDR-TB, respectively). Thus, HPLC method was deemed reliable, sensitive, reproducible and accurate for the determination of CPZEN-45 concentrations in plasma, BAL, lung and spleen tissues. Therefore, this method was used in subsequent studies in the guinea pig model to determine the disposition of CPZEN-45 after administration of solutions by the IV and SC routes. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Derivatization reactions in the gas—liquid chromatographic analysis of drugs in biological fluids

    NARCIS (Netherlands)

    Hulshoff, A.; Lingeman, H.

    1984-01-01

    Alkylation, acylation, silylation and other derivatization reactions applied to the gas chromatographic analysis of drugs in biological matrices are reviewed. Reaction conditions are discussed in relation to reaction mechanisms. Detector-oriented labelling of drugs, and derivatization with chiral

  1. Core-shell in liquid chromatography: application for determining sulphonamides in feed and meat using conventional chromatographic systems

    Directory of Open Access Journals (Sweden)

    Antonio Armentano

    2016-12-01

    Full Text Available A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-μm column have been optimized on a column packed with 2.6 μm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 μL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster.

  2. High-performance liquid chromatographic determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine in isoniazid tablet formulations.

    Science.gov (United States)

    Butterfield, A G; Lovering, E G; Sears, R W

    1980-02-01

    A high-performance liquid chromatographic procedure is presented for the simultaneous determination of isoniazid and 1-isonicotinyl-2-lactosylhydrazine (I) in isoniazid tablet formulations. An aliquot of a diluted aqueous tablet extract is introduced onto a microparticulate cyanopropyl bonded-phase column using a valve-loop injector and chromatographed using a mobile phase of acetonitrile--0.01 M, pH 3.5 aqueous acetate buffer (5:95). Compound I can be determined at levels as low as 0.5% of the isoniazid label claim. The relative standard deviations are 0.4 and 0.7% for the simultaneous determination of isoniazid and I, respectively. Seven commercial tablet formulations contained 93.8--97.0% of the labeled isoniazid amounts and 0.3--5.8% of I, expressed as equivalent isoniazid relative to the labeled isoniazid level.

  3. Validation of high-performance liquid chromatographic method for analysis of fluconazole in microemulsions and liquid crystals

    Directory of Open Access Journals (Sweden)

    Hilris Rocha e Silva

    2014-04-01

    Full Text Available In recent decades, there has been a significant increase in the incidence of fungal diseases. Certain fungal diseases cause cutaneous lesions and in the usual treatment, generally administred orally, the drug reaches the site of action with difficulty and its concentration is too low. An approach much explored in recent years is the development of nanotechnology-based drug delivery systems, and microemulsions (ME and liquid crystals (LC are promising. ME and LC were developed with oleic acid or copaiba oil as the oil phase, propoxyl (5OP ethoxyl (20 OE cetyl alcohol as surfactant and water. An analytical method to assess the incorporation of fluconazole (FLU in the systems under study was validated according to guidelines of the International Conference on Harmonization (ICH guidelines and the Brazilian Food, Drug and Sanitation Agency (ANVISA. The method was conducted on a C18-RP column (250 × 4.6 mm i.d., maintained at room temperature. The mobile phase consisted of acetonitrile and water (50:50, v/v, run at a flow rate of 1.0mL/min and using ultraviolet detection at 210nm. The chromatographic separation was obtained with a retention time of 6.3min, and was linear in the range of 20-400 µg/mL (r2=0.9999. The specificity showed no interference of the excipients. The accuracy was 100.76%. The limits of detection and quantitation were 0.057 and 0.172 µg.mL-1, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the incorporation of FLU in ME and LC, contributing to improve the quality control and to assure the therapeutic efficacy.

  4. Storing of Extracts in Polypropylene Microcentrifuge Tubes Yields Contaminant Peak During Ultra-flow Liquid Chromatographic Analysis.

    Science.gov (United States)

    Kshirsagar, Parthraj R; Hegde, Harsha; Pai, Sandeep R

    2016-05-01

    This study was designed to understand the effect of storage in polypropylene microcentrifuge tubes and glass vials during ultra-flow liquid chromatographic (UFLC) analysis. One ml of methanol was placed in polypropylene microcentrifuge tubes (PP material, Autoclavable) and glass vials (Borosilicate) separately for 1, 2, 4, 8, 10, 20, 40, and 80 days intervals stored at -4°C. Contaminant peak was detected in methanol stored in polypropylene microcentrifuge tubes using UFLC analysis. The contaminant peak detected was prominent, sharp detectable at 9.176 ± 0.138 min on a Waters 250-4.6 mm, 4 μ, Nova-Pak C18 column with mobile phase consisting of methanol:water (70:30). It was evident from the study that long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peak. Further, this may mislead in future reporting an unnatural compound by researchers. Long-term storage of biological samples prepared using methanol in polypropylene microcentrifuge tubes produce contaminant peakContamination peak with higher area under the curve (609993) was obtained in ultra-flow liquid chromatographic run for methanol stored in PP microcentrifuge tubesContamination peak was detected at retention time 9.113 min with a lambda max of 220.38 nm and 300 mAU intensity on the given chromatographic conditionsGlass vials serve better option over PP microcentrifuge tubes for storing biological samples. Abbreviations used: UFLC: Ultra Flow Liquid Chromatography; LC: Liquid Chromatography; MS: Mass spectrometry; AUC: Area Under Curve.

  5. In-syringe dispersive liquid-liquid microextraction with liquid chromatographic determination of synthetic pyrethroids in surface water

    Directory of Open Access Journals (Sweden)

    Saeed S. Albaseer

    2012-03-01

    Full Text Available An indigenously fabricated in laboratory glass syringe was used for in-syringe dispersive liquid-liquid microextraction (is-DLLME and preconcentration of synthetic pyrethroids (SPs from surface waters suitable for their determination by high performance liquid chromatography. In contrast to classical DLLME, is-DLLME allows the use of lighter-than-water organic solvents and the analysis of environmental contaminants’ samples without prior filtration, which is of great importance due to the high affinity of pyrethroids to adsorb to solid particulates present in environmental samples. The effects of various parameters on the extraction efficiency were evaluated and optimized systemically using one-factor-at-a-time method (OFAT and statistically using full factorial design (24. Three SPs (viz.; cypermethrin, resmethrin and permethrin were analyzed. The method showed good accuracy with RSD% in the range of of 4.8–6.9%. The method detection limits of the three pesticides ranged from 0.14 to 0.16 ng mL-1. The proposed method was applied for the determination of synthetic pyrethroids in lake water

  6. A simple high-performance liquid chromatographic method for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

    Science.gov (United States)

    Shah, Shailesh A; Rathod, Ishwarsinh S; Suhagia, Bhanubhai N; Pandya, Saurabh S; Parmar, Vijay K

    2008-09-01

    A simple, rapid, and reproducible reverse-phase high-performance liquid chromatographic method is developed for the estimation of boswellic acids, the active constituents in Boswellia serrata oleo-gum resin. The chromatographic separation is performed using a mobile phase consisting of acetonitrile-water (90:10, % v/v) adjusted to pH 4 with glacial acetic acid on a Kromasil 100 C18 analytical column with flow rate of 2.0 mL/min and detection at 260 nm. The elution times are 4.30 and 7.11 min for 11-keto beta-boswellic acid (11-KBA) and 3-acetyl 11-keto beta-boswellic acid (A-11-KBA), respectively. The calibration curve is linear in the 11.66-58.30 microg/mL and 6.50-32.50 microg/mL range for 11-KBA and A-11-KBA, respectively. The limits of detection are 2.33 microg/mL and 1.30 microg/mL for 11-KBA and A-11-KBA, respectively. The mean recoveries are 98.24% to 104.17% and 94.12% to 105.92% for 11-KBA and A-11-KBA, respectively. The inter- and intra-day variation coefficients are less than 5%. The present method is successfully applied for the estimation of boswellic acids from the market formulations containing Boswellia serrata extract.

  7. Study and ICH validation of a reverse-phase liquid chromatographic method for the quantification of the intact monoclonal antibody cetuximab

    Directory of Open Access Journals (Sweden)

    Antonio Martínez-Ortega

    2016-04-01

    Full Text Available Cetuximab (CTX is a potent chimeric mouse/human monoclonal antibody (mAb approved worldwide for treatment of metastatic colorectal cancer. Among the various biological and physical analyses performed for full study on this biopharmaceutic, the determination of the concentration preparations throughout manufacturing and subsequent handling in hospital is particularly relevant. In the present work, the study and validation of a method for quantifying intact CTX by reverse-phase high-performance liquid chromatography with diode array detection ((RPHPLC/DAD is presented. With that end, we checked the performance of a chromatographic method for quantifying CTX and conducted a study to validate the method as stability-indicating in accordance with the International Conference on Harmonization guidelines (ICH for biotechnological drugs; therefore, we evaluated linearity, accuracy, precision, detection and quantification limits, robustness and system suitability. The specificity of the method and the robustness of the mAb formulation against external stress factors were estimated by comprehensive chromatographic analysis by subjecting CTX to several informative stress conditions. As demonstrated, the method is rapid, accurate, and reproducible for CTX quantification. It was also successfully used to quantify CTX in a long-term stability study performed under hospital conditions.

  8. High performance liquid chromatographic separation of polycyclic aromatic hydrocarbons on microparticulate pyrrolidone and application to the analysis of shale oil

    International Nuclear Information System (INIS)

    Mourey, T.H.; Siggia, S.; Uden, P.C.; Crowley, R.J.

    1980-01-01

    A chemically bonded pyrrolidone substrate is used for the high performance liquid chromatographic separation of polycyclic aromatic hydrocarbons. The cyclic amide phase interacts electronically with the polycyclic aromatic hydrocarbons in both the normal and reversed phase modes. Separation is effected according to the number of aromatic rings and the type of ring condensation. Information obtained is very different from that observed on hydrocarbon substrates, and thus these phases can be used in a complementary fashion to give a profile of polycyclic aromatics in shale oil samples. 7 figures, 1 table

  9. Rapid process development of chromatographic process using direct analysis in real time mass spectrometry as a process analytical technology tool.

    Science.gov (United States)

    Yan, Binjun; Chen, Teng; Xu, Zhilin; Qu, Haibin

    2014-06-01

    The concept of quality by design (QbD) is widely applied in the process development of pharmaceuticals. However, the additional cost and time have caused some resistance about QbD implementation. To show a possible solution, this work proposed a rapid process development method, which used direct analysis in real time mass spectrometry (DART-MS) as a process analytical technology (PAT) tool for studying the chromatographic process of Ginkgo biloba L., as an example. The breakthrough curves were fast determined by DART-MS at-line. A high correlation coefficient of 0.9520 was found between the concentrations of ginkgolide A determined by DART-MS and HPLC. Based on the PAT tool, the impacts of process parameters on the adsorption capacity were discovered rapidly, which showed a decreased adsorption capacity with the increase of the flow rate. This work has shown the feasibility and advantages of integrating PAT into QbD implementation for rapid process development. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Rapid determination of ampicillin in bovine milk by liquid chromatography with fluorescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Ang, C.Y.W.; Luo, Wenhong [National Center for Toxicological Research, Jefferson, AR (United States)

    1997-01-01

    A rapid and sensitive liquid chromatographic (LC) method was developed for the determination of ampicillin residues in raw bovine milk, processed skim milk, and pasteurized, homogenized whole milk with vitamin D. Milk samples were deproteinized with trichloroacetic acid (TCA) and acetonictrile. After centrifugation, the clear supernatant was reacted with formaldehyde and TCA under heat. The major fluorescent derivative of ampicillin was then determined by reversed-phase LC with fluorescence detection. Average recoveries of ampicillin fortified at 5, 10, and 20 ppb (ng/mL) were all >85% with coefficients of variation <10%. Limits of detection ranged from 0.31 to 0.51 ppb and limits of quantitation, from 0.66 to 1.2 ppb. After appropriate validation, this method should be suitable for rapid analysis of milk for ampicillin residues at the tolerance level of 10 ppb. 16 refs., 4 figs., 3 tabs.

  11. Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

    Science.gov (United States)

    Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

    2014-06-13

    This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. High performance liquid chromatographic method for determination of ezetimibe in pharmaceutical formulation tablets

    Directory of Open Access Journals (Sweden)

    Hossein Danafar

    2016-09-01

    Full Text Available Ezetimide belongs to a class of lipid lowering    compounds    that    selectively    inhibits intestinal   absorption   of   cholesterol   and   related phytosterols. The purpose of this study is to establish a reliable and quick method for the assignment of ezetimibe in tablets form by high performance liquid chromatography with ultraviolet detection (HPLC-UV. A rapid  and  sensitive  HPLC  method  has  been developed  for  determination  of  ezetimibe in tablets formulation.  Mobile phase was composed of acetonitrile-ammonium acetate (10 mM, pH 3.0, 75:25 (v/v with a flow rate of 1 ml/min. The eluted peaks were detected by a UV detector was set at wavelength of 240 nm. The method results in excellent separation with good resolution of analyte. Standard curves were linear (r = 0.996 over the wide ezetimibe concentration range of 10-60.0 µg mL-1 with acceptable accuracy and precision. The limits of detection (LOD and quantitation (LOQ of the method were 5 and 10 µg/ml, respectively. The average drug recovery was 95.3% throughout the linear concentration range. Statistical  assessment  of  various  in  vitro  dissolution  parameters  and  assay  results was  also  conducted  to  establish  if  there were  any significant difference among them. The validated HPLC method has been used successfully to study ezetimibe. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

  13. Ultra-performance liquid chromatographic determination of tocopherols and retinol in human plasma.

    Science.gov (United States)

    Bell, Edward C; John, Mathew; Hughes, Rodney J; Pham, Thu

    2014-10-01

    A rapid, selective and sensitive ultra-performance liquid chromatography method has been developed for the detection and quantification of tocopherols and retinol in human plasma. Alpha-tocopherol, gamma-tocopherol and retinol are assayed using fluorescence detection. Excitation/emission wavelengths are 295/330 nm and 325/470 nm for the analysis of both tocopherols and retinol, respectively. Retinol acetate is employed as the internal standard. The reversed-phase method incorporates gradient elution with a mobile phase consisting of methanol and acetonitrile. Separation of vitamin compounds is achieved using a bridged ethyl hybrid C18 column. The retention times for retinol, retinol acetate, gamma-tocopherol and alpha-tocopherol are 1.6, 1.8, 3.9 and 4.3 min, respectively. The limits of quantification for retinol, gamma-tocopherol and alpha-tocopherol were 0.02, 0.02 and 0.1 µg/mL, respectively. The assay method is suitable for the analysis of tocopherols and retinol in human plasma. The method may be applied following the ingestion of foods fortified with these fat-soluble vitamins. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. A simple high-performance liquid chromatographic practical approach for determination of flurbiprofen

    Directory of Open Access Journals (Sweden)

    Muhammad Akhlaq

    2011-01-01

    Full Text Available A simple, rapid, sensitive, and specific high-performance liquid chromatography (HPLC assay for flurbiprofen has been developed and validated practically. The chromatography was conducted using Gemini C18 column (5 μm; 4.6 mm × 250 mm, Phenomenex, California, USA. The mobile phase containing disodium hydrogen phosphate solution (30 mM pH 7.0 and acetonitrile (50:50; and the isocratic flow rate of 1.0 ml/min were used in the current study. Detection was made at 247 nm. The calibration curve was linear (r ≥ 0.9996 over the concentration range of 5-50 mm/ml. Mean percentage (% recovery ± % relative standard deviation (RSD ranged from 97.07 ± 0.008 to 103.66 ± 0.013. Within-day and between-day precision were also in acceptable range of 98.83 ± 0.004 to 104.56 ± 0.009. In order to confirm the practical applicability of the method developed, flurbiprofen controlled release matrix tablets were subjected to the dissolution studies and the release rate was analyzed. The reported HPLC for flurbiprofen provides several advantages of simplicity, high specificity, accuracy, and very short run-cycle time. It is suggested that the method should be used for the routine quality control analysis of flurbiprofen pure drug and its dosage forms.

  15. Evaluation of rapid immuno chromatographic assay kit using monoclonal mpt64 antibodies for identification of mycobacterium tuberculosis complex

    International Nuclear Information System (INIS)

    Satti, L.; Ikram, A.; Malik, N.

    2010-01-01

    To evaluate the performance of rapid immuno chromatographic kit MPT64 Ag for the identification of Mycobacterium tuberculosis complex from various Mycobacterium tuberculosis culture positive specimens. Department of Microbiology, Armed Forces Institute of Pathology Rawalpindi, from August 2008 through March 2009. Eighty four Mycobacterium tuberculosis positive cultures on I BACTEC 460 and MGIT 960, one ATCC 25177 MTB strain, three institutional control MTB strains, two institutional control MOTT strains and 20 different bacterial isolates were tested. Tests were performed according to the instructional manual. Out of total 84 tested samples, MPT64 showed positive result in 80 cultures. Only four positive cultures did not display any band on MPT64 kit. These four strains were reconfirmed as Mycobacterium tuberculosis by PCR method. MOTT control strains and all the 20 bacterial isolates were negative for band. The sensitivity and specificity of ICT assay in our study was 95.2% and 100% respectively. Rapid MPT64 Kit is a good diagnostic tool to differentiate between Mycobacterium tuberculosis complex and MOTT with 100% specificity. The technique is simple and can provide prompt information to the clinicians to initiate early and appropriate antituberculosis therapy. (author)

  16. Direct coupling of a liquid chromatograph to a continuous flow hydrogen nuclear magnetic resonance detector for analysis of petroleum and synthetic fuels

    International Nuclear Information System (INIS)

    Haw, J.F.; Glass, T.E.; Hausler, D.W.; Motell, E.; Dorn, H.C.

    1980-01-01

    Initial results obtained for a flow 1 H nuclear magnetic resonance (NMR) detector directly coupled to a liquid chromatography unit are described. Results achieved for a model mixture and several jet fuel samples are discussed. Chromatographic separation of alkanes, alkylbenzenes, and substituted naphthalenes present in the jet fuel samples are easily identified with the 1 H NMR detector. Results with our present flow 1 H NMR insert indicate that 5-Hz linewidths are readily obtainable for typical chromatographic flow rates. The limitations and advantages of this liquid chromatography detector are compared with more commonly employed detectors (e.g., refractive index detectors). 11 figures

  17. Liquid chromatographic method for simultaneous determination of citalopram with NSAIDs in bulk drug, pharmaceutical formulation and human serum

    International Nuclear Information System (INIS)

    Ali, S.N.; Akram, S.

    2017-01-01

    A high performance liquid chromatographic method was developed and validated to simultaneously quantify citalopram with piroxicam, celecoxib and diclofenac sodium. Chromatographic analysis was performed at ambient temperature using Shimadzu Shim-pack CLC-ODS (M) 25M column linked to a UV-visible detector adjusted at 230 nm, employing 80:20 (v/v) methanol: water (pH 3.5) as mobile phase with flow rate 1.0 mL min-1. Validation was performed in the ranges 0.6-20, 0.9-28, 0.6-20 and 1.0-32 mu g mL-1 with lowest level corresponding to detection limit 16.45, 23.33, 27.66 and 14.44 ng mL-1 respectively. With-in the day precision ranged from 0.14-1.67% and between-day precision from 0.40-1.50%, accuracies were 99.61-100.86%. The analytes were successfully detected without any observable interference in pharmaceutical formulation and human serum samples demonstrating effectiveness of method. (author)

  18. Liquid Chromatographic-Chemometric Techniques for the Simultaneous HPLC Determination of Lansoprazole, Amoxicillin and Clarithromycin in Commercial Preparation.

    Science.gov (United States)

    Aktas, A Hakan; Saridag, Ayse Mine

    2017-09-01

    Two multivariate calibration-prediction techniques, principal component regression (PCR) and partial least-squares regression (PLSR) were applied to the chromatographic multicomponent analysis of the drug containing lansoprazole (LAN), clarithromycin (CLA) and amoxicillin (AMO). Optimum chromatographic separation of LAN, CLA and AMO with atorvastatin as the internal standard (IS) was obtained by using Xterra® RP18 column 5 μm 4.6 × 250 mm2, and 25 mM ammonium chloride buffer prepared ammonium chloride, acetonitrile and bidistilled water (45:45:10 v/v) as the mobile phase at flow rate 1.0 mL/min. The high pressure liquid chromatography data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using diode array detector detection at five wavelengths (205, 210, 215, 220 and 225 nm). LC-chemometric calibration for LAN, CLA and AMO were separately constructed by using the relationship between the peak-area ratio and training sets for each analyte. A series of synthetic solutions containing different concentrations of LAN, CLA and AMO were used to check the prediction ability of the PCR and PLS. Both of the two-chemometric methods in this study can be satisfactorily used for the quantitative analysis and for dissolutions tests of multicomponent commercial drug. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. An innovative, simple, fast, and less toxic high-performance liquid chromatographic method for determination of prednisone in capsules

    Directory of Open Access Journals (Sweden)

    Pedro Henrique Reis da Silva

    2017-06-01

    Full Text Available ABSTRACT Prednisone is an anti-inflammatory steroid drug widely used in clinical practice. However, no high-performance liquid chromatographic (HPLC method has been described in the literature for the determination of prednisone in capsules until now. Thus, an HPLC method was developed using a C18 (250x4.0, 5 µm column, with methanol:water (70:30 as mobile phase at a flow rate of 1 mL/min and detection at 240 nm. The developed method was validated following current Brazilian legislation. Additionally, linearity was assessed by evaluating the assumptions of normality, homoscedasticity, and independency of residuals, and the fit to the linear model. The method showed linearity (r2>0.99 over the range of 14.0-26.0 µg/mL, selectivity, precision (RSD<2.0%, robustness, and accuracy (average recovery of 100.05%. The chromatographic procedure was applied for assay and uniformity content determination of three different batches of prednisone capsules, showing to be suitable for their quality control.

  20. A high performance liquid chromatographic assay of Mefloquine in saliva after a single oral dose in healthy adult Africans

    Directory of Open Access Journals (Sweden)

    Gbotosho Grace O

    2012-02-01

    Full Text Available Abstract Background Mefloquine-artesunate is a formulation of artemisinin based combination therapy (ACT recommended by the World Health Organization and historically the first ACT used clinically. The use of ACT demands constant monitoring of therapeutic efficacies and drug levels, in order to ensure that optimum drug exposure is achieved and detect reduced susceptibility to these drugs. Quantification of anti-malarial drugs in biological fluids other than blood would provide a more readily applicable method of therapeutic drug monitoring in developing endemic countries. Efforts in this study were devoted to the development of a simple, field applicable, non-invasive method for assay of mefloquine in saliva. Methods A high performance liquid chromatographic method with UV detection at 220 nm for assaying mefloquine in saliva was developed and validated by comparing mefloquine concentrations in saliva and plasma samples from four healthy volunteers who received single oral dose of mefloquine. Verapamil was used as internal standard. Chromatographic separation was achieved using a Hypersil ODS column. Results Extraction recoveries of mefloquine in plasma or saliva were 76-86% or 83-93% respectively. Limit of quantification of mefloquine was 20 ng/ml. Agreement between salivary and plasma mefloquine concentrations was satisfactory (r = 0.88, p Conclusion Disposition of mefloquine in saliva paralleled that in plasma, making salivary quantification of mefloquine potentially useful in therapeutic drug monitoring.

  1. Simultaneous determination of piracetam and vincamine by spectrophotometric and high-performance liquid chromatographic methods.

    Science.gov (United States)

    El-Saharty, Yasser Shaker Ibrahim

    2008-01-01

    A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 10-45 and 2-14 microg/mL with mean recoveries of 99.22 +/- 0.72 and 99.67 +/- 0.79%, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 5-45 and 2-14 microg/mL, with mean recoveries of 100.33 +/- 0.54 and 100.44 +/- 0.98% for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphate-methanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5-100 and 2-200 microg/mL, with mean recoveries of 99.62 +/- 0.67 and 99.32 +/- 0.85% for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

  2. Development of liquid chromatographic methods for the determination of phytosterols in Standard Reference Materials containing saw palmetto.

    Science.gov (United States)

    Bedner, Mary; Schantz, Michele M; Sander, Lane C; Sharpless, Katherine E

    2008-05-23

    Liquid chromatographic (LC) methods using atmospheric pressure chemical ionization/mass spectrometric (APCI-MS) detection were developed for the separation and analysis of the phytosterols campesterol, cycloartenol, lupenone, lupeol, beta-sitosterol, and stigmasterol. Brassicasterol and cholesterol were also included for investigation as internal standards. The methods were used to identify and quantify the phytosterols in each of two Serenoa repens (saw palmetto) Standard Reference Materials (SRMs) developed by the National Institute of Standards and Technology (NIST). Values obtained by LC-MS were compared to those obtained using the more traditional approach of gas chromatography with flame ionization detection. This is the first reported use of LC-MS to determine phytosterols in saw palmetto dietary supplement materials.

  3. Development and validation of high-perfomance liquid chromatographic method for determination of ofloxacin and lomefloxacin in human plasma

    Directory of Open Access Journals (Sweden)

    DRAGICA ZENDELOVSKA

    2005-12-01

    Full Text Available Ahigh-performance liquid chromatographicmethod for the determination of ofloxacin and lomefloxacin in human plasma has been developed and validated. The effect of organic modifiers on the retention of the investigated drugs was investigated. Asimple isocratic chromatographic assay with UV-detection at 280 nm was performed on a Hibar Lichrospher 100 RP 8 column (250×4.6 mm, 5 mm. Merck, Germany using a mixture of acetonitrile and 0.5 % triethylamine in water (pH adjusted to 2.5 with H3PO4 (15:85, V/V as the mobile phase at flow rate of 1.2 mL min-1. The calibration curves were linear in the concentration ragne of 0.5 – 6.0 mg mL-1 for ofloxacin and 0.2-4.5 mg mL-1 for lomefloxacin.

  4. General and selective isolation procedure for high-performance liquid chromatographic determination of anabolic steroids in tissues.

    Science.gov (United States)

    Laganà, A; Marino, A

    1991-12-27

    A multi-residue method has been developed for the determination of anabolic steroids in animal tissue. The analytes are extracted from tissue with methanol and the extract is subjected to two solid-phase extractions, one using a non-specific adsorbing material, such as graphitized carbon black (Carbopack B), and the other Amberlite CG-400 I in the OH form. This procedure allowed the neutral anabolics (testosterone, trenbolone and progesterone) to be isolated and separated from the acidic type (phenolic group), such as diethylstilbestrol, oestradiol, zeranol/zearalenone and their respective metabolites. The determination was effected using high-performance liquid chromatography with different detectors (ultraviolet, fluorimetric and electrochemical). Several analytical parameters were studied: chromatographic conditions, recoveries, evaporation step, solvent flow-rate, cartridges reusability, interference of plastic cartridges. For all the anabolics investigated the recoveries were greater than 83.6%.

  5. High performance liquid chromatographic determination of vanadium in crude oils and cobalt and iron in pharmaceutical preparations

    International Nuclear Information System (INIS)

    Khuhawar, M.Y.; Lanjwani, S.N.; Khaskhely, G.Q.

    1993-01-01

    High performance liquid Chromatographic (HPLC) method has ben developed for the determination of vanadium in crude oils, based on acid decomposition of oils, followed by complexation with bis (salicylaldehyde) tetramethyl ethylenediamine (H2SA2Ten). The complex is extracted in organic phase and is separated from copper and nickel using normal phase HPLC column. Detection is achieved using spectrophtmetric detector. The vanadium in oil is obtained at sub microgram/g level. Similarly cobalt(II), cobalt(III) and iron(II) are separated on reversed phase HPLC column. Pre column derivatization is used to develop HPLC method for the determination of cobalt and iron in pharmaceutical preparations. Finally results are compared using atomic absorption spectrometer. (author)

  6. High performance liquid chromatographic hydrocarbon group-type analyses of mid-distillates employing fuel-derived fractions as standards

    Science.gov (United States)

    Seng, G. T.; Otterson, D. A.

    1983-01-01

    Two high performance liquid chromatographic (HPLC) methods have been developed for the determination of saturates, olefins and aromatics in petroleum and shale derived mid-distillate fuels. In one method the fuel to be analyzed is reacted with sulfuric acid, to remove a substantial portion of the aromatics, which provides a reacted fuel fraction for use in group type quantitation. The second involves the removal of a substantial portion of the saturates fraction from the HPLC system to permit the determination of olefin concentrations as low as 0.3 volume percent, and to improve the accuracy and precision of olefins determinations. Each method was evaluated using model compound mixtures and real fuel samples.

  7. A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jian; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu, Min [Hubei Instrument for Food and Drug Control, Wuhan (China)

    2015-08-15

    Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc.

  8. A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances

    International Nuclear Information System (INIS)

    Li, Jian; Xu, Li; Shi, Zhi-guo; Hu, Min

    2015-01-01

    Highlights: • A novel two-dimensional liquid chromatographic system was developed. • The 1st dimension was ODS to separate components in the sample. • The 2nd dimension was biopartitioning micellar chromatography to predict toxicity. • The system was used to screen toxicity of pharmaceuticals and related substances. • It was promising for fast online toxicity screening of complex sample in one step. - Abstract: In this study, a novel two-dimensional liquid chromatographic (2D-LC) system was developed for simultaneous separation and toxicity prediction of pharmaceutical and its related substances. A conventional ODS column was used on the 1st-D to separate the sample; while, bio-partitioning micellar chromatography served as the 2nd-D to predict toxicity of the components. The established system was tested for the toxicity of ibuprofen and its impurities with known toxicity. With only one injection, ibuprofen and its impurities were separated on the 1st-D; and LC50 values of individual impurity were obtained based on the quantitative retention–activity relationships, which agreed well with the reported data. Furthermore, LC50 values of photolysis transformation products (TPs) of carprofen, ketoprofen and diclofenac acid (as unknown compounds) were screened in this 2D-LC system, which could be an indicator of the toxicity of these TPs and was meaningful for the environmental monitoring and drinking water treatment. The established 2D-LC system was cost-effective, time-saving and reliable, and was promising for fast online screening of toxicity of known and unknown analytes in the complex sample in a single step. It may find applications in environment, pharmaceutical and food, etc

  9. Further Validation of a Rapid Screening Semiquantitative Thin-Layer Chromatographic Method for Marketed Antimalarial Medicines for Adoption in Malawi

    Directory of Open Access Journals (Sweden)

    Dorcas Osei-Safo

    2018-01-01

    Full Text Available A recently developed semiquantitative thin-layer chromatographic (SQ-TLC assay has been employed in postmarketing surveillance of antimalarial medicines used in Malawi prior to HPLC assay. Both methods gave analogous results in a significant majority of the samples, with a good correlation (r = 0.9012 for the active pharmaceutical ingredients of the dosage forms assayed. Artemether-containing medicines had the highest percentage (92.67% of samples with comparable results for both assays. The lowest percentage (66.67% was observed in artesunate-containing medicines. The SQ-TLC method was validated for specificity, accuracy, precision, linearity, and stability according to the International Conference on Harmonisation guidelines, with the results falling within acceptable limits. For specificity, retention factor values of the test samples and reference standards were comparable, while accuracy and precision of 91.1 ± 5.7% were obtained for all samples. The method was linear in the range 1.0–2.0 µg/spot with a correlation coefficient of r = 0.9783. Stability tests also fell within acceptable limits. In this study, we present the validation of the SQ-TLC method and propose its adoption as a rapid screening tool for field estimation of the quality of antimalarial and other essential medicines in Malawi and other parts of the developing world prior to a more accurate HPLC assay.

  10. Optimization of the reversed-phase high-performance liquid chromatographic separation of synthetic estrogenic and progestogenic steroids using the multi-criteria decision making method

    NARCIS (Netherlands)

    Smilde, A. K.; Bruins, C. H.; Doornbos, D. A.; Vink, J.

    1987-01-01

    The optimization of the reversed-phase high-performance liquid chromatographic separation of a mixture of ethynylestradiol, desogestrel and three related compounds is described. A procedure is used that allows the prediction of the capacity factors of each individual synthetic steroid, depending on

  11. INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

    Science.gov (United States)

    A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

  12. HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC PROFILING OF TRYPTOPHAN AND RELATED INDOLES IN BODY-FLUIDS AND TISSUES OF CARCINOID PATIENTS

    NARCIS (Netherlands)

    KEMA, IP; SCHELLINGS, AMJ; HOPPENBROUWERS, CJM; RUTGERS, HM; DEVRIES, EGE; MUSKIET, FAJ

    1993-01-01

    A high performance liquid chromatographic method with quaternary gradient elution and fluorometric detection was developed for profiling of tryptophan (TRP), 5-hydroxytryptophan, serotonin (5-HT) and 5-hydroxyindole-3-acetic acid (5-HIAA) in urine, platelet-rich plasma and (tumour) tissue of

  13. Sample preparation for large-scale bioanalytical studies based on liquid chromatographic techniques.

    Science.gov (United States)

    Medvedovici, Andrei; Bacalum, Elena; David, Victor

    2018-01-01

    Quality of the analytical data obtained for large-scale and long term bioanalytical studies based on liquid chromatography depends on a number of experimental factors including the choice of sample preparation method. This review discusses this tedious part of bioanalytical studies, applied to large-scale samples and using liquid chromatography coupled with different detector types as core analytical technique. The main sample preparation methods included in this paper are protein precipitation, liquid-liquid extraction, solid-phase extraction, derivatization and their versions. They are discussed by analytical performances, fields of applications, advantages and disadvantages. The cited literature covers mainly the analytical achievements during the last decade, although several previous papers became more valuable in time and they are included in this review. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Rapid chromatographic determination of caseins in milk with photometric and fluorimetric detection using a hydrophobic monolithic column.

    Science.gov (United States)

    Ramírez-Palomino, P; Fernández-Romero, J M; Gómez-Hens, A

    2014-01-01

    Reverse-phase liquid chromatographic methods using a hydrophobic C18 monolithic column and on-line photometric and fluorimetric detection for the determination of the major casein (CN) proteins in milk are presented. The separation of αs1-CN, αs2-CN, β-CN and κ-CN was achieved in only five minutes. Fluorimetric detection enabled better analytical results than photometric detection. Thus, the dynamic ranges of the calibration graphs and detection limits obtained using fluorimetric detection were (mgmL(-)(1)): αs1-CN (0.74-10.0, 0.22), αs2-CN (0.15-10.0, 0.045), β-CN (0.68-10.0, 0.20) and κ-CN (0.21-10.0, 0.06). The analytical features of the photometric method, which does not allow the quantification of β-casein, were (mgmL(-)(1)): αs1-CN (1.5-9.0, 0.45), αs2-CN (1.4-10.0, 0.43) and κ-CN (0.4-9.0, 0.12). Precision data, expressed as relative standard deviation, ranged between 0.6% and 5.3% for the fluorimetric method and between 2.4% and 6.2% for the photometric method. Both methods were applied to the analysis of three different milk samples, obtaining recoveries in the ranges of 86.6-103.2% and 92.0-106.5% using fluorimetric and photometric detection, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Stability-indicating liquid Chromatographic assaymethod for Opthalmic solutions containing combination of Dexamethasone and Chloramphenicol

    International Nuclear Information System (INIS)

    Rao, R.M.; Al-Ashban, R.M.; Shah, A.H.

    2004-01-01

    A selective high-performance chromatographic procedure for the stability monitoring of ophthalmic solutions containing a combination of dexamethasone and chloramphenicolis demonstrated. The separation of the active components and the degradation product of chloramphenicol (1-amino-1-(4-nitrophenyl)-propane-1, 3diol) was achieved on a u-Bondapack C-18 column ( 5 um, 300 mm x 3.9 mm) maintained at ambient temperature (15-20C) by utilizing a mobile phase consisting acidified water (5% actified water with glacial acetic acid ) : acetonitrile : triethyl amine 700 : 300 : 2and pH was adjusted to 5.0 by using 10 M Na OH. The flow rate was 1.5 ml min-1; and elutes were followed with UV-detection at 254 nm. Complete resolution of dexamethasone, chloramphenicol and its hydrolytic product could be attained. The sensitivity, accuracy and specificity were tested. The method was successfully applied in post-marketing stability of the commercial batches of ophthalmic solutions. (author)

  16. High Performance Liquid Chromatographic Analysis of Almotriptan Malate in Bulk and Tablets

    Directory of Open Access Journals (Sweden)

    Chandra Bala Sekaran

    2013-02-01

    Full Text Available Purpose: A simple RP-HPLC method has been developed and validated for the determination of almotriptan malate (ATM in bulk and tablets. Methods: Chromatographic separation of ATM was achieved by using a Thermo Scientific C18 column. A Mobile phase containing a mixture of methanol, water and acetic acid (4:8:0.1 v/v was pumped at the flow rate of 1 mL/min. Detection was performed at 227 nm. According to ICH guidelines, the method was validated. Results: The calibration curve was linear in the concentration range 5–60 μg/mL for the ATM with regression coefficient 0.9999. The method was precise with RSD <1.2%. Excellent recoveries of 99.60 - 100.80% proved the accuracy of the method. The limits of detection and quantification were found to be 0.025 and 0.075 μg/mL, respectively. Conclusion: The method was successfully applied for the quantification of ATM in tablets with acceptable accuracy and precision.

  17. Simple fluorimetric liquid chromatographic method for the analysis of undecylenic acid and zinc undecylenate in pharmaceutical preparations.

    Science.gov (United States)

    Lin, Ming-Chun; Wu, Hsin-Lung; Kou, Hwang-Shang; Wu, Shou-Mei

    2006-06-30

    A simple and selective liquid chromatographic method is described for the analysis of undecylenic acid (UA) and zinc undecylenate (ZnUA) in pharmaceutical preparations. The method is based on the derivatization of the analytes extracted from various samples with 2-(2-naphthoxy)ethyl 2-(piperidino)ethanesulfonate. The resulting derivative was analyzed by liquid chromatography with fluorimetric detection. The quantitation of the method is in the range of 3.0-50.0 microM UA with a detection limit of about 0.3 microM (S/N = 3 with 10 microl injection). We found that acetonitrile is a selective solvent for differentially dissolving UA from coexisted ZnUA in compound formulation. This results in the specific analysis of UA in the presence of ZnUA and simply analyzing the coexisted ZnUA by the value of total UA (UA+ZnUA) minus that of UA. Application of the method to the analysis of undecylenic acid and zinc undecylenate in ointment, powder and solution preparations proved feasible.

  18. Evaluation of highly polar ionic liquid gas chromatographic column for the determination of the fatty acids in milk fat.

    Science.gov (United States)

    Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Kramer, John K G; Mossoba, Magdi M; Sidisky, Len; Tyburczy, Cynthia; Rader, Jeanne I

    2012-04-13

    The SLB-IL111, a new ionic liquid capillary column for gas chromatography available from Supelco Inc., was recently shown to provide enhanced separation of unsaturated geometric and positional isomers of fatty acid (FAs) when it was compared to cyanopropylsiloxane (CPS) columns currently recommended for the analysis of fatty acid methyl esters (FAMEs). A 200 m SLB-IL111 capillary column, operated under a combined temperature and eluent flow gradient, was successfully used to resolve most of the FAs contained in milk fat in a single 80 min chromatographic separation. The selected chromatographic conditions provided a balanced, simultaneous separation of short-chain (from 4:0), long-chain polyunsaturated fatty acids (PUFAs), and most of the unsaturated FA positional/geometric isomers contained in milk fat. Among the monounsaturated fatty acids (MUFAs), these conditions separated t11-18:1 and t10-18:1 FAs, the two most abundant trans fatty acids (t-FA) contained in most dairy products. These t-FAs reportedly have different biological activities. The conjugated linoleic acid (CLA) isomers commonly found in dairy products were separated from each other, including t7,c9-18:2 from c9,t11-18:2, which eliminated the need for their complementary silver ion HPLC analysis. The application of the SLB-IL111 column provided a complementary elution profile of FAMEs to those obtained by CPS columns, allowing for a more comprehensive FA analysis of total milk fat. The FAMEs were identified by the use of available reference materials, previously synthesized and characterized reference mixtures, and prior separations of the milk fat FAMEs by silver ion chromatography based on the number/geometry of double bonds. Published by Elsevier B.V.

  19. New liquid chromatographic-chemometric approach for the determination of sunset yellow and tartrazine in commercial preparation.

    Science.gov (United States)

    Dinç, Erdal; Aktaş, A Hakan; Ustündağ, Ozgür

    2005-01-01

    A new liquid chromatographic (LC)-chemometric approach was developed for the determination of sunset yellow (SUN) and tartrazine (TAR) in commercial preparations. This approach uses LC and chemometric calibration methods, i.e., classical least-squares (CLS), principal component regression (PCR), and partial-least squares (PLS), simultaneously. The combined LC-chemometric approaches, denoted as LC-CLS, LC-PCR, and LC-PLS, are based on photodiode array (PDA) detection at multiple wavelengths. Optimum chromatographic separation of SUN and TAR with allura red as the internal standard (IS) was obtained by using a Waters Symmetry C18 column, 5 microm, 4.6 x 250 mm, and 0.2 M acetate buffer (pH 5)-acetonitrile-methano-bidistilled water (55 + 20 + 15 + 10, v/v) as the mobile phase at a flow rate of 1.9 mL/min. The LC data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using PDA detection at 5 wavelengths (465, 470, 475, 480, and 485 nm). LC-chemometric calibrations for SUN and TAR were separately constructed by using the relationship between the peak-area ratio and the training sets for each colorant. LC-chemometric approaches were tested for different synthetic mixtures containing SUN and TAR in the presence of the IS. These LC-chemometric calibrations were applied to a commercial preparation of the 2 colorants. The experimental results of the LC-chemometric approaches were compared with those obtained by a developed classical LC method using single-wavelength detection.

  20. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG

    Directory of Open Access Journals (Sweden)

    Y. Zhang

    2016-11-01

    Full Text Available We present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography–mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes (Zhang et al., 2014. Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arranged into an input data matrix for positive matrix factorization (PMF, where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS, TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level

  1. Liquid-phase microextraction for simultaneous chromatographic analysis of three antidepressant drugs in plasma

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Dobrovolskni Porto

    2012-01-01

    Full Text Available A method using Liquid Phase Microextraction for simultaneous detection of citalopram (CIT, paroxetine (PAR and fluoxetine (FLU, using venlafaxine as internal standard, in plasma by high performance liquid chromatography with fluorescence detection was developed. The linearity was evaluated between 5.0 and 500 ng mL-1 (r > 0.99 and the limit of quantification was 2.0, 3.0 and 5.0 ng mL-1 for CIT, PAR and FLU, respectively. Therefore, it can be applied to therapeutic drug monitoring, pharmacokinetics or bioavailability studies and its advantages are that it necessary relatively inexpensive equipment and sample preparation techniques.

  2. Validation of a high-performance liquid chromatographic method with UV detection for the determination of ethopabate residues in poultry liver.

    Science.gov (United States)

    Granja, Rodrigo H M M; Niño, Alfredo M Montes; Zucchetti, Roberto A M; Niño, Rosario E Montes; Salerno, Alessandro G

    2008-01-01

    Ethopabate is frequently used in the prophylaxis and treatment of coccidiosis in poultry. Residues of this drug in food present a potential risk to consumers. A simple, rapid, and sensitive column high-performance liquid chromatographic (HPLC) method with UV detection for determination of ethopabate in poultry liver is presented. The drug is extracted with acetonitrile. After evaporation, the residue is dissolved with an acetone-hexane mixture and cleaned up by solid-phase extraction using Florisil columns. The analyte is then eluted with methanol. LC analysis is carried out on a C18 5 microm Gemini column, 15 cm x 4.6 mm. Ethopabate is quantified by means of UV detection at 270 nm. Parameters such as decision limit, detection capability, precision, recovery, ruggedness, and measurement uncertainty were calculated according to method validation guidelines provided in 2002/657/EC and ISO/IEC 17025:2005. Decision limit and detection capability were determined to be 2 and 3 microg/kg, respectively. Average recoveries from poultry samples fortified with 10, 15, and 20 microg/kg levels of ethopabate were 100-105%. A complete statistical analysis was performed on the results obtained, including an estimation of the method uncertainty. The method is to be implemented into Brazil's residue monitoring and control program for ethopabate.

  3. High Speed Liquid Chromatographic Determination of Total Aromatics in Enamel and Lacquer Solvents.

    Science.gov (United States)

    Esposito, G. G.

    Aromatic solvents possess the strongest solvency of the hydrogen types, but various air pollution control districts have established maximum limits on the amount that may be present in organic coatings. In the proposed procedure, high efficiency liquid chromatography is used to determine total aromatics in enamels and lacquer thinners, their…

  4. Liquid chromatographic-tandem mass spectrometric determination of selected sulphonamides in milk

    NARCIS (Netherlands)

    Rhijn, van J.A.; Lasaroms, J.J.P.; Berendsen, B.J.A.; Brinkman, U.A.Th.

    2002-01-01

    Liquid chromatography–tandem mass spectrometry is used for the quantitative analysis of selected sulphonamides in milk. Ultrafiltration is the only sample pre-treatment technique which is required. Consequently, sample throughput is much higher than with conventional procedures, and analyte

  5. Evaluation of the phase ratio for three C18 high performance liquid chromatographic columns.

    Science.gov (United States)

    Caiali, Edvin; David, Victor; Aboul-Enein, Hassan Y; Moldoveanu, Serban C

    2016-02-26

    For a chromatographic column, phase ratio Φ is defined as the ratio between the volume of the stationary phase Vst and the void volume of the column V0, and it is an important parameter characterizing the HPLC process. Although apparently simple, the evaluation of Φ presents difficulties because there is no sharp boundary between the mobile phase and the stationary phase. In addition, the boundary depends not only on the nature of the stationary phase, but also on the composition of the mobile phase. In spite of its importance, phase ratio is seldom reported for commercially available HPLC columns and the data typically provided by the vendors about the columns do not provide key information that would allow the calculation of Φ based on Vst and V0 values. A different procedure for the evaluation of Φ is based on the following formula: log k'j=a log Kow,j+log Φ, where k'j is the retention factor for a compound j that must be a hydrocarbon, Kow,j is the octanol/water partition coefficient, and a is a proportionality constant. Present study describes the experimental evaluation of Φ based on the measurement of k'j for the compounds in the homologous series between benzene and butylbenzene for three C18 columns: Gemini C18, Luna C18 both with 5 μm particles, and a Chromolith Performance RP-18. The evaluation was performed for two mobile phase systems at different proportions of methanol/water and acetonitrile/water. The octanol/water partition coefficients were obtained from the literature. The results obtained in the study provide further support for the new procedure for the evaluation of phase ratio. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Sample preparation for liquid chromatographic analysis of phytochemicals in biological fluids.

    Science.gov (United States)

    Oh, Ju-Hee; Lee, Young-Joo

    2014-01-01

    Natural products have been used traditionally for the treatment and prevention of diseases for thousands of years and are nowadays consumed as dietary supplements and herbal medicine. To ensure the safe and effective use of these herbal products, information about bioavailability of active compounds in plasma or target tissues should be provided via validated analytical methods combined with appropriate sampling methods. To provide comprehensive and abridged information about sample preparation methods for the quantification of phytochemicals in biological samples using liquid chromatography analysis. Sample pre-treatment procedures used in analytical methods for in vivo pharmacokinetic studies of natural compounds or herbal medicines were reviewed. These were categorised according to the biological matrices (plasma, bile, urine, faeces and tissues) and sample clean-up processes (protein precipitation, liquid-liquid extraction and solid-phase extraction). Although various kinds of sample pre-treatment methods have been developed, liquid-liquid extraction is still widely used and solid-phase extraction is becoming increasingly popular because of its efficiency for extensive clean up of complex matrix samples. However, protein precipitation is still favoured due to its simplicity. Sample treatment for phytochemical analysis in biological fluids is an indispensable and critical step to obtain high quality results. This step could dominate the overall analytical process because both the duration of the process as well as the reliability of the data depend in large part on its efficiency. Thus, special attention should be given to the choice of a proper sample treatment method that targets analytes and their biomatrix. Copyright © 2013 John Wiley & Sons, Ltd.

  7. Rapid chromatographic separation of dissoluble Ag(I) and silver-containing nanoparticles of 1-100 nanometer in antibacterial products and environmental waters.

    Science.gov (United States)

    Zhou, Xiao-Xia; Liu, Rui; Liu, Jing-Fu

    2014-12-16

    Sensitive and rapid methods for speciation analysis of nanoparticulate Ag (NAg) and Ag(I) in complex matrices are urgently needed for understanding the environmental effects and biological toxicity of silver nanoparticles (AgNPs). Herein we report the development of a universal liquid chromatography (LC) method for rapid and high resolution separation of dissoluble Ag(I) from nanoparticles covering the entire range of 1-100 nm in 5 min. By using a 500 Å poresize amino column, and an aqueous mobile phase containing 0.1% (v/v) FL-70 (a surfactant) and 2 mM Na2S2O3 at a flow rate of 0.7 mL/min, all the nanoparticles of various species such as Ag and Ag2S were eluted in one fraction, while dissoluble Ag(I) was eluted as a baseline separated peak. The dissoluble Ag(I) was quantified by the online coupled ICP-MS with a detection limit of 0.019 μg/L. The NAg was quantified by subtracting the dissoluble Ag(I) from the total Ag content, which was determined by ICP-MS after digestion of the sample without LC separation. While the addition of FL-70 and Na2S2O3 into the mobile phase is essential to elute NAg and Ag(I) from the column, the use of 500 Å poresize column is the key to baseline separation of Ag(I) from ∼ 1 nm AgNPs. The feasibility of the proposed method was demonstrated in speciation analysis of dissoluble Ag(I) and NAg in antibacterial products and environmental waters, with very good chromatographic repeatability (relative standard deviations) in both peak area (<2%) and retention time (<0.6%), excellent spiked recoveries in the range of 84.7-102.7% for Ag(I) and 81.3-106.3% for NAg. Our work offers a novel approach to rapid and baseline separation of dissoluble metal ions from their nanoparticulate counterparts covering the whole range of 1-100 nm.

  8. Rapid, facile synthesis of conjugated polymer zwitterions in ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Page, Zachariah A. [Polymer Science & Engineering Department; Conte Center for Polymer Research; University of Massachusetts; Amherst, USA; Liu, Feng [Polymer Science & Engineering Department; Conte Center for Polymer Research; University of Massachusetts; Amherst, USA; Russell, Thomas P. [Polymer Science & Engineering Department; Conte Center for Polymer Research; University of Massachusetts; Amherst, USA; Emrick, Todd [Polymer Science & Engineering Department; Conte Center for Polymer Research; University of Massachusetts; Amherst, USA

    2014-01-01

    Ionic liquids (ILs) were utilized for the rapid air-stable Suzuki polymerization of polar zwitterionic thiophene monomers, precluding the need for volatile organic solvents, phosphine ligands and phase transfer catalysts typically used in conjugated polymer synthesis.

  9. High-performance Liquid Chromatographic Ultraviolet Detection of Nilotinib in Human Plasma from Patients with Chronic Myelogenous Leukemia, and Comparison with Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Nakahara, Ryosuke; Satho, Yuhki; Itoh, Hiroki

    2016-11-01

    A method for determining nilotinib concentration in human plasma is proposed using high-performance liquid chromatography and ultraviolet detection. Nilotinib and the internal standard dasatinib were separated using a mobile phase of 0.5% Na 2 PO 4 H 2 O (pH 2.5)-acetonitrile-methanol (55:25:20, v/v/v) on a Capcell Pak C18 MG II column (250 × 4.6 mm) at a flow rate of 1.0 ml/min, and ultraviolet measurement at 250 nm. The calibration curve exhibited linearity over the nilotinib concentration range of 50-2,500 ng/ml at 250 nm, with relative standard deviations (n = 5) of 7.1%, 2.5%, and 2.9% for 250, 1,500, and 2,500 ng/ml, respectively. The detection limit for nilotinib was 5 ng/ml due to three blank determinations (ρ = 3). This method was successfully applied to assaying nilotinib in human plasma samples from patients with chronic myelogenous leukemia. In addition, we compared the results with those measured by liquid chromatography-tandem mass spectrometry (LC-MS/MS) at BML, Inc. (a commercial laboratory). A strong correlation was observed between the nilotinib concentrations measured by our high-performance liquid chromatographic method and those obtained by LC/MS-MS (r 2 = 0.988, P < 0.01). © 2016 Wiley Periodicals, Inc.

  10. Extraction chromatographic separation of iron from complex liquid samples and the determination of 55Fe

    International Nuclear Information System (INIS)

    Grahek, Z.; Rozmaric Macefat, M.

    2006-01-01

    Iron separation is described from liquid samples with a high concentration of ions that enables simple determination of 55 Fe. One of the described methods consists of iron precipitation from a large volume seawater by sodium hydroxide and/or ammonium carbonate and separation from other elements (Ca, Sr, Cu, Mg, etc.) on a TRU column with 4M HCl or 8M HNO 3 . In the other procedure iron is separated directly from a mixture of seawater samples and HCl on a TRU column. In both methods, the iron recovery is almost 100%. After separation, 55 Fe is determined by counting with a liquid scintillation counter. The binding of Fe and Zn on TEVA, U/TEVA and TRU resins from seawater solutions of HCl and HNO 3 depends on the type of the resin, concentration of acid and other ions. Iron and zinc can be separated from seawater on a U/TEVA column with 2M HCl. (author)

  11. High performance liquid chromatographic determination of Ginseng saponin by ultraviolet derivatisation

    International Nuclear Information System (INIS)

    Besso, H.; Saruwatari, Y.; Futamura, K.; Kunihiro, K.; Fuwa, T.; Tanaka, O.

    1979-01-01

    Ginsenoides Rb 1 , b 2 , c, d, e and g 1 quantitatively reacted with benzoyl chloride in pyridine to afford the respective derivatives having strong UV absorption. The UV-derivatized saponins were separated by high performance liquid chromatography (HPLC), and the saponin-contents of the various Ginseng varieties were determined. It is possible to distinguish white Ginseng from the root hairs of Ginseng by the pattern analysis of HPLC. (orig.) [de

  12. High-performance liquid chromatographic method for the determination of dansyl-polyamines

    Science.gov (United States)

    Subhash C. Minocha; Rakesh Minocha; Cheryl A. Robie

    1990-01-01

    This paper describes a fast reliable, and a sensitive technique for the separation and quantification of dansylated polyamines by high-performance liquid chromatography. Using a small 33 x 4.6 mm I.D., 3 ?m particle size, C18 reversed-phase cartridge column and a linear gradient of acetonitrile-heptanesulfonate (10 mM, pH 3.4...

  13. New Liquid Phases for the Gas Chromatographic Separation of Strong Bases on Capillary Columns

    OpenAIRE

    Grob, K.

    2017-01-01

    The current practice of pretreating the solid support with free alkali to increase separation efficiency for basic compounds proved to be unsuitable for capillary columns. Instead of this, homogenous organic materials of high base strength are required. We found polyethylene imine (PEI) and polypropylene imine (PPI) to be very efficient as liquid phases of capillary columns for the separation of bases. The preparation of polymers is mentioned. Silanization or acetylation of the free hydroxyl ...

  14. Chromatographic separations of stereoisomers

    Energy Technology Data Exchange (ETDEWEB)

    Souter, R.W.

    1985-01-01

    This text covers both diastereomers and enantiomers; describes techniques for GC, HPLC, and other chromatographic methods; and tabulates results of various applications by both techniques and compound class. It provides current knowledge about separation mechanisms and interactions of asymmetric molecules, as well as experimental and commercial materials such as columns, instruments, and derivatization reagents. The contents also include stereoisomer separations by gas chromatography. Stereoisomer separations by high-performance liquid chromatography. Stereoisomer separations by other chromatographic techniques.

  15. Correlation of liquid chromatographic and biological assay for potency assessment of filgrastim and related impurities.

    Science.gov (United States)

    Skrlin, Ana; Kosor Krnic, Ela; Gosak, Darko; Prester, Berislav; Mrsa, Vladimir; Vuletic, Marko; Runac, Domagoj

    2010-11-02

    In vivo and in vitro potency assays have always been a critical tool for confirmation of protein activity. However, due to their complexity and time consuming procedures, it remains a challenge to find an alternative analytical approach that would enable their replacement with no impact on the quality of provided information. The goal of this research was to determine if a correlation between liquid chromatography assays and in vitro biological assay could be established for filgrastim (recombinant human granulocyte-colony stimulating factor, rhG-CSF) samples containing various amounts of related impurities. For that purpose, relevant filgrastim related impurities were purified to homogeneity and characterized by liquid chromatography and mass spectrometry. A significant correlation (R(2)>0.90) between the two types of assays was revealed. Potency of oxidized filgrastim was determined to be approximately 25% of filgrastim stated potency (1 x 10(8)IU/mg of protein). Formyl-methionine filgrastim had potency of 89% of the filgrastim stated potency, while filgrastim dimer had 67% of filgrastim stated potency. A mathematical model for the estimation of biological activity of filgrastim samples from chromatography data was established and a significant correlation between experimental potency values and potency values estimated by the mathematical model was obtained (R(2)=0.92). Based on these results a conclusion was made that reversed phase high performance liquid chromatography could be used as an alternative for the in vitro biological assay for potency assessment of filgrastim samples. Such an alternative model would enable substitution of a complex and time consuming biological assay with a robust and precise instrumental method in many practical cases. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  16. Determination of Diffusion Coefficients and Activation Energy of Selected Organic Liquids using Reversed-Flow Gas Chromatographic Technique

    International Nuclear Information System (INIS)

    Khalisanni Khalid; Rashid Atta Khan; Sharifuddin Mohd Zain

    2012-01-01

    Evaporation of vaporize organic liquid has ecological consequences when the compounds are introduced into both freshwater and marine environments through industrial effluents, or introduced directly into the air from industrial unit processes such as bioreactors and cooling towers. In such cases, a rapid and simple method are needed to measure physicochemical properties of the organic liquids. The Reversed-Flow Gas Chromatography (RF-GC) sampling technique is an easy, fast and accurate procedure. It was used to measure the diffusion coefficients of vapors from liquid into a carrier gas and at the same time to determine the rate coefficients for the evaporation of the respective liquid. The mathematical expression describing the elution curves of the samples peaks was derived and used to calculate the respective parameters for the selected liquid pollutants selected such as methanol, ethanol, 1-propanol, 1-butanol, n-pentane, n-hexane, n-heptane and n-hexadecane, evaporating into the carrier gas of nitrogen. The values of diffusion coefficients found were compared with those calculated theoretically or reported in the literature. The values of evaporation rate were used to determine the activation energy of respective samples using Arrhenius equation. An interesting finding of this work is by using an alternative mathematical analysis based on equilibrium at the liquid-gas interphase, the comparison leads to profound agreement between theoretical values of diffusion coefficients and experimental evidence. (author)

  17. Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

    Science.gov (United States)

    Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2015-05-01

    Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Ultra-performance liquid chromatographic determination of L-ergothioneine in commercially available classes of cow milk.

    Science.gov (United States)

    Sotgia, Salvatore; Pisanu, Elisabetta; Cambedda, Debora; Pintus, Gianfranco; Carru, Ciriaco; Zinellu, Angelo

    2014-09-01

    A new efficient and sensitive precolumn hydrophilic interaction ultra-performance liquid chromatography (HILIC-UPLC) method was established for the quantitative determination of L-ergothioneine (ERT) in milk. After derivatization of ERT with 7-diethylamino-3-[4-(iodoacetamido)phenyl]-4-methylcoumarin, chromatographic separation was achieved in a fairly short time, less than 5 min, on a 100 × 2.1 mm Waters Cortecs UPLC HILIC 1.6-μm column, by using a mixture of 30 mmol/L ammonium acetate/acetonitrile (10:90, v/v) as a mobile phase flowing isocratically at 0.9 mL/min. Limit of detection and the limit of quantification were 0.03 and 0.10 μmol/L, respectively. The method exhibited linearity in a concentration range of 0.16 and 5.08 μmol/L. Mean recovery was 106.66%, whereas intra- and interassay precisions were determined to be within 6 RSD%. On average, ERT concentration in different commercially available classes of cow milk was found to be 0.442 ± 0.191 μmol/L, with the highest levels in the ultra-high temperature milks and low values in the unprocessed and HTST whole milks. In this light, our experiments suggest that ERT could be used as a marker for the heat treatment of milk. © 2014 Institute of Food Technologists®

  19. Reversed-phase liquid chromatographic profile of free amino acids in strawberry-tree (Arbutus unedo L.) honey.

    Science.gov (United States)

    Spano, Nadia; Piras, Irene; Ciulu, Marco; Floris, Ignazio; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino

    2009-01-01

    The typical profile of the free amino acids contained in strawberry-tree (Arbutus unedo L.) honey is reported for the first time. An optimized reversed-phase liquid chromatographic (RP-LC) method with phenyl isothiocyanate precolumn derivatization was used. Fourteen free amino acids were identified and quantified in 16 analytical samples. Proline (65.63%) was found to be the most abundant free amino acid, followed by glutamic acid (6.49%), arginine (5.21%), alanine (5.17%), and phenylalanine (4.97%). The total free amino acid content of strawberry-tree honey (average value, 436 mg/kg) was found to be low in comparison to amounts cited in the literature concerning unifloral honeys. The analytical method was optimized and fully validated in terms of detection and quantitation limits, precision (by testing repeatability and reproducibility), linearity, and bias (by means of recovery tests). The acceptability of the validation protocol results was verified using Horwitz's mathematical model and AOAC guidelines.

  20. Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

    Science.gov (United States)

    Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

    2016-06-05

    This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Forensic Analysis of Blue Ball point Pen Inks Using Ultraviolet-Visible Spectrometer and Ultra-Performance Liquid Chromatograph

    International Nuclear Information System (INIS)

    Lee, L.C.; Shandu, K.T.S.; Nor Syahirah Mohamad Razi; Ab Aziz Ishak; Khairul Osman

    2015-01-01

    Twelve varieties of blue ball point pens were selected and analyzed using UV-Vis spectrometer and ultra-performance liquid chromatography (UPLC). The aim of the study was to determine discrimination power (DP) of these methods in differentiating pen inks collected from the market in Malaysia. Discrimination analysis of 66 possible pen-pair of blue ball point pens was carried out via one-way ANOVA based on obtained chromatogram and spectra. A total of 18 peaks were determined as coming from inks based on the chromatographic data extracted at three different wavelengths (279, 370 and 400 nm). While for the UV-Vis spectrometer analysis, presence of peaks at 303, 545, 577 and 584 nm wavelengths were recorded. UV-Vis spectral data were mainly produced by the colorant components (for example, dyes) found in inks and UPLC may detect ink components other than dyes, for example, additives. As conclusion, the DP for UV-Vis and UPLC were determined to be 72.12 % and 98.48 %, respectively. This manuscript demonstrates the potential of UPLC for discriminating pen inks based on non-dye components. Additionally, the dye components in inks do not seem to play important role in discrimination of pen inks. (author)

  2. Stability-indicating liquid chromatographic method for quantification of new anti-epileptic drug lacosamide in bulk and pharmaceutical formulation

    Directory of Open Access Journals (Sweden)

    Chhalotiya Usmangani K.

    2012-01-01

    Full Text Available An isocratic stability indicating reversed-phase liquid chromatographic determination was developed for the quantitative determination of lacosamide in the pharmaceutical dosage form. A Hypersil C-18, 4.5μm column with mobile phase containing acetonitrile-water (20:80, v/v was used. The flow rate was 1.0 mL min-1 and effluents were monitored at 258 nm. The retention time of lacosamide was 8.9 min. The method was found to be linear in the concentration range of 5-100 μg/ml and the recovery was found to be in the range of 99.15 - 100.09 %. The limit of detection and limit of quantification were found to be 2 μg/ml and 5 μg/ml, respectively. Lacosamide stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and dry heat degradation. The drug was found to be stable to the dry heat and acidic condition attempted. The proposed method was validated and successfully applied to the estimation of lacosamide in tablet dosage forms.

  3. Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

    Science.gov (United States)

    Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

    2013-03-05

    A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. High-performance liquid chromatographic assay for two rifamycin-derived hypocholesterolemic agents in liver and biological fluids.

    Science.gov (United States)

    Moore, D J; Perrino, P J; Klerer, C P; Robertson, P

    1993-02-26

    CGP 43371 (compound I), a mono-pivaloyl oxazole derivative of a 3-piperazino-rifamycin, has been in clinical trials as a potential hypocholesterolemic agent. A reversed-phase high-performance liquid chromatographic (HPLC) assay was developed using a C18 column and a gradient solvent system of methanol-0.1 M sodium acetate, pH 4.5, at a flow-rate of 1 ml/min. The compound and internal standard (rifampicin) were detected by their ultraviolet absorption at 254 nm. Isolation of the compounds from plasma and liver homogenates was accomplished by precipitation of proteins with acetonitrile, followed by evaporation under nitrogen and reconstitution in methanol. Bile, lymph and urine were injected onto the HPLC column without pretreatment. Calibration curves were linear (r > 0.999) over the concentration range 0.25-20.0 micrograms/ml. The assay procedure was also applicable to other rifamycin derivatives and was able to distinguish between molecular species containing small differences in functionality.

  5. Multivariate curve-resolution analysis of pesticides in water samples from liquid chromatographic-diode array data.

    Science.gov (United States)

    Maggio, Rubén M; Damiani, Patricia C; Olivieri, Alejandro C

    2011-01-30

    Liquid chromatographic-diode array detection data recorded for aqueous mixtures of 11 pesticides show the combined presence of strongly coeluting peaks, distortions in the time dimension between experimental runs, and the presence of potential interferents not modeled by the calibration phase in certain test samples. Due to the complexity of these phenomena, data were processed by a second-order multivariate algorithm based on multivariate curve resolution and alternating least-squares, which allows one to successfully model both the spectral and retention time behavior for all sample constituents. This led to the accurate quantitation of all analytes in a set of validation samples: aldicarb sulfoxide, oxamyl, aldicarb sulfone, methomyl, 3-hydroxy-carbofuran, aldicarb, propoxur, carbofuran, carbaryl, 1-naphthol and methiocarb. Limits of detection in the range 0.1-2 μg mL(-1) were obtained. Additionally, the second-order advantage for several analytes was achieved in samples containing several uncalibrated interferences. The limits of detection for all analytes were decreased by solid phase pre-concentration to values compatible to those officially recommended, i.e., in the order of 5 ng mL(-1). Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Liquid chromatographic determination of chloramine-T and its primary degradation product, p-toluenesulfonamide, in water

    Science.gov (United States)

    Dawson, Verdel K.; Davis, Ruth A.

    1997-01-01

    N-sodium-N-chloro-rho-toluenesulfonamide (chloramine-T) effectively controls bacterial gill disease (BGD) in cultured fishes, BGD, a common disease of hatchery-reared salmonids, causes more fish losses than any other disease among these species. This study describes a liquid chromatographic (LC) method that is capable of direct, simultaneous analysis of chloramine-T and its primary degradation product, rho-toluenesulfonamide (rho-TSA), in water. The procedure involves reversed-phase (C-18) LC analysis with ion suppression, using 0.01 M phosphate buffer at pH 3. The mobile phase is phosphate buffer-acetonitrile (60 + 40) at 1 mL/min. Both chemicals can be detected with a UV spectrophotometer at 229 nm; the method is linear up to 40 mg, chloramine-T or rho-TSA/L. Mean recoveries were 96.4 +/- 6.1% for water samples fortified with 0.03 mg chloramine-T/L and 95.3 +/- 4.6% for water samples fortified with 0.005 mg rho-TSA/L. Limits of detection without sample enrichment for chloramine-T and rho-TSA are 0.01 mg/L and 0.001 mg/L, respectively.

  7. Radioimmunoassay and liquid-chromatographic analysis for free cortisol in urine compared with isotope dilution-mass spectrometry

    International Nuclear Information System (INIS)

    Lantto, O.

    1982-01-01

    Three different routine methods for analysis for urinary cortisol with those by a highly specific reference method based on isotope dilution-mass spectrometry (I) were compared. A ''high-performance'' liquid-chromatographic method (II) gave the most comparable results (regression coefficient 0.86, intercept 9 nmol/L). For some urines much lower values were obtained by I than by II. Two radioimmunoassay (III) methods, one involving direct assay and one involving extraction, gave less-accurate results (regression coefficients of 1.87 and 1.52 and intercepts of 86 and 12 nmol/L, respectively), although values obtained by III and by I correlated well (r = 0.95-0.99), indicating a relation between the free cortisol and the compounds interfering in III. The apparent accuracy for the extraction method was improved by using as calibration standards urine samples previously assayed by I (regression coefficient 0.90, intercept 6 nmol/L). All four methods investigated showed a statistically significant sex-related difference in 24-h urinary cortisol excretion; evidently such a finding should be a prerequisite in any such method proposed for routine use

  8. Gas-liquid chromatographic determination of aniline metabolites of substituted urea and carbamate herbicides in aqueous solution.

    Science.gov (United States)

    Hargesheimer, E E; Coutts, R T; Pasutto, F M

    1981-07-01

    A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and N-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 mL distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

  9. A simple and rapid chromatographic method to determine unauthorized basic colorants (rhodamine B, auramine O, and pararosaniline) in processed foods.

    Science.gov (United States)

    Tatebe, Chiye; Zhong, Xining; Ohtsuki, Takashi; Kubota, Hiroki; Sato, Kyoko; Akiyama, Hiroshi

    2014-09-01

    A simple and rapid high-performance liquid chromatography (HPLC) method to determine basic colorants such as pararosaniline (PA), auramine O (AO), and rhodamine B (RB) in various processed foods was developed. Linearity of the calibration curves ranged from 0.05 to 50 μg/mL for PA and 0.05-100 μg/mL for AO and RB. The detection and quantification limits (LOD and LOQ) of the basic colorants, which were evaluated as signal-to-noise ratios of 3 for LOD and 10 for LOQ, ranged from 0.0125 to 0.05 and 0.025 to 0.125 μg/g, respectively. The recoveries and relative standard deviations of three basic colorants in six processed foods, namely, chili sauce, curry paste, gochujang (hot pepper paste), tandoori chicken (roasted chicken prepared with yogurt and spices), powder soup, and shrimp powder ranged from 70.2% to 102.8% and 0.8% to 8.0%, respectively. The intraday precision of the recovery test ranged from 1.7% to 4.5%, whereas the interday precision ranged from 3.7% to 7.7%. The reported method has been successfully applied to basic colorant determination in various processed foods such as fat-based food matrices (curry paste and tandoori chicken), chili products (gochujang and chili sauce), and protein-based products (shrimp powder and powder soup). Thin layer chromatography and liquid chromatography/mass spectrometry methods for the determination of basic colorants in processed foods were also developed for rapid analysis and identification, respectively. These methods are very useful for monitoring unauthorized basic colorants in inspection centers or quarantine laboratories in many countries.

  10. Determination of rare earth elements by liquid chromatographic separation using inductively coupled plasma mass spectrometric detection

    International Nuclear Information System (INIS)

    Braverman, D.S.

    1992-01-01

    High-performance liquid chromatography (HPLC) is used to separate the rare earth elements (REEs) prior to detection by inductively coupled plasma mass spectrometry (ICP-MS). The use of HPLC-ICP-MS in series combines the separation power and speed of HPLC with the sensitivity, isotopic selectivity and speed of ICP-MS. The detection limits for the REEs are in the sub-ng ml -1 range and the response is linear over four orders of magnitude. A preliminary comparison of isotope dilution and external standard results for the determination of REEs in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM 1633a) Fly Ash is presented. (author)

  11. Solid-phase extraction and high-performance liquid chromatographic separation of pigments of red wines.

    Science.gov (United States)

    Csiktusnádi Kiss, G A; Forgács, E; Cserháti, T; Candeias, M; Vilas-Boas, L; Bronze, R; Spranger, I

    2000-08-11

    The adsorption and desorption capacities of 11 different solid-phase extraction sorbents were tested for the preconcenration of pigments of various Hungarian red wines. The concentrates were evaluated by multiwavelengh spectrophotometry combined with a spectral mapping technique (SPM) and by reversed-phase high-performance liquid chromatography. The highest (10-fold) concentration of pigments was achieved on octadecylsilica sorbent. It can be used five times without losing adsorption and desorption characteristics. SPM indicated that multiwavelength spectrophotometry can be employed for the differentiation of red wines. Comparison of the chromatograms of pigments with and without preconcentration showed that preconcentration makes possible the separation and detection of pigments present in low concentration in red wines.

  12. Comparison of liquid chromatographic and bioassay procedures for determining depletion of intramuscularly injected tylosin.

    Science.gov (United States)

    Moats, W A; Harris, E W; Steele, N C

    1985-01-01

    Crossbred pigs weighing 80-110 kg were injected intramuscularly in the ham with 8.8 mg/kg tylosin. Animals were slaughtered in groups of 3 at intervals of 4 h, and 1, 2, 4, and 8 days after injection, and samples of blood, injected muscle, uninjected muscle, liver, and kidney were analyzed by liquid chromatography (LC) and by bioassay using Sarcina lutea as the test organism. The LC method was far more sensitive with a detection limit of less than 0.1 ppm, while the detection limit by bioassay was about 0.5 ppm in tissue. Results by bioassay and LC sometimes differed considerably for tissue samples. Residues in all tissues were below the tolerance limit of 0.2 ppm at 24 h, except in the injected muscle in one animal. Residues were not detected in any tissue of any animal at 48 h after treatment.

  13. A narrow open tubular column for high efficiency liquid chromatographic separation.

    Science.gov (United States)

    Chen, Huang; Yang, Yu; Qiao, Zhenzhen; Xiang, Piliang; Ren, Jiangtao; Meng, Yunzhu; Zhang, Kaiqi; Juan Lu, Joann; Liu, Shaorong

    2018-04-30

    We report a great feature of open tubular liquid chromatography when it is run using an extremely narrow (e.g., 2 μm inner diameter) open tubular column: more than 10 million plates per meter can be achieved in less than 10 min and under an elution pressure of ca. 20 bar. The column is coated with octadecylsilane and both isocratic and gradient separations are performed. We reveal a focusing effect that may be used to interpret the efficiency enhancement. We also demonstrate the feasibility of using this technique for separating complex peptide samples. This high-resolution and fast separation technique is promising and can lead to a powerful tool for trace sample analysis.

  14. High-performance liquid chromatographic assay for the determination of Aloe Emodin in mouse plasma.

    Science.gov (United States)

    Zaffaroni, M; Mucignat, C; Pecere, T; Zagotto, G; Frapolli, R; D'Incalci, M; Zucchetti, M

    2003-10-25

    An isocratic high-performance liquid chromatography (HPLC) method was developed and validated to determine Aloe Emodin (AE) in mouse plasma. The analysis required 0.3 ml of plasma and involves extraction with dichloromethane. The HPLC separation was carried out on Symmetry Shield RP18, a mobile phase of methanol-water-acetic acid (65:35:0.2) and fluorescence detection at lambda(ex)=410 nm and lambda(em)=510 nm. The retention time of AE was 11.7 min. The assay was linear from 10 to 1,000 ng/ml (r2 > or = 0.999), showed intra- and inter-day precision within 7.8 and 4.7%, and accuracy of 87.3-105.7%. Detection limit (LOD) and quantification limit (LOQ) were 4.5 and 5 ng/ml, respectively. The method was applied to determine for the first time the pharmacokinetic of AE in mice.

  15. High-Performance Liquid Chromatographic Ultraviolet Determination of Memantine Hydrochloride after In Vitro Transdermal Diffusion Studies

    Directory of Open Access Journals (Sweden)

    Sergio del Rio-Sancho

    2013-01-01

    Full Text Available The purpose of the present work was to validate an accurate and precise high-performance liquid chromatography (HPLC method involving ultraviolet detection for the quantitative analysis of memantine hydrochloride. In order to analyze a molecule with no chromophoric groups that could be detected by a UV/visible detector, it was necessary to extract the drug and to perform a dansylation reaction that enabled the UV/visible detection of the derivatized molecule. Separation was carried out with a 150 mm Kromasil C18 column at room temperature. The detection response, at 218 nm, was found to be linear in the concentration range from 0.5 to 50 μg/mL. The method was validated for specificity, linearity, precision, accuracy, limit of detection, limit of quantification, and robustness. The limit of detection (LOD was 0.144 μg/mL, and the limit of quantification (LOQ was 0.437 μg/mL. The dansylated memantine complex was stable for at least five days in all the conditions evaluated. The potential use of this method has been demonstrated by the quantification of memantine hydrochloride contained in samples from the study of its in vitro transdermal permeation.

  16. High-performance liquid chromatographic quantification of rifampicin in human plasma: method for Therapecutic drug monitoring

    International Nuclear Information System (INIS)

    Sameh, T.; Hanene, E.; Jebali, N.

    2013-01-01

    A high performance liquid chromatography (HPLC) method has been developed that allows quantification of Rifampicin in human plasma. The method is based on the precipitation of proteins in human plasma with methanol. Optimal assay conditions were found with a C18 column and a simple mobile phase consisting of 0.05 M dipotassic hydrogen phosphate buffer and acetonitrile (53/47, V/V) with 0.086 % diethylamin, pH = 4.46. The flow-rate was 0.6 ml /mm and the drug was monitored at 340 nm. Results from the HPLC analyses showed that the assay method is linear in the concentration range of 1-40 micro g/ml, (r2 >0.99). The limit of quantification and limit of detection of Rifampicin were 0.632 micro g/ml and 0.208 micro g/ml, respectively. Intraday and interday coefficient of variation and bias were below 10% for all samples, suggesting good precision and accuracy of the method. Recoveries were greater than 90% in a plasma sample volume of 100 micro l. The method is being successfully applied to therapeutic drug monitoring of Rifapicin in plasma samples of tuberculosis and staphylococcal infections patients. (author)

  17. Rapid-action valve especially for liquid metal

    International Nuclear Information System (INIS)

    Velek, V.; Cejka, J.; Jakl, J.

    1976-01-01

    A rapid-action large-diameter valve and control fitting was designed for cooling circuits of nuclear power plants with fast liquid metal cooled reactors, namely sodium cooled. The design meets the requirements for axial symmetry about the flow axis and secures the equilibrium of hydraulic and hydrodynamic forces observing the uniformity of the thickness of the fitting walls which is a pre-requisite for good resistance to thermal shock. (F.M.)

  18. Calculation of retention time tolerance windows with absolute confidence from shared liquid chromatographic retention data.

    Science.gov (United States)

    Boswell, Paul G; Abate-Pella, Daniel; Hewitt, Joshua T

    2015-09-18

    Compound identification by liquid chromatography-mass spectrometry (LC-MS) is a tedious process, mainly because authentic standards must be run on a user's system to be able to confidently reject a potential identity from its retention time and mass spectral properties. Instead, it would be preferable to use shared retention time/index data to narrow down the identity, but shared data cannot be used to reject candidates with an absolute level of confidence because the data are strongly affected by differences between HPLC systems and experimental conditions. However, a technique called "retention projection" was recently shown to account for many of the differences. In this manuscript, we discuss an approach to calculate appropriate retention time tolerance windows for projected retention times, potentially making it possible to exclude candidates with an absolute level of confidence, without needing to have authentic standards of each candidate on hand. In a range of multi-segment gradients and flow rates run among seven different labs, the new approach calculated tolerance windows that were significantly more appropriate for each retention projection than global tolerance windows calculated for retention projections or linear retention indices. Though there were still some small differences between the labs that evidently were not taken into account, the calculated tolerance windows only needed to be relaxed by 50% to make them appropriate for all labs. Even then, 42% of the tolerance windows calculated in this study without standards were narrower than those required by WADA for positive identification, where standards must be run contemporaneously. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Simultaneous Liquid Chromatographic Determination of 10 Ultra-Violet Filters in Sunscreens.

    Science.gov (United States)

    Wharton, Mary; Geary, Michael; O'Connor, Niamh; Curtin, Laura; Ketcher, Krystal

    2015-09-01

    A rapid HPLC method was developed for the simultaneous determination of 10 UV filters found in sunscreen. The following UV filters were analyzed in this method; 2-phenylbenzimidazole-5-sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl dimethyl 4-aminobenzoic acid, ethylhexyl methoxycinnamate, butyl methoxydibenzoylmethane, ethylhexyl salicylate and homosalate. The method was developed on two columns; a Thermo Hypersil C18 BDS, 3 µm column (4.6 × 100 mm) and a Chromolith RP-18e Monolithic column (4.6 × 100 mm). The same mobile phase of ethanol and 1% acetic acid (70:30, v/v) was employed for both columns. The separation of the 10 UV filters was carried out successfully on both columns; the optimal resolution was obtained on the Thermo Scientific Hypersil column in a time frame of 7 min. An isocratic elution utilizing ethanol and acetic acid (70:30, v/v) at a temperature of 35°C was employed. The method was applied to a number of commercial samples of sunscreen and lotions and was validated according to International Conference on Harmonisation guidelines for selectivity, linearity, accuracy, precision and robustness. A comparison of the performances of both columns was also carried out. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  20. Novel liquid chromatographic assay for the low-level determination of apomorphine in plasma.

    Science.gov (United States)

    Priston, M J; Sewell, G J

    1996-05-31

    A novel HPLC assay which is rapid, reproducible and sensitive has been developed for the analysis of apomorphine in plasma. The assay incorporates boldine as an internal standard, and uses solid-phase extraction on C18 mini-columns for sample clean-up and concentration, so enabling quantitation of apomorphine at 500 pg/ml using fluorescence detection (lambda(ex) 270 nm, lambda(em) 450 nm). The HPLC assay comprised a 25 cm-long Techopak C18 column and a mobile phase of (0.25 M sodium dihydrogen phosphate plus 0.25% heptane sulphonic acid, to pH 3.3 with orthophosphoric acid) containing 30% (v/v) methanol and 0.003% (w/v) EDTA, run at a flow-rate of 1.5 ml/min. Calibration plots prepared in plasma were linear over the range 1-30 ng/ml, (limit of quantitation (LOQ) = 490 pg/ml) with R.S.D. of 0.05% and R.E. of 5.0% at the level of 1 ng/ml. Preliminary pharmacokinetic data from two patients given apomorphine by 12 h subcutaneous infusion (patient A dose = 35 mg and patient B dose = 141 mg) showed apomorphine elimination from plasma to fit a two-compartment model, with initial half-lives of 8.2 and 46.6 min, elimination half-lives of 76.4 and 166.5 min and area under the plasma concentration-time curve (AUC) values of 236 and 405 ng h/ml, respectively.

  1. A New High-Performance Liquid Chromatographic Method for the Determination and Distribution of Linalool in Michelia alba

    Directory of Open Access Journals (Sweden)

    Hua-Bin Li

    2010-07-01

    Full Text Available A new high-performance liquid chromatographic method with photodiode array detection was established for the determination of linalool in the plant Michelia alba. Linalool was extracted from the plant sample with the aid of ultrasound, and was analyzed on a Waters RP C18 column (4.6 × 150 mm, 5 μm using an acetonitrile and water (55:45, v/v mobile phase at a flow rate of 1.0 mL/min. The column temperature was set at 25 ºC, and the detection wavelength was 210 nm. The linear range of the method was 5–200 μg/mL with a correlation coefficient of 0.9975. The recovery was 92–112%, and the relative standard deviation was 1.85% (n = 9. The present method has been used to study the distribution of linalool in the plant Michelia alba. The plant samples include flowers, leaves and tender twigs. Furthermore, leaves included samples in their tender, grown-up and fallen phases, and flowers included samples in their juvenile, middle and whitening phases. The concentrations of linalool in different parts of the plant were 0.21–0.65%, 1.63–4.89% and 0.43% for leaves, flowers and tender twigs, respectively. The results showed that all the plant materials contained relative high concentration of linalool, and juvenile phase flowers contained the highest concentration of linalool. Notably, the fallen leaves also contained high concentrations of linalool, which could be a potential resource of this compound. The results obtained are very helpful for the potential full utilization of this plant.

  2. Supramolecular solvent-based extraction of benzimidazolic fungicides from natural waters prior to their liquid chromatographic/fluorimetric determination.

    Science.gov (United States)

    Moral, Antonia; Sicilia, María Dolores; Rubio, Soledad

    2009-05-01

    A supramolecular solvent made up of vesicles of decanoic acid in the nano- and microscale regimes dispersed in a continuous aqueous phase is proposed for the extraction/preconcentration of benzimidazolic fungicides (BFs) from river and underground water samples prior to their determination by liquid chromatography (LC)/fluorimetry. The solvent is produced from the coacervation of decanoic acid aqueous vesicles by the action of tetrabutylammonium (Bu(4)N(+)). Carbendazim (CB), thiabendazole (TB) and fuberidazole (FB) are extracted on the basis of hydrophobic and pi-cation interactions and the formation of hydrogen bonds. The extraction provides high preconcentration factors (160 for CB and 190 for TB and FB), requires a short time (the procedure takes less than 20 min and several samples can be simultaneously processed) and a low sample volume (20 mL), and avoids the use of toxic organic solvents. Because of the absence of matrix interferences and the low viscosity of the extracts, these can be directly injected into the chromatographic system without the need of cleaning-up or diluting them. Recoveries are not influenced by the presence of salt concentrations up to 1 M. The proposed method provides detection limits for the determination of CB, TB and FB in natural waters of 32, 4 and 0.1 ng L(-1), respectively, and a precision, expressed as relative standard deviation (n=11) of 5.5% for CB (100 ng L(-1)), 4.0% for TB (80 ng L(-1)) and 2.5% for FB (30 ng L(-1)). Recoveries obtained by applying this approach to the analysis of river and underground water samples fortified at the ng L(-1) level are in the intervals 75-83, 95-102 and 97-101% for CB, TB and FB, respectively.

  3. An ecofriendly green liquid chromatographic method for simultaneous determination of nicotinamide and clindamycin phosphate in pharmaceutical gel for acne treatment

    Directory of Open Access Journals (Sweden)

    Fawzia Ibrahim

    2017-07-01

    Full Text Available A new green micellar liquid chromatographic method was developed and validated for the quantitative estimation of nicotinamide (NICO and clindamycin phosphate (CLD in bulk and pharmaceutical gel formulation. The analytes are well resolved in less than 6.0 minutes using micellar mobile phase consisting of 0.10M sodium dodecyl sulfate (SDS, 0.3% triethylamine, and 10% 2-propanol in 0.02M orthophosphoric acid at pH 3.0, running through an Eclipse XDB-C8 column (150 mm×4.6 mm, 5 μm particle size with flow rate 1.0 mL/min. The effluent was monitored with diode array detection at 210 nm. The retention times of NICO and CLD were 3.8 minutes and 5.6 minutes, respectively. The method was validated according to the International Conference on Harmonisation (ICH guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, robustness, and specificity to prove its reliability. Linear correlation was achieved by plotting the peak area of each drug against its concentration. It was found to be rectilinear in the ranges of 1.0–40.0 μg/mL and 0.5–15.0 μg/mL with limits of detection of 0.06 μg/mL and 0.03 μg/mL and limits of quantification of 0.19 μg/mL and 0.09 μg/mL for NICO and CLD, respectively. The method was successfully implemented for the simultaneous determination of the analytes in their bulk powder and combined gel formulation with high % recoveries. The ease of sample treatment facilitates and greatly expedites the treatment with reduced cost and improved accuracy of the procedure.

  4. Reductive amination of glutaraldehyde 2,4-dinitrophenylhydrazone using 2-picoline borane and high-performance liquid chromatographic analysis.

    Science.gov (United States)

    Uchiyama, Shigehisa; Sakamoto, Hironari; Ohno, Akiko; Inaba, Yohei; Nakagome, Hideki; Kunugita, Naoki

    2012-09-21

    A typical method for the measurement of glutaraldehyde (GLA) employs 2,4-dinitrophenylhydrazine (DNPH) to form GLA-DNPhydrazone derivatives. However, this method is subject to analytical errors because GLA-DNPhydrazone is a quaternary bis-derivative and forms three geometric isomers (E-E, E-Z and Z-Z) as a result of the two C[double bond, length as m-dash]N double bonds. To overcome this issue, a method for transforming the C[double bond, length as m-dash]N double bond into a C-N single bond, using reductive amination of DNPhydrazone derivatives, has been applied. The amination reaction of GLA-DNPhydrazones with 2-picoline borane is accelerated with catalytic amounts of acid and is completed within 10 minutes in the presence of 100 mmol L(-1) phosphoric acid. Reduction of GLA-DNPhydrazone by 2-picoline borane is unique and results in the formation of N-(2,4-dinitrophenyl)-1-piperidinamine (DNPPA). NMR and LC-APCI-MS data confirmed the product identification. DNPPA is very stable and did not change when stored for at least four weeks at room temperature. DNPPA has excellent solubility of 14.6 g L(-1) at 20 °C in acetonitrile. The absorption maximum wavelength and the molar absorptivity of DNPPA were 351 nm and 4.2 × 10(4) L mol(-1) cm(-1) respectively. Complete separation between the reduced forms of C1-C10 aldehyde DNPhydrazones, including DNPPA, can be achieved by operating the reversed-phase high-performance liquid chromatograph at 351 nm in gradient mode using a C18 amide column. The reductive amination method for GLA overcomes analytical errors caused by E-E, E-Z and Z-Z geometrical isomers.

  5. [Influences of ion-suppressors on retention behaviors of nine food additives in reversed-phase high performance liquid chromatographic separation].

    Science.gov (United States)

    Zhao, Yonggang; Chen, Xiaohong; Li, Xiaoping; Yao, Shanshan; Jin, Micong

    2011-10-01

    The influences of ion-suppressors on retention behaviors of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in reversed-phase high performance liquid chromatographic (RP-HPLC) separation were investigated. The organic modification effects of acids, i. e. , trifluoroacetic acid (TFA) and buffer salts, i. e. , TFA-ammonium acetate (AmAc) were studied emphatically. The relationships between retention factors of solutes and volume percentages of ion-suppressors in the mobile phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, separately. The separation of nine food additives was completed by a gradient elution with acetonitrile-TFA (0.01%, v/v)-AmAc (2. 5 mmol/L) aqueous solution as the mobile phases. An RP-HPLC method was established for the simultaneous determination of nine food additives in red wine. In the range of 10. 0 - 100. 0 mg/L, nine food additives showed good linearity with the correlation coefficients ( r2 ) larger than 0. 999 1. The limits of detection (LODs) were in the range of 0. 33 - 2. 36 mg/L and the limits of quantification (LOQs) were in the range of 1. 11 - 7. 80 mg/L. The spiked recoveries were between 87. 61% and 108. 4% with the relative standard deviations (RSDs) of 2. 2% -9. 4%. These results are of referential significance for the rapid establishment and accu- rate optimization of RP-HPLC separation for the simultaneous determination of food additives in other foods.

  6. Analysis of anti-neoplastic drug in bacterial ghost matrix, w/o/w double nanoemulsion and w/o nanoemulsion by a validated 'green' liquid chromatographic method.

    Science.gov (United States)

    Youssof, Abdullah M E; Salem-Bekhit, Mounir M; Shakeel, Faiyaz; Alanazi, Fars K; Haq, Nazrul

    2016-07-01

    The objective of the present investigation was to develop and validate a 'green' reversed phase high-performance liquid chromatography (RP-HPLC) method for rapid analysis of a cytotoxic drug 5-fluorouracil (5-FU) in bulk drug, marketed injection, water-in-oil (w/o) nanoemulsion, double water-in-oil-in-water (w/o/w) nanoemulsion and bacterial ghost (BG) matrix. The chromatography study was carried out at room temperature (25±1°C) using an HPLC system with the help of ultraviolet (UV)-visible detector. The chromatographic performance was achieved with a Nucleodur 150mm×4.6mm RP C8 column filled with 5µm filler as a static phase. The mobile phase consisted of ethyl acetate: methanol (7:3% v/v) which was delivered at a flow rate of 1.0mLmin(-1) and the drug was detected in UV mode at 254nm. The developed method was validated in terms of linearity (r(2)=0.998), accuracy (98.19-102.09%), precision (% RSD=0.58-1.17), robustness (% RSD=0.12-0.53) and sensitivity with satisfactory results. The efficiency of the method was demonstrated by the assay of the drug in marketed injection, w/o nanoemulsion, w/o/w nanoemulsion and BG with satisfactory results. The successful resolution of the drug along with its degradation products clearly established the stability-indicating nature of the proposed method. Overall, these results suggested that the proposed analytical method could be effectively applied to the routine analysis of 5-FU in bulk drug, various pharmaceutical dosage forms and BG. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. High Performance Liquid Chromatographic Method for the Determination of Piroxicam, Naproxen, Diclofenac Sodium, and Mefenamic Acid in Bulk Drug and Pharmaceutical Preparations

    Directory of Open Access Journals (Sweden)

    Sarmad Bahjat Dikran

    2018-03-01

    Full Text Available A simple accurate and rapid reversed phase high performance liquid chromatographic method has been developed and validated for the determination of four nonsteroidal anti-inflammatory drugs;  Piroxicam(PX,  Naproxen(NAP,  Diclofenac sodium(DCL and Mefenamic acid(MFNC in their pure form and different commercial pharmaceutical formulation. The separation was performed on a NUCLEODUR® 100-5 C18ec (250 × 4.6 mm i.d.; particle size 5 μm column as stationary phase with a mobile phase comprising of acetonitrile: deionized water acidified with 1% acetic acid in gradient mode. The flow rate was 1.5 mL.min-1 at the temperature 35 ºC and detection was carried out at 264 nm. Separation has been completed within 8 min. The retention times of Piroxicam, Naproxen, Diclofenac sodium, and Mefenamic acid were 4.267 min, 4.785 min, 6.555 min, and 7.683 min respectively. The linearity for Piroxicam was in the range of 3–200 μg.mL-1 and for Naproxen and Mefenamic acid was in the range 1-200 μg.mL-1, while for Diclofenac sodium was in the range 1.5–200 μg.mL-1. The proposed method was successfully applied for the determination of these drugs in their pure form and different pharmaceutical preparations (tablets, capsules, and ampoule and there is no interference with additives.

  8. Development and validation of a dissolution test with reversed-phase high performance liquid chromatographic analysis for Candesartan cilexetil in tablet dosage forms

    Directory of Open Access Journals (Sweden)

    Vairappan Kamalakkannan

    2016-09-01

    Full Text Available A simple, rapid, selective and reproducible reversed-phase high performance liquid chromatographic (RP-HPLC method has been developed and validated for the estimation of release of Candesartan cilexetil (CC in tablets. Analysis was performed on an Agilent, Zorbax C8 column (150mm × 4.6mm, 5μm with the mobile phase consisting of phosphate buffer (pH2.5–acetonitrile (15:85, v/v at a flow rate of 1.0mL/min. UV detection was performed at 215nm and the retention time for CC was 2.2. The calibration curve was linear (correlation coefficient = 1.000 in the selected range of analyte. The optimized dissolution conditions include the USP apparatus 2 at a paddle rotation rate of 50rpm and 900mL of phosphate buffer (pH7.2 with 0.03% of polysorbate 80 as dissolution medium, at 37.0 ± 0.5°C. The method was validated for precision, linearity, specificity, accuracy, limit of quantitation and ruggedness. The system suitability parameters, such as theoretical plate, tailing factor and relative standard deviation (RSD between six standard replicates were well within the limits. The stability result shows that the drug is stable in the prescribed dissolution medium. Three different batches (A, B and C of the formulation containing 8mg of Candesartan cilexetil was performed with the developed method and the results showed no significant differences among the batches.

  9. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation....... The argon chloride interference at m/z 75 was eliminated by chromatographic separation of the chloride present in the sample from the arsenic analytes. The ClO+ ion detected at m/z 51 and 53 was used to monitor the retention time of chloride in the anion-exchange system. The chloride eluted about 100 s...

  10. Validation and implementation of liquid chromatographic-mass spectrometric (LC-MS) methods for the quantification of tenofovir prodrugs.

    Science.gov (United States)

    Hummert, Pamela; Parsons, Teresa L; Ensign, Laura M; Hoang, Thuy; Marzinke, Mark A

    2018-04-15

    The nucleotide reverse transcriptase inhibitor tenofovir (TFV) is widely administered in a disoproxil prodrug form (tenofovir disoproxil fumarate, TDF) for HIV management and prevention. Recently, novel prodrugs tenofovir alafenamide fumarate (TAF) and hexadecyloxypropyl tenofovir (CMX157) have been pursued for HIV treatment while minimizing adverse effects associated with systemic TFV exposure. Dynamic and sensitive bioanalytical tools are required to characterize the pharmacokinetics of these prodrugs in systemic circulation. Two parallel methods have been developed, one to combinatorially quantify TAF and TFV, and a second method for CMX157 quantification, in plasma. K 2 EDTA plasma was spiked with TAF and TFV, or CMX157. Following the addition of isotopically labeled internal standards and sample extraction via solid phase extraction (TAF and TFV) or protein precipitation (CMX157), samples were subjected to liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis. For TAF and TFV, separation occurred using a Zorbax Eclipse Plus C18 Narrow Bore RR, 2.1 × 50 mm, 3.5 μm column and analytes were detected on an API5000 mass analyzer; CMX157 was separated using a Kinetex C8, 2.1 × 50 mm, 2.6 μm column and quantified using an API4500 mass spectrometer. Methods were validated according to FDA Bioanalytical Method Validation guidelines. Analytical methods: were optimized for the multiplexed monitoring of TAF and TFV, and CMX157 in plasma. The lower limits of quantification (LLOQs) for TAF, TFV, and CMX157 were 0.03, 1.0, and 0.25 ng/mL, respectively. Calibration curves were generated via weighted linear regression of standards. Intra- and inter-assay precision and accuracy studies demonstrated %CVs ≤ 14.4% and %DEVs ≤ ± 7.95%, respectively. Stability and matrix effects studies were also performed. All results were acceptable and in accordance with the recommended guidelines for bioanalytical methods. Assays were also

  11. High performance liquid chromatographic-mass spectrometric assay for the quantitation of BMS-204352 in dog K(3)EDTA plasma.

    Science.gov (United States)

    Yao, Ming; Mantha, Subbarao; Shah, Vinod R; Vachharajani, Nimish N; Arnold, Mark E; Pursley, Janice M; Srinivas, Nuggehally R

    2002-05-01

    A high performance liquid chromatographic-mass spectrometric (LC/MS) assay was developed and validated for the determination of BMS-204352 in dog K(3)EDTA plasma. A 0.5 mL aliquot of control plasma was spiked with BMS-204352 and internal standard (IS) and buffered with 1 mL of 5 mM ammonium acetate. The mixture was then extracted with 3 mL of toluene. After separation and evaporation of the organic phase to dryness using nitrogen at 40 degrees C, the residue was reconstituted in the mobile phase and 25 microL of the sample were injected onto a Hypersil C(18) column (2 x 50 mm; 3 microm) at a flow rate of 0.5 mL/min. The mobile phase was consisted of two solvent mixtures (A and B). Solvent A was composed of 5 mM ammonium acetate and 0.1% triethylamine in 75:25 v/v water:methanol, pH adjusted to 5.5 with glacial acetic acid, and solvent B was 5 mM ammonium acetate in methanol. A linear gradient system was used to elute the analytes. The mass spectrometer was programmed to admit the de-protonated molecules at m/z 352.7 (IS) and m/z 357.9 (BMS-204352). Standard curves of BMS-204352 were linear (r(2) > or = 0.998) over the concentration range of 0.5-1000 ng/mL. The mean predicted quality control (QC) concentrations deviated less than 5.1% from the corresponding nominal values (ie 4, 80, 400 and 2000 ng/mL); the within- and between-assay precision of the assay were within 5.5% relative standard deviation. Stability of BMS-204352 was confirmed after at least three freeze/thaw cycles and BMS-204532 was stable in dog plasma when stored frozen at or below -20 degrees C for at least 16 weeks in spiked QC samples and for at least 4 1/2 weeks for in vivo study samples. BMS-204352 and IS were stable in the injection solvent at room temperature for at least 24 h. The assay was applied to delineate the pharmacokinetic disposition of BMS-204352 in dogs following a single intravenous dose administration. In conclusion, the assay is accurate, precise, specific, sensitive and

  12. Improved stochastic resonance algorithm for enhancement of signal-to-noise ratio of high-performance liquid chromatographic signal

    International Nuclear Information System (INIS)

    Xie Shaofei; Xiang Bingren; Deng Haishan; Xiang Suyun; Lu Jun

    2007-01-01

    Based on the theory of stochastic resonance, an improved stochastic resonance algorithm with a new criterion for optimizing system parameters to enhance signal-to-noise ratio (SNR) of HPLC/UV chromatographic signal for trace analysis was presented in this study. Compared with the conventional criterion in stochastic resonance, the proposed one can ensure satisfactory SNR as well as good peak shape of chromatographic peak in output signal. Application of the criterion to experimental weak signals of HPLC/UV was investigated and the results showed an excellent quantitative relationship between different concentrations and responses

  13. Development of Chromatographic Fingerprints of Eurycoma longifolia (Tongkat Ali Roots Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC

    Directory of Open Access Journals (Sweden)

    Nor Nasriah Zaini

    2016-04-01

    Full Text Available E. longifolia is attracting interest due to its pharmacological properties and pro-vitality effects. In this study, an online SPE-LC approach using polystyrene divinyl benzene (PSDVB and C18 columns was developed in obtaining chromatographic fingerprints of E. longifolia. E. longifolia root samples were extracted using pressurized liquid extraction (PLE technique prior to online SPE-LC. The effects of mobile phase compositions and column switching time on the chromatographic fingerprint were optimized. Validation of the developed method was studied based on eurycomanone. Linearity was in the range of 5 to 50 µg∙mL−1 (r2 = 0.997 with 3.2% relative standard deviation of peak area. The developed method was used to analyze 14 E. longifolia root samples and 10 products (capsules. Selected chemometric techniques: cluster analysis (CA, discriminant analysis (DA, and principal component analysis (PCA were applied to the fingerprint datasets of 37 selected peaks to evaluate the ability of the chromatographic fingerprint in classifying quality of E. longifolia. Three groups were obtained using CA. DA yielded 100% correlation coefficient with 19 discriminant compounds. Using PCA, E. longifolia root samples were clearly discriminated from the products. This study showed that the developed online SPE-LC method was able to provide comprehensive evaluation of E. longifolia samples for quality control purposes.

  14. A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

    Science.gov (United States)

    Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

    1990-01-01

    A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

  15. A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.

    Science.gov (United States)

    Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

    2016-07-01

    A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Rapid determination of environmental plutonium in large water samples by means of manganese dioxide Co-precipitation and extraction chromatographic separation

    International Nuclear Information System (INIS)

    Sidhu, R.S.; Hoff, P.

    1999-01-01

    Plutonium activity determinations in environmental water samples are routinely performed in many laboratories. Due to the low plutonium concentrations and the complexity of the plutonium aqueous chemistry, these analysis involve cumbersome preconcentration and separation procedures and long measurement times. We describe a procedure where MnO 2 (s) is used as scavenger to preconcentrate Pu prior to separation by the transuranium specific extraction chromatographic resin TRU-Resin. The ability of MnO 4 - /MnO 2 (s) to destroy organic matter and oxidise plutonium is combined with the specific behaviour of the TRU-resin for transuranium elements. The method facilitates a rapid preconcentration and separation of plutonium. With the use of this procedure, the laboratory work on one sample can be performed in one day with minimum attention. The overall yields from a 200 litre fresh- or seawater sample to a measurable Pu source are between 70-85%. (orig.)

  17. Alternative solvent-based methyl benzoate vortex-assisted dispersive liquid-liquid microextraction for the high-performance liquid chromatographic determination of benzimidazole fungicides in environmental water samples.

    Science.gov (United States)

    Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2014-11-01

    Vortex-assisted dispersive liquid-liquid microextraction using methyl benzoate as an alternative extraction solvent for extracting and preconcentrating three benzimidazole fungicides (i.e., carbendazim, thiabendazole, and fluberidazole) in environmental water samples before high-performance liquid chromatographic analysis has been developed. The selected microextraction conditions were 250 μL of methyl benzoate containing 300 μL of ethanol, 1.0% w/v sodium acetate, and vortex agitation speed of 2100 rpm for 30 s. Under optimum conditions, preconcentration factors were 14.5-39.0 for the target fungicides. Limits of detection were obtained in the range of 0.01-0.05 μg/L. The proposed method was then applied to surface water samples and the recovery evaluations at three spiked concentration levels of 5, 30, and 50 μg/L were obtained in the range of 77.4-110.9% with the relative standard deviation water samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Development and validation of a high-performance liquid chromatographic method for the determination of cyproterone acetate in human skin.

    Science.gov (United States)

    Henry de Hassonville, Sandrine; Chiap, Patrice; Liégeois, Jean-François; Evrard, Brigitte; Delattre, Luc; Crommen, Jacques; Piel, Géraldine; Hubert, Philippe

    2004-09-21

    In the framework of a preliminary study on the transdermal penetration of cyproterone acetate (CPA), a simple and rapid procedure involving an extraction step coupled to a HPLC-UV determination has been developed for the separation and quantification of CPA in the two main skin layers-epidermis and dermis-after local application. The separation of epidermis and dermis layers was carefully carried out by means of a sharp spatula after skin immersion in heated water at 65 degrees C. The two skin layers were then treated separately according to the same process: (1) sample homogenization by vibration after freezing with liquid nitrogen in a Mikro-Dismembrator; (2) CPA extraction with methanol after addition of the internal standard (betamethasone dipropionate); (3) centrifugation; (4) evaporation of a supernatant aliquot; (5) dissolution of the dry residue in methanol and addition of water; (6) centrifugation; (7) injection of a supernatant aliquot into the HPLC system. The separation was achieved on octadecylsilica stationary phase using a mobile phase consisting in a mixture of acetonitrile and water (40:60 (v/v)). The method was then validated using a new approach based on accuracy profiles over a CPA concentration range from 33 to 667 ng/ml for each skin layer. Finally, the method was successfully applied to the determination of CPA to several skin samples after topical application of different gel formulations containing CPA.

  19. High-performance liquid chromatographic determination of histamine in biological samples: the cerebrospinal fluid challenge--a review.

    Science.gov (United States)

    Wang, Zhaopin; Wu, Juanli; Wu, Shihua; Bao, Aimin

    2013-04-24

    Histamine, a neurotransmitter crucially involved in a number of basic physiological functions, undergoes changes in neuropsychiatric disorders. Detection of histamine in biological samples such as cerebrospinal fluid (CSF) is thus of clinical importance. The most commonly used method for measuring histamine levels is high performance liquid chromatography (HPLC). However, factors such as very low levels of histamine, the even lower CSF-histamine and CSF-histamine metabolite levels, especially in certain neuropsychiatric diseases, rapid formation of histamine metabolites, and other confounding elements during sample collection, make analysis of CSF-histamine and CSF-histamine metabolites a challenging task. Nonetheless, this challenge can be met, not only with respect to HPLC separation column, derivative reagent, and detector, but also in terms of optimizing the CSF sample collection. This review aims to provide a general insight into the quantitative analyses of histamine in biological samples, with an emphasis on HPLC instruments, methods, and hyphenated techniques, with the aim of promoting the development of an optimal and practical protocol for the determination of CSF-histamine and/or CSF-histamine metabolites. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Rapid and simple clean-up and derivatizaton procedure for the gas chromatographic determination of acidic drugs in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Hulshoff, A.

    1979-01-01

    A rapid and simple clean-up and derivatization procedure that can be generally applied to the gas chromatographie (GC) determination of acidic drugs of various chemical and therapeutic classes is described. The drugs are extracted from acidified plasma with chloroform containing 5% of isopropanol,

  1. A RAPID THIN-LAYER CHROMATOGRAPHIC PROCEDURE TO IDENTIFY POOR AND EXTENSIVE OXIDATIVE DRUG METABOLIZERS IN MAN USING DEXTROMETHORPHAN

    NARCIS (Netherlands)

    DEZEEUW, RA; EIKEMA, D; FRANKE, JP; JONKMAN, JHG

    A rapid TLC method is presented to distinguish poor oxidative drug metabolizers from extensive oxidative drug metabolizers. Dextromethorphan (1) is used as test probe because it is safe, well characterized, generally available and easy to measure. The method is based on the extraction of 1 and its

  2. High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Ying Zhou

    2012-02-01

    Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

  3. [Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

    Science.gov (United States)

    Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

    2015-08-01

    In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

  4. Chromatographic background drift correction coupled with parallel factor analysis to resolve coelution problems in three-dimensional chromatographic data: quantification of eleven antibiotics in tap water samples by high-performance liquid chromatography coupled with a diode array detector.

    Science.gov (United States)

    Yu, Yong-Jie; Wu, Hai-Long; Fu, Hai-Yan; Zhao, Juan; Li, Yuan-Na; Li, Shu-Fang; Kang, Chao; Yu, Ru-Qin

    2013-08-09

    Chromatographic background drift correction has been an important field of research in chromatographic analysis. In the present work, orthogonal spectral space projection for background drift correction of three-dimensional chromatographic data was described in detail and combined with parallel factor analysis (PARAFAC) to resolve overlapped chromatographic peaks and obtain the second-order advantage. This strategy was verified by simulated chromatographic data and afforded significant improvement in quantitative results. Finally, this strategy was successfully utilized to quantify eleven antibiotics in tap water samples. Compared with the traditional methodology of introducing excessive factors for the PARAFAC model to eliminate the effect of background drift, clear improvement in the quantitative performance of PARAFAC was observed after background drift correction by orthogonal spectral space projection. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Optimization of chromatographic conditions for determination of aflatoxin B1, B2, G1 and G2 by using liquid chromatography-mass Spectrometry

    Science.gov (United States)

    Ramadhaningtyas, Dillani Putri; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

    2017-11-01

    The optimization of instrument condition and chromatographic separation for analysis of aflatoxin B1, B2, G1 and G2 using liquid chromatography tandem with mass spectrometer detector was conducted in the aim to provide more accurate and reliable analysis results. The aflatoxin known to be serious threat for human health as it is classified as the carcinogenic compounds. The aflatoxin B1, B2, G1 and G2 were selected due to its extensive contamination in various agricultural commodities. The best chromatographic separation was obtained using C-18 column with gradient elution of solvent 5 mM ammonium acetate and 0.1% formic acid in methanol at 7 minutes runtime analysis. The linearity of the detector showed satisfied results as the coefficient determination found to be 0.9994, 0.9996, 0.9998 and 0.9987 for aflatoxin B1, G1, B2, and G2 respectively in the range concentration from 1 to 20 ng/g. The quantifier ion selected for the aflatoxin B1, B2, G1 and G2 was m/z 285.1, 259, 243 and 313 respectively. The instrument precision at these quantifier ions also showed satisfied result with %RSD was around 3.4 to 6.8%. The optimized method present in this study can be used for further sample analysis.

  6. Liquid chromatographic method for the simultaneous determination of cefalexin and trimethoprim in dog plasma and application to the pharmacokinetic studies of a coformulated preparation.

    Science.gov (United States)

    Qi, Meiling; Wang, Peng; Sun, Ping; Liu, Xia

    2006-03-07

    A liquid chromatographic method is described for the simultaneous determination of cefalexin and trimethoprim in dog plasma. A simple protein precipitation procedure was adopted for the sample preparation with satisfactory extraction recoveries for both analytes. Chromatographic separation of the analytes was achieved on a C(18) column using a mixture of 2 mol/l formate buffer (pH 3.5), methanol and acetonitrile (22:7:7, v/v/v) containing a 0.002 mol/l sodium dodecyl sulfate as mobile phase and detection was performed at 240 nm. The linearity was obtained over the concentration ranges of 1.0-100.0 microg/ml for cefalexin and 0.5-50.0 microg/ml for trimethoprim. For each level of QC samples including the lower limit of quantification, both inter- and intra-day precisions (R.S.D.) were trimethoprim, and accuracy (RE) was -1.4% for cefalexin and -3.0% for trimethoprim. The present LC method was successfully applied to the pharmacokinetic studies of coformulated cefalexin dispersible tablets after oral administration to beagle dogs.

  7. Systematic evaluation of commercially available ultra-high performance liquid chromatography columns for drug metabolite profiling: optimization of chromatographic peak capacity.

    Science.gov (United States)

    Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Gross, Gerhard; Hankemeier, Thomas; Vreeken, Rob J

    2014-12-29

    The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC

  8. Rapid determination of octanol-water partition coefficient using vortex-assisted liquid-liquid microextraction.

    Science.gov (United States)

    Román, Iván P; Mastromichali, Anna; Tyrovola, Konstantina; Canals, Antonio; Psillakis, Elefteria

    2014-02-21

    Vortex-assisted liquid-liquid microextraction (VALLME) coupled with high-performance liquid chromatography (HPLC) is proposed here for the rapid determination of octanol-water partitioning coefficients (Kow). VALLME uses vortex agitation, a mild emulsification procedure, to disperse microvolumes of octanol in the aqueous phase thus increasing the interfacial contact area and ensuring faster partitioning rates. With VALLME, 2min were enough to achieve equilibrium conditions between the octanolic and aqueous phases. Upon equilibration, separation was achieved using centrifugation and the octanolic microdrop was collected and analyzed in a HPLC system. Six model compounds with logKow values ranging between ∼0.5 and 3.5 were used during the present investigations. The proposed method produced logKow values that were consistent with previously published values and the recorded uncertainty was well within the acceptable log unit range. Overall, the key features of the proposed Kow determination procedure comprised speed, reliability, simplicity, low cost and minimal solvent consumption. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Nanofluid of zinc oxide nanoparticles in ionic liquid for single drop liquid microextraction of fungicides in environmental waters prior to high performance liquid chromatographic analysis.

    Science.gov (United States)

    Amde, Meseret; Tan, Zhi-Qiang; Liu, Rui; Liu, Jing-Fu

    2015-05-22

    Using a nanofluid obtained by dispersing ZnO nanoparticles (ZnO NPs) in 1-hexyl-3-methylimidazolium hexafluorophosphate, new single drop microextraction method was developed for simultaneous extraction of three fungicides (chlorothalonil, kresoxim-methyl and famoxadone) in water samples prior to their analysis by high performance liquid chromatography (HPLC-VWD). The parameters affecting the extraction efficiency such as amount of ZnO NPs in the nanofluid, solvent volume, extraction time, stirring rate, pH and ionic strength of the sample solution were optimized. Under the optimized conditions, the limits of detection were in the range of 0.13-0.19ng/mL, the precision of the method assessed with intra-day and inter-day relative standard deviations were water samples including lake water, river water, as well as effluent and influent of wastewater treatment plant, with recoveries in the range of 74.94-96.11% at 5ng/mL spiking level. Besides to being environmental friendly, the high enrichment factor and the data quality obtained with the proposed method demonstrated its potential for application in multi residue analysis of fungicides in actual water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Rapid Analysis Procedures for Triglycerides and Fatty Acids as Pentyl and Phenethyl Esters for the Detection of Butter Adulteration Using Chromatographic Techniques

    Directory of Open Access Journals (Sweden)

    Daniele Naviglio

    2017-01-01

    Full Text Available This paper presents the development of three methods for quality control, fraud detection, and authentication of butter fat and other oils/fats using chromatographic techniques, with one method for triglycerides and two methods for fatty acids (FAs. The procedure for the analysis of triglycerides requires only dissolution of the sample in n-hexane and gas chromatography (GC analysis using a capillary column. The second method is based on the transesterification of triglycerides as pentyl esters in a single-step reaction using sodium pentanoate in pentanol. The reaction proceeds at room temperature and is similar to the potassium hydroxide-catalysed transesterification of triglycerides with methanol and even more similar to the sodium methoxide method and sodium butanoate method. The advantage of using pentyl esters includes reducing the volatility of short-chain FAs, and substantial recoveries were obtained compared with methyl ester analysis. The third method involves the transesterification of triglycerides in fat through reaction with 2-phenylethanol in a single step; 2-phenylethanol possesses a chromophore, and the phenethyl esters formed are analysed by high-performance liquid chromatography (HPLC with UV detection.

  11. A simple and rapid gas chromatographic method for the determination of dissolved deuterium and nitrogen in heavy water coolant of a nuclear reactor

    International Nuclear Information System (INIS)

    Nair, B.K.S.

    1976-01-01

    A known volume of a heavy water sample is equilibrated with a known volume of pure helium gas at atmospheric pressure in a sample tube. The dissolved gases evolve into the helium and distribute themselves between the gaseous and liquid phases according to their equilibrium partial pressures. These partial pressures of the gases in the equilibrium gas mixture are determined by analysing it gas-chromatographically. From these analytical data and the absorption coefficients of deuterium and nitrogen, their original concentrations in heavy water are calculated. Corrections for the increase in the total pressure of the gaseous phase owing to evolved gases are calculated and found to be negligible. Air contamination during sampling and analysis can be detected by the presence of the oxygen peak in the chromatogram and corrected for. The calculation is facilitated by programming it on an electronic calculator. The method is much simpler and faster than the vacuum method usually applied for this analysis. One determination can be completed in about an hour. The average deviation and standard deviation have been estimated at 0.19 ml/litre heavy water and 0.25 ml/litre heavy water respectively in deuterium, and 0.36 and 0.68 ml/litre in nitrogen. (author)

  12. Rapid determination of 226Ra in drinking water samples using dispersive liquid-liquid microextraction coupled with liquid scintillation counting

    International Nuclear Information System (INIS)

    Sadi, B.K.; Chunsheng Li; Kramer, G.H.; Johnson, C.L.; Queenie Ko; Lai, E.P.C.

    2011-01-01

    A new radioanalytical method was developed for rapid determination of 226 Ra in drinking water samples. The method is based on extraction and preconcentration of 226 Ra from a water sample to an organic solvent using a dispersive liquid-liquid microextraction (DLLME) technique followed by radiometric measurement using liquid scintillation counting. In DLLME for 226 Ra, a mixture of an organic extractant (toluene doped with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone) and a disperser solvent (acetonitrile) is rapidly injected into the water sample resulting in the formation of an emulsion. Within the emulsion, 226 Ra reacts with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone and partitions into the fine droplets of toluene. The water/toluene phases were separated by addition of acetonitrile as a de-emulsifier solvent. The toluene phase containing 226 Ra was then measured by liquid scintillation counting. Several parameters were studied to optimize the extraction efficiency of 226 Ra, including water immiscible organic solvent, disperser and de-emulsifier solvent type and their volume, chelating ligands for 226 Ra and their concentrations, inorganic salt additive and its concentration, and equilibrium pH. With the optimized DLLME conditions, the accuracy (expressed as relative bias, B r ) and method repeatability (expressed as relative precision, S B ) were determined by spiking 226 Ra at the maximum acceptable concentration level (0.5 Bq L -1 ) according to the Guidelines for Canadian Drinking Water Quality. Accuracy and repeatability were found to be less than -5% (B r ) and less than 6% (S B ), respectively, for both tap water and bottled natural spring water samples. The minimum detectable activity and sample turnaround time for determination of 226 Ra was 33 mBq L -1 and less than 3 h, respectively. The DLLME technique is selective for extraction of 226 Ra from its decay progenies. (author)

  13. Development and validation of a rapid chromatographic method for the analysis of flunarizine and its main production impurities

    Directory of Open Access Journals (Sweden)

    Niamh O’Connor

    2013-06-01

    Full Text Available A rapid selective method for the analysis of flunarizine and its associated impurities was developed and validated according to ICH guidelines. The separation was carried out using a Thermo Scientific Hypersil Gold C18 column (50mm×4.6mm i.d., 1.9μm particle size with a gradient mobile phase of acetonitrile–ammonium acetate–tetrabutylammoniumhydrogen sulfate buffer, at a flow rate of 1.8mL/min and UV detection at 230nm. Naturally aged samples were also tested to determine sample stability. A profile of sample and impurity breakdown was also presented. Keywords: Flunarizine, Sub 2μm column, Active pharmaceutical ingredient, HPLC

  14. Liquid Chromatography with Electrospray Ionization and Tandem Mass Spectrometry Applied in the Quantitative Analysis of Chitin-Derived Glucosamine for a Rapid Estimation of Fungal Biomass in Soil

    Directory of Open Access Journals (Sweden)

    Madelen A. Olofsson

    2016-01-01

    Full Text Available This method employs liquid chromatography-tandem mass spectrometry to rapidly quantify chitin-derived glucosamine for estimating fungal biomass. Analyte retention was achieved using hydrophilic interaction liquid chromatography, with a zwitter-ionic stationary phase (ZIC-HILIC, and isocratic elution using 60% 5 mM ammonium formate buffer (pH 3.0 and 40% ACN. Inclusion of muramic acid and its chromatographic separation from glucosamine enabled calculation of the bacterial contribution to the latter. Galactosamine, an isobaric isomer to glucosamine, found in significant amounts in soil samples, was also investigated. The two isomers form the same precursor and product ions and could not be chromatographically separated using this rapid method. Instead, glucosamine and galactosamine were distinguished mathematically, using the linear relationships describing the differences in product ion intensities for the two analytes. The m/z transitions of 180 → 72 and 180 → 84 were applied for the detection of glucosamine and galactosamine and that of 252 → 126 for muramic acid. Limits of detection were in the nanomolar range for all included analytes. The total analysis time was 6 min, providing a high sample throughput method.

  15. A rapid method to estimate uranium using ionic liquid as extracting agent from basic aqueous media

    International Nuclear Information System (INIS)

    Prabhath Ravi, K.; Sathyapriya, R.S.; Rao, D.D.; Ghosh, S.K.

    2016-01-01

    Room temperature ionic liquids, as their name suggests are salts with a low melting point typically less than 100 °C and exist as liquid at room temperature. The common cationic parts of ionic liquids are imidazolium, pyridinium, pyrrolidinium, quaternary ammonium, or phosphonium ions, and common anionic parts are chloride, bromide, boron tetrafluorate, phosphorous hexafluorate, triflimide etc. The physical properties of ionic liquids can be tuned by choosing appropriate cations with differing alkyl chain lengths and anions. Application of ionic liquids in organic synthesis, liquid-liquid extractions, electrochemistry, catalysis, speciation studies, nuclear reprocessing is being studied extensively in recent times. In this paper a rapid method to estimate the uranium content in aqueous media by extraction with room temperature ionic liquid tricaprylammoniumthiosalicylate ((A- 336)(TS)) followed by liquid scintillation analysis is described. Re-extraction of uranium from ionic liquid phase to aqueous phase was also studied

  16. Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

    Science.gov (United States)

    Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

    2016-06-01

    In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

    International Nuclear Information System (INIS)

    Canada-Canada, Florentina; Espinosa-Mansilla, Anunciacion; Munoz de la Pena, Arsenio; Mancha de Llanos, Alicia

    2009-01-01

    A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL -1 , for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 μg mL -1 for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIO total /CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIO total /CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIO total /CREA: 0.48, by iodine oxidation method.

  18. Determination of marker pteridins and biopterin reduced forms, tetrahydrobiopterin and dihydrobiopterin, in human urine, using a post-column photoinduced fluorescence liquid chromatographic derivatization method

    Energy Technology Data Exchange (ETDEWEB)

    Canada-Canada, Florentina, E-mail: floricanada@gmail.com [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain); Espinosa-Mansilla, Anunciacion; Munoz de la Pena, Arsenio; Mancha de Llanos, Alicia [Department of Analytical Chemistry, University of Extremadura, 06071 Badajoz (Spain)

    2009-08-19

    A liquid chromatographic method for the simultaneous analysis of marker pteridins and biopterin reduced forms, in urine samples is proposed. A Zorbax Eclipse XDB-C18 column was used for the chromatographic separation, using a 98/2 (v/v), citrate buffer (pH 5.5)-acetonitrile mobile phase, in isocratic mode. A post-column photoderivatization was carried out with an on-line photoreactor, located between a diode array detector (DAD) and a fast scanning fluorescence detector (FSFD). Neopterin (NEO), biopterin (BIO), pterin (PT) and dihydrobiopterin (BH2) were determined by measuring native fluorescence, using the photoreactor in OFF-mode, and tetrahydrobiopterin (BH4) was determined by measuring of the induced fluorescence of the generated photoproducts, using the photoreactor in ON-mode. In addition, Creatinine (CREA), as a reference of metabolites excrection in urine, was simultaneously determined using the DAD detector. Detection limits were 0.2, 13.0, 0.3, 0.3 and 3.5 ng mL{sup -1}, for NEO, BH2, BIO, PT and BH4, respectively, and 0.4 {mu}g mL{sup -1} for CREA. Ratio values for NEO/CREA, PT/CREA, BH4/CREA, BH2/CREA, NEO/BIO and BIO{sub total}/CREA, in urine samples, of healthy children and adults, phenylketonuric children and infected mononucleosis children, are reported. A comparative study, about the mean values obtained for each of the compounds, by the present procedure and by the classical iodine oxidation method (Fukushimas method), has been performed, in urine samples belonging to healthy volunteers. The values obtained were BH4/CREA: 0.41, BH2/CREA: 0.31 and BIO{sub total}/CREA: 0.73, by the proposed method, and BH4/CREA: 0.35, BH2/CREA: 0.20 and BIO{sub total}/CREA: 0.48, by iodine oxidation method.

  19. Quantitative determination of 14C(-)-epicatechin and 14C-rutin on the Uncaria plant by a two-step heterogeneous thin-layer chromatographic-liquid scintillation counting procedure

    International Nuclear Information System (INIS)

    Das, N.P.; Law, K.H.

    1987-01-01

    A simple, rapid, precise and relatively inexpensive thin-layer chromatographic method coupled to heterogeneous liquid scintillation counting procedure was used for the quantitation of radioactivity of biologically synthesized ( 14 C) flavonoids and other phenolic plant constituents. The two flavonoids, namely ( 14 C) rutin and ( 14 C) (-) -epicatechin, extracted from the plant Uncaria elliptica Roxb were separated on plastic thin-layer plates coated with silica gel using the two solvent systems : acetonitrile-acetic acid-water (8.5:0.5:1.5) and ethyl acetate-acetic acid-water (3:1:3). The respective spots on the plates that corresponded to the two flavonoids were cut out and eluted with 3 ml aliquots of methanol followed by direct addition of scintillation flour. This method gave 99 +- 2 per cent of the total count indicating the excellent elution procedure. The results were reproducible and showed linearity over the range of 0 - 35000 dpm. The elution efficiency by several other organic solvents were also investigated. (author). 19 refs., 4 tables

  20. Rapid Analysis of Apolar Low Molecular Weight Constituents in Wood Using High Pressure Liquid Chromatography with Evaporative Light Scattering Detection

    NARCIS (Netherlands)

    Claassen, F.W.; Haar, van de C.; Beek, van T.A.; Dorado, J.; Martinez-Inigo, M.; Sierra-Alvarez, R.

    2000-01-01

    A new high pressure liquid chromatographic method with evaporative light scattering detection was developed for the qualitative and quantitative analysis of apolar, low molecular weight constituents in wood. The wood extractives were obtained by means of a 6 h Soxhlet extraction with acetone. The

  1. Application of Chromatographic and Electrophoretic Methods for the Analysis of Imidazolium and Pyridinium Cations as Used in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    P. Stepnowski

    2006-11-01

    Full Text Available Interest in ionic liquids for their potential in different chemical processes isconstantly increasing, as they are claimed to be environmentally benign – excellent, non-volatile solvents for a wide range of applications. The wide applicability of thesecompounds also demands reliable, relatively simple and reproducible analytical techniques.These methods must be applicable not only to different technical or natural matrices but alsoto the very low concentrations that are likely to be present in biological and environmentalsystems. In this review, therefore, methods for separating and analysing imidazolium- andpyridinium-type ionic liquids in aqueous matrices using high performance liquidchromatography (HPLC and capillary electrophoresis (CE are examined. The techniquesfor identifying ionic liquids are meant primarily to track the concentrations of ionic liquidsas residues not only in products and wastes but also in biological or environmental samples.The application of hyphenated techniques in this field is intended to selectively separate thequaternary entity from other cationic and non-ionic species present in the matrix, and toenable its fine-scale quantification. Nowadays, methods developed for cation analysis arebased mostly on reversed-phase high-performance liquid chromatography, ionchromatography, ion-pair chromatography and capillary electrophoresis, where variousbuffered mobile phases are used.

  2. Optimisation and characterisation of silica-based reversed-phase liquid chromatographic systems for the analysis of basic pharmaceuticals

    NARCIS (Netherlands)

    Vervoort, R.J.M.; Debets, A.J.J.; Claessens, H.A.; Cramers, C.A.M.G.; Jong, de G.J.

    2000-01-01

    Reversed-phase liquid chromatography using silica-based columns is successfully applied in many separations. However, also some drawbacks exist, i.e. the analysis of basic compounds is often hampered by ionic interaction of the basic analytes with residual silanols present on the silica surface,

  3. Method development for liquid chromatographic/triple quadrupole mass spectrometric analysis of trace level perfluorocarboxylic acids in articles of commerce

    Science.gov (United States)

    An analytical method to identify and quantify trace levels of C5 to C12 perfluorocarboxylic acids (PFCAs) in articles of commerce (AOC) is developed and rigorously validated. Solid samples were extracted in methanol, and liquid samples were diluted with a solvent consisting of 60...

  4. Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

    Science.gov (United States)

    Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

    2014-01-01

    An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

  5. Single-step preparation of selected biological fluids for the high performance liquid chromatographic analysis of fat-soluble vitamins and antioxidants.

    Science.gov (United States)

    Lazzarino, Giacomo; Longo, Salvatore; Amorini, Angela Maria; Di Pietro, Valentina; D'Urso, Serafina; Lazzarino, Giuseppe; Belli, Antonio; Tavazzi, Barbara

    2017-12-08

    Fat-soluble vitamins and antioxidants are of relevance in health and disease. Current methods to extract these compounds from biological fluids mainly need use of multi-steps and multi organic solvents. They are time-consuming and difficult to apply to treat simultaneously large sample number. We here describe a single-step, one solvent extraction of fat-soluble vitamins and antioxidants from biological fluids, and the chromatographic separation of all-trans-retinoic acid, 25-hydroxycholecalciferol, all-trans-retinol, astaxanthin, lutein, zeaxanthin, trans-β-apo-8'-carotenal, γ-tocopherol, β-cryptoxanthin, α-tocopherol, phylloquinone, lycopene, α-carotene, β-carotene and coenzyme Q 10 . Extraction is obtained by adding one volume of biological fluid to two acetonitrile volumes, vortexing for 60s and incubating for 60min at 37°C under agitation. HPLC separation occurs in 30min using Hypersil C18, 100×4.6mm, 5μm particle size column, gradient from 70% methanol+30% H 2 O to 100% acetonitrile, flow rate of 1.0ml/min and 37°C column temperature. Compounds are revealed using highly sensitive UV-VIS diode array detector. The HPLC method suitability was assessed in terms of sensitivity, reproducibility and recovery. Using the present extraction and chromatographic conditions we obtained values of the fat-soluble vitamins and antioxidants in serum from 50 healthy controls similar to those found in literature. Additionally, the profile of these compounds was also measured in seminal plasma from 20 healthy fertile donors. Results indicate that this simple, rapid and low cost sample processing is suitable to extract fat-soluble vitamins and antioxidants from biological fluids and can be applied in clinical and nutritional studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. New high performance liquid chromatographic method for simultaneous determination of diclofenac and meloxicam in oral formulation of liposomes and human plasma

    International Nuclear Information System (INIS)

    Madni, A.; Ahmad, M.; Usman, M.; Zubair, M.M.; Shoiab, H.M.; Khan, S.A.; Qureshi, M.S.

    2010-01-01

    A new, easy and consistent reversed-phase high-performance liquid chromatographic method with diode array detection has been developed and validated for the simultaneous determination of diclofenac potassium (DP) and meloxicam (MLX) in liposome, marketed brands and human plasma. Microextraction method based on liquid-liquid extraction principal was used to extract drug from plasma matrix. The optimized mobile phase was used in the molar ratio of 20:20:60 (v/v/v) mixture of acetonitrile, methanol and 20 x 10/sup -3/ M potassium dihydrogen phosphate buffer (pH 3.7), pumped at an optimized flow rate of 1.0 mL.min/sup -1/. The linearity was performed in the concentration range of 15 ng.mL/sup -1/ to 10 mu g.mL/sup -1/ with gamma/sup 2/ of 0.9989 +- 0.13 and 0.9979 +- 0.11 (n = 6) for DP and MLX, respectively. The assay was repeatable at concentration levels of 10 ng.mL/sup -1/, 1 mu g.mL/sup -1/ and 10 mu g.mL/sup -1/ with coefficient of variation of 0.168 - 0.603% for 10 ng.mL-1 (DP), 15 ng.mL/sup -/1 (MLX) and 1 mu g.mL/sup -1/ and 10 mu g.mL/sup -1/ for DP and MLX. The LOD values were 3 and 5 ng.mL/sup -1/, while values of LOQ were 10 and 15 ng.mL/sup =11, for DP and MLX. The present method is applicable in routine quality control operations, advanced drug delivery formulations (Liposomes) and in human Plasma samples for pharmacokinetics and bioequivalence studies. (author)

  7. Chiral high-performance liquid chromatographic analysis of fluoxetine and norfluoxetine in rabbit plasma, urine, and vitreous humor using an acetylated beta-cyclodextrin column.

    Science.gov (United States)

    Yee, L; Wong, S H; Skrinska, V A

    2000-10-01

    Fluoxetine (Prozac) is a potent selective serotonin reuptake inhibitor used for the treatment of major depression. Both fluoxetine (F) and its demethylated metabolite, norfluoxetine (NF), are racemic. S-Fluoxetine (SF) and S-norfluoxetine (SNF) are more potent inhibitors of serotonin reuptake than R-fluoxetine (RF) and R-norfluoxetine (RNF). Quantitation of individual enantiomers may provide a greater understanding of pharmacokinetic properties. The objective of this study was to perform a limited chiral selectivity study using rabbit plasma, urine, and vitreous humor analyzed by a solid-phase extraction protocol and a newly developed chiral analysis with an acetylated beta-cyclodextrin (CD) column. Liquid chromatographic parameters for CD were as follows: a mobile phase composition of methanol/0.3% triethylamine buffer, pH 5.6, (30:70), a flow rate of 1 mL/min, detection at 214 nm, and a temperature of 40 degrees C. Elution order was SNF, SF, RNF, and RF with capacity factors of 6, 7, 8, and 9, respectively. The corresponding resolution factors were as follows: R1,2 = 0.8, R2,3 = 1.2, and R3,4 = 0.9. The conditions for solid-phase extraction were optimized for Varian Bond Elut Certify columns. Following sample application, the column was rinsed with water, acetic acid, and then with methanol. Drug enantiomers were eluted with methylene chloride, isopropanol, and ammonium hydroxide (78:20:2). After extract evaporation, the extract residue was reconstituted for high-performance liquid chromatographic analysis. To investigate chiral pharmacology, a biodistribution study was performed by administering 2 mg/kg of F to five rabbits. Blood, urine, and vitreous specimens were collected. Plasma samples collected 45 min postinjection showed nearly equal concentrations of RF and SE After 24 h, the only metabolite detected in plasma was RNF. Drugs were not detectable in vitreous humor. Urine concentrations of SNF, SF, RNF, and RF were 51, 76, 34, and 8 microg/L, respectively

  8. High-performance liquid chromatographic characterization of dissolved organic matter from low-level radioactive waste leachates

    International Nuclear Information System (INIS)

    Caron, F.; Elchuk, S.; Walker, Z.H.

    1996-01-01

    Leachates from a waste degradation experiment, containing ∼700-3700 mg C/I of dissolved organic matter (DOM), were analyzed by high-performance liquid chromatography (HPLC) and liquid chromatography (LC), using various separation strategies. Scaling up of the separation scheme to a semi-preparative scale, suitable for hyphenated techniques, was also investigated. Separations with reversed-phase columns suggested that ∼70-93% of the DOM was hydrophilic, and ion-pair chromatography of this fraction showed the presence of several discrete compounds. Labile and non-labile complexes were formed by adding 60 Co radiotracer. Size-exclusion chromatography indicated that the DOM was primarily in the <1000-1500 Da molecular mass range. (author)

  9. Comparison of gravimetric and gas chromatographic methods for assessing performance of textile materials against liquid pesticide penetration.

    Science.gov (United States)

    Shaw, Anugrah; Abbi, Ruchika

    2004-01-01

    Penetration of liquid pesticides through textile materials is a criterion for determining the performance of protective clothing used by pesticide handlers. The pipette method is frequently used to apply liquid pesticides onto textile materials to measure penetration. Typically, analytical techniques such as Gas Chromatography (GC) are used to measure percentage penetration. These techniques are labor intensive and costly. A simpler gravimetric method was developed, and tests were conducted to compare the gravimetric and GC methods of analysis. Three types of pesticide formulations and 4 fabrics were used for the study. Diluted pesticide formulations were pipetted onto the test specimens and percentage penetration was measured using the 2 methods. For homogeneous formulation, the results of the two methods were fairly comparable. However, due to the filtering action of the textile materials, there were differences in the percentage penetration between the 2 methods for formulations that were not homogeneous.

  10. Chromatographic methods

    International Nuclear Information System (INIS)

    Marhol, M.; Stary, J.

    1975-01-01

    The characteristics are given of chromatographic separation and the methods are listed. Methods and data on materials used in partition, adsorption, precipitation and ion exchange chromatography are listed and conditions are described under which ion partition takes place. Special attention is devoted to ion exchange chromatography where tables are given to show the course of values of the partition coefficients of different ions in dependence on the concentration of agents and the course of equilibrium sorptions on different materials in dependence on the solution pH. A theoretical analysis is given and the properties of the most widely used ion exchangers are listed. Experimental conditions and apparatus used for each type of chromatography are listed. (L.K.)

  11. Liquid chromatographic separation and indirect detection of non-absorbing aliphatic compounds using m-nitrophenol as a detection agent

    International Nuclear Information System (INIS)

    Lee, Seung Seok; Kang, Sam Woo; Moon, Young Ja

    1991-01-01

    m-Nitrophenol(m-NP) was a detection agent for the use of the detection and separation of non-absorbing compounds such as aliphatic acids, alcohols, amines and tetraalkylammonium salts by indirect photometric detection in reversed-phase liquid chromatography. Response of samples was investigated to the several factors such as pH, temperature, and concentration of MeOH as well as concentration of detection reagent in mobile phase. The separation of several mixtures were attempted under optimum condition. (Author)

  12. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

    OpenAIRE

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the prod...

  13. Rapid, cost-effective liquid chromatograghic method for the ...

    African Journals Online (AJOL)

    GRACE

    2006-07-03

    Jul 3, 2006 ... The method was validated and used for pharmacokinetic studies. Key words: Metronidazole ... by the intrinsic analytical properties of the drug molecule ... In addition, such factors as sample size ... account, since these affect the reliability of the quantitation. ... phase and ion-pair high–performance liquid.

  14. High pressure liquid chromatographic analysis of the main pungent principles of solar dried West Indian ginger (Zingiber officinale Roscoe)

    Energy Technology Data Exchange (ETDEWEB)

    Balladin, D.A.; Headley, O. [University of the West Indies, Cave Hill Campus, St. Michael, Barbados (West Indies). Centre for Resource Management and Environmental Studies; Chang-Yen, I. [University of the West Indies, St. Augustine Campus, Trinidad (West Indies). Faculty of Agriculture and Natural Sciences; McGaw, D.R. [University of the West Indies, St. Augustine Campus, Trinidad (West Indies). Dept. of Chemical Engineering

    1998-12-31

    The main pungent principles of West Indian ginger (Zingiber officinale Roscoe) were quantified and qualified using High Pressure Liquid Chromatography. This procedure was used to evaluate the pungency profile of fresh, solar dried and solar dried/steam distilled ginger rhizomes. In this investigation, the total oleoresin extracted was in the ratio [20: 1: 2] for [fresh ginger: solar dried: solar dried/steam distilled ginger rhizomes] with respect to the [6]-gingerol content. This simple isocratic HPLC method can be used to investigate the pungency profile of the extracted oleoresin from the ginger rhizomes. (author)

  15. Matrix effect and correction by standard addition in quantitative liquid chromatographic-mass spectrometric analysis of diarrhetic shellfish poisoning toxins.

    Science.gov (United States)

    Ito, Shinya; Tsukada, Katsuo

    2002-01-11

    An evaluation of the feasibility of liquid chromatography-mass spectrometry (LC-MS) with atmospheric pressure ionization was made for quantitation of four diarrhetic shellfish poisoning toxins, okadaic acid, dinophysistoxin-1, pectenotoxin-6 and yessotoxin in scallops. When LC-MS was applied to the analysis of scallop extracts, large signal suppressions were observed due to coeluting substances from the column. To compensate for these matrix signal suppressions, the standard addition method was applied. First, the sample was analyzed and then the sample involving the addition of calibration standards is analyzed. Although this method requires two LC-MS runs per analysis, effective correction of quantitative errors was found.

  16. Liquid chromatographic analysis of the main pungent principles of solar dried West Indian ginger (Zingiber officinale Roscoe)

    Energy Technology Data Exchange (ETDEWEB)

    Balladin, D.A.; Headley, Oliver [University of the West Indies, Center for Resource Management and Environmental Studies, St. Michael (Barbados)

    1999-10-01

    The main pungent principles and essential oils of West Indian ginger (Zingiber officinale Roscoe) were identified and quantified by liquid chromatography. The stationary phase used was (5.0 g silica gel 70-230 mesh) and the mobile phase [petroleum ether (60-80degC) : diethyl ether (3:7 v/v)]. The first 15 ml contained the very volatile and least polar compounds present in the extracted oleoresin from the solar dried ginger rhizome. These compounds are the essential oils (R{sub f} = 0.90) and 25.63% (w/w) of the total oleoresin charge to the column. The next 5 ml aliquot was without any compounds. The following 25 ml contained the shogaol fraction (R{sub f} = 0.42) and 47.74% (w/w) of the total oleoresin charge to the column. The next 5 ml aliquot was without any compounds. The following 35 ml contained the gingerol fraction (R{sub f} = 0.20) and 27.13% (w/w) of the total oleoresin charge to the column. This simple liquid chromatography method can be used to investigate the essential oils and pungent principles of the extracted oleoresin from the solar dried ginger rhizomes. (Author)

  17. High-performance liquid chromatographic assay of parabens in wash-off cosmetic products and foods using chemiluminescence detection

    International Nuclear Information System (INIS)

    Zhang Qunlin; Lian Mei; Liu Lijuan; Cui Hua

    2005-01-01

    A new method for the simultaneous determination of parabens including methylparaben, ethylparaben, propylparaben, and butylparaben by high-performance liquid chromatography (HPLC) coupled with chemiluminescence detection was developed. The procedure was based on the chemiluminescent enhancement by parabens of the cerium(IV)-rhodamine 6G system in the strong sulfuric acid medium. The good separation of parabens was carried out with an isocratic elution using a mixture of methanol and water (60:40, v/v) within 8.5 min. Under the optimized conditions, a linear working range extends three orders of magnitude with the relative standard deviations of intra- and inter-day precision below 4.5%, and the detection limits were 1.9 x 10 -9 , 2.7 x 10 -9 , 3.9 x 10 -9 , and 5.3 x 10 -9 g ml -1 for methylparaben, ethylparaben, propylparaben, and butylparaben, respectively. The chemiluminescence reaction was well compatible with the mobile phase of high-performance liquid chromatography. The proposed method has been successfully applied to the assay of parabens in wash-off cosmetic products and foods with the minimal sample preparation

  18. Validation of a stability-indicating hydrophilic interaction liquid chromatographic method for the quantitative determination of vitamin k3 (menadione sodium bisulfite) in injectable solution formulation.

    Science.gov (United States)

    Ghanem, Mashhour M; Abu-Lafi, Saleh A; Hallak, Hussein O

    2013-01-01

    A simple, specific, accurate, and stability-indicating method was developed and validated for the quantitative determination of menadione sodium bisulfite in the injectable solution formulation. The method is based on zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC) coupled with a photodiode array detector. The desired separation was achieved on the ZIC-HILIC column (250 mm × 4.6 mm, 5 μm) at 25°C temperature. The optimized mobile phase consisted of an isocratic solvent mixture of 200mM ammonium acetate (NH4AC) solution and acetonitrile (ACN) (20:80; v/v) pH-adjusted to 5.7 by glacial acetic acid. The mobile phase was fixed at 0.5 ml/min and the analytes were monitored at 261 nm using a photodiode array detector. The effects of the chromatographic conditions on the peak retention, peak USP tailing factor, and column efficiency were systematically optimized. Forced degradation experiments were carried out by exposing menadione sodium bisulfite standard and the injectable solution formulation to thermal, photolytic, oxidative, and acid-base hydrolytic stress conditions. The degradation products were well-resolved from the main peak and the excipients, thus proving that the method is a reliable, stability-indicating tool. The method was validated as per ICH and USP guidelines (USP34/NF29) and found to be adequate for the routine quantitative estimation of menadione sodium bisulfite in commercially available menadione sodium bisulfite injectable solution dosage forms.

  19. High performance liquid chromatographic separation of beryllium from some transition metals produced in high energy proton irradiations of medium mass elements: measurement of (p,7Be) cross sections

    International Nuclear Information System (INIS)

    Fassbender, M.; Spellerberg, S.; Qaim, S.M.

    1996-01-01

    A high performance liquid chromatographic (HPLC) method was developed for the separation of 7 Be formed in high energy proton irradiation of medium mass elements like Fe, Cu etc. The bulk of the target material was removed in a preseparation step. Thereafter beryllium was obtained in a high purity within a few minutes elution time using a mixture of 5 mM citric acid and 1.0 mM pyridinedicarboxylic acid as eluent and a SYKAM KO2 analytical cation-exchange column. The effect of Be-carrier on the quality of separation was investigated. The quality of separation deteriorated with the increasing Be-carrier column loading. A certain amount of Be-carrier was, however, necessary in order to quantitate the results. By using low Be-carrier amounts (∝100 μg) and determining the elution yield via a conductometric method, it was possible to obtain quantitative separation results. Besides the analytical column, a semi-preparative column was also used, and the Be separation yield determined gravimetrically. The cross sections for the (p, 7 Be) process on Cu obtained using the two separation columns (analytical and semipreparative) and the two separation yield determination methods agreed within 15%. (orig.)

  20. High-performance liquid chromatographic method for the determination of nicardipine in pure, pharmaceutical preparations and plasma and its application to pharmacokinetics in humans

    Directory of Open Access Journals (Sweden)

    Sheikha M. Al-Ghannam

    2009-01-01

    Full Text Available A simple, sensitive and reproducible reversed-phase liquid chromatographic method has been developed and validated for the determination of nicardipine hydrochloride (NC in pure, pharmaceutical preparations, human plasma and the study of the pharmacokinetics of the drug in human body. Nicardipine in plasma were extracted with hexane-butanol (12:1,v/v after addition of borate buffer (0.5 M, pH=9.0, and then measured by HPLC-UV using a Waters Symmetry C18 column as stationary phase and methanol– triethylamine buffer (0.01M pH 4 with acetic acid (70:30 as mobile phase. Nicardipine was quantified by ultraviolet absorbance at 353 nm. The method proved to be linear in the pure drug in the ranges of 15-200 ng/mL (r=0.9989 and 5-40 ?g/mL (r=0.9995, and for the pharmaceutical preparations and plasma for drug concentrations in the range of 5-40 ?g/mL (r =0.9992 and 25-150 ng/mL (r=0.9991, respectively. The lower limit of detection and the lower quantitation limit of NC in plasma were 11.74 and 35.57 ng/mL, respectively. The method is sensitive and reliable for harmacokineticstudies of nicardipine in humans after the oral administration of immediate-release capsules to healthy subjects.

  1. High-performance liquid chromatographic method for the determination of nicardipine in pure, pharmaceutical preparations and plasma and its application to pharmacokinetics in humans

    Directory of Open Access Journals (Sweden)

    Sheikha Mohammed Al-Ghannam

    2008-12-01

    Full Text Available A simple, sensitive and reproducible reversed-phase liquid chromatographic method has been developed and validated for the determination of nicardipine hydrochloride (NC in pure, pharmaceutical preparations, human plasma and the study of the pharmacokinetics of the drug in human body. Nicardipine in plasma were extracted with hexane-butanol (12:1,v/v after addition of borate buffer (0.5 M, pH=9.0, and then measured by HPLC-UV using a Waters Symmetry C18 column as stationary phase and methanol– triethylamine buffer (0.01M pH 4 with acetic acid (70:30 as mobile phase. Nicardipine was quantified by ultraviolet absorbance at 353 nm. The method proved to be linear in the pure drug in the ranges of 15-200 ng/mL (r=0.9989 and 5-40 µg/mL (r=0.9995, and for the pharmaceutical preparations and plasma for drug concentrations in the range of 5-40 µg/mL (r =0.9992 and 25-150 ng/mL (r=0.9991, respectively. The lower limit of detection and the lower quantitation limit of NC in plasma were 11.74 and 35.57 ng/mL, respectively. The method is sensitive and reliable for pharmacokinetic studies of nicardipine in humans after the oral administration of immediate-release capsules to healthy subjects.

  2. Surface-bubble-modulated liquid chromatography: a new approach for manipulation of chromatographic retention and investigation of solute distribution at water/hydrophobic interfaces.

    Science.gov (United States)

    Nakamura, Keisuke; Nakamura, Hiroki; Saito, Shingo; Shibukawa, Masami

    2015-01-20

    In this paper, we present a new chromatographic method termed surface-bubble-modulated liquid chromatography (SBMLC), that has a hybrid separation medium incorporated with surface nanobubbles. Nanobubbles or nanoscale gas phases can be fixed at the interface between water and a hydrophobic material by delivering water into a dry column packed with a nanoporous material. The incorporation of a gas phase at the hydrophobic surface leads to the formation of the hybrid separation system consisting of the gas phase, hydrophobic moieties, and the water/hydrophobic interface or the interfacial water. One can change the volume of the gas phase by pressure applied to the column, which in turn alters the area of water/hydrophobic interface or the volume of the interfacial water, while the amount of the hydrophobic moiety remains constant. Therefore, this strategy provides a novel technique not only for manipulating the separation selectivity by pressure but also for elucidating the mechanism of accumulation or retention of solute compounds in aqueous solutions by a hydrophobic material. We evaluate the contributions of the interfacial water at the surface of an octadecyl bonded silica and the bonded layer itself to the retention of various solute compounds in aqueous solutions on the column packed with the material by SBMLC. The results show that the interfacial water formed at the hydrophobic surface has a key role in retention even though its volume is rather small. The manipulation of the separation selectivity of SBMLC for some organic compounds by pressure is demonstrated.

  3. Incorporating high-pressure electroosmotic pump and a nano-flow gradient generator into a miniaturized liquid chromatographic system for peptide analysis.

    Science.gov (United States)

    Chen, Apeng; Lynch, Kyle B; Wang, Xiaochun; Lu, Joann J; Gu, Congying; Liu, Shaorong

    2014-09-24

    We integrate a high-pressure electroosmotic pump (EOP), a nanoflow gradient generator, and a capillary column into a miniaturized liquid chromatographic system that can be directly coupled with a mass spectrometer for proteomic analysis. We have recently developed a low-cost high-pressure EOP capable of generating pressure of tens of thousands psi, ideal for uses in miniaturized HPLC. The pump worked smoothly when it was used for isocratic elutions. When it was used for gradient elutions, generating reproducible gradient profiles was challenging; because the pump rate fluctuated when the pump was used to pump high-content organic solvents. This presents an issue for separating proteins/peptides since high-content organic solvents are often utilized. In this work, we solve this problem by incorporating our high-pressure EOP with a nano-flow gradient generator so that the EOP needs only to pump an aqueous solution. With this combination, we develop a capillary-based nano-HPLC system capable of performing nano-flow gradient elution; the pump rate is stable, and the gradient profiles are reproducible and can be conveniently tuned. To demonstrate its utility, we couple it with either a UV absorbance detector or a mass spectrometer for peptide separations. Copyright © 2014. Published by Elsevier B.V.

  4. Determination and validation of a simple high-performance liquid chromatographic method for simultaneous assay of iprodione and vinclozolin in human urine.

    Science.gov (United States)

    Carlucci, Giuseppe; Pasquale, Dorina Di; Ruggieri, Fabrizio; Mazzeo, Pietro

    2005-12-15

    A method based on solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) was developed for the simultaneous determination of 3-(3,5-diclorophenyl)-5-ethenyl-5-methyl-2,4-oxazolidinedione (vinclozolin) and 3-(3,5-diclorophenyl)-N-(1-methylethyl)-2,4-dioxo-1-imidazolidinecarboxamide (iprodione) in human urine. Urine samples containing vinclozolin and iprodione were collected by solid phase extraction using C(18) cartridges. The chromatographic separation was achieved on a Spherisorb ODS2 (250 mm x 4.6 mm, 5 microm) column with an isocratic mobile phase of acetonitrile-water (60:40, v/v). Detection was UV absorbance at 220 nm. The calibration graphs were linear from 30 to 1000 ng/mL for the two fungicides. Intra- and inter-day R.S.D. did not exceed 2.9%. The quantitation limit was 50 ng/mL for vinclozolin and 30 ng/mL for iprodione, respectively.

  5. Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

    Science.gov (United States)

    Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

    2015-08-01

    A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

  6. High-performance liquid chromatographic determination of selenium in coal after derivatization to 2,1,3-benzoselenadiazoles

    Energy Technology Data Exchange (ETDEWEB)

    Khuhawar, M.Y.; Bozdar, R.B.; Babar, M.A. (Sindh University, Jamshoro (Pakistan). Inst. of Chemistry)

    1992-11-01

    High-performance liquid chromatography was examined for the determination of selenium after derivatization to 2,1,3-benzoselenadiazoles using 1,2-diaminobenzene, 1,2-diamino-4-nitrobenzene (NDAB), 2,3-diaminonaphthalene and 3,3-diaminobenzidine as derivatizing agents. Elution was carried out using a mixture of chloroform and hexane, with ultraviolet spectrophotometric detection. The 2,1,3-benzoselenadiazoles were extracted into toluene. Linear calibrations were obtained for 0-4[mu]g of selenium in 10 cm[sup 3] of solution and the detection limits were 20-50 ng of selenium in 10 cm[sup 3] of solution. The method was applied to the determination of selenium in coal samples and a shampoo using NDAB as the derivatizing reagent in acidic solution.

  7. Validation of a Chiral Liquid Chromatographic Method for the Degradation Behavior of Flumequine Enantiomers in Mariculture Pond Water.

    Science.gov (United States)

    Wang, Yan-Fei; Gao, Xiao-Feng; Jin, Huo-Xi; Wang, Yang-Guang; Wu, Wei-Jian; Ouyang, Xiao-Kun

    2016-09-01

    In this work, flumequine (FLU) enantiomers were separated using a Chiralpak OD-H column, with n-hexane-ethanol (20:80, v/v) as the mobile phase at a flow rate of 0.6 mL/min. Solid phase extraction (SPE) was used for cleanup and enrichment. The limit of detection, limit of quantitation, linearity, precision, and intra/interday variation of the chiral high-performance liquid chromatography (HPLC) method were determined. The developed method was then applied to investigate the degradation behavior of FLU enantiomers in mariculture pond water samples. The results showed that the degradation of FLU enantiomers under natural, sterile, or dark conditions was not enantioselective. Chirality 28:649-655, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

  8. High pressure liquid chromatographic assay of technetium in solutions of sodium pertechnetate produced at the AAEC Research Establishment

    International Nuclear Information System (INIS)

    Farrington, K.J.

    1985-12-01

    High pressure liquid chromatography (HPLC) is used for the assay of nanogram quantities of technetium and to determine technetium in decayed pharmaceutical products, derived from three methods of manufacture. These methods of manufacture give comparably low levels of technetium-99, at the time of collection of the solution. However, when the solutions are used to produce ready-to-inject technetium-99m, high levels of technetium-99 are present at the time of calibration, which is the day after the collection date. Where sensitive reagent kits are to be labelled, freshly collected solutions of technetium-99m should be used. The HPLC assay is a valuable technique for the quality control of technetium-based radiopharmaceuticals, and for investigation of methods of manufacture of technetium-99m. Experimental studies confirmed the findings of previous workers

  9. Determination of glibenclamide, metformin hydrochloride and rosiglitazone maleate by reversed phase liquid chromatographic technique in tablet dosage form

    Directory of Open Access Journals (Sweden)

    Havele Shweta S.

    2014-01-01

    Full Text Available A simple, precise and accurate high performance liquid chromatography (HPLC method was developed for the simultaneous estimation of metformin hydrochloride, rosiglitazone maleate, glibenclamide present in multicomponent dosage forms. Chromatography was performed on a 25 cm × 4.6 mm i.d., 5-μm particle, C18 column with 78:22 (v/v methanol: 20 mM potassium dihydrogen phosphate buffer as mobile phase at a flow rate of 1.0 ml/min and UV detection at 238 nm for metformin hydrochloride, rosiglitazone maleate, and glibenclamide. The total elution time was shorter than 9 min. This method was found to be precise and reproducible. This proposed method was successfully applied for the analysis of metformin hydrochloride, rosiglitazone maleate, glibenclamide as a bulk drug and in pharmaceutical formulation without any interference from the excipients.

  10. High-performance liquid chromatographic assay for acetaminophen and phenacetin in the presence of their metabolites in biological fluids

    International Nuclear Information System (INIS)

    Pang, K.S.; Taburet, A.M.; Hinson, J.A.; Gillette, J.R.

    1979-01-01

    The authors propose a method in which tracer amounts of a radiolabeled compound are used as the internal standard for the same unlabeled compound in high-performance liquid chromatography. The approach is valuable when a response from the internal standard becomes undesirable due to the presence of interference by the metabolites. The authors tested their approach with phenacetin and its metabolites, 2-hydroxyphenacetin, N-hydroxyphenacetin, phenetidine, acetaminophen sulfate conjugate and acetaminophen glucuronide conjugate in biological fluids with the use of [ 14 C] phenacetin and [ 3 H] acetaminophen as the internal standards, and were able to quantitate both phenacetin and acetaminophen simultaneously. They also tested the alternative approach in which the unlabeled drug was used as internal standard for tracer amounts of the same radiolabeled compound, with phenacetin and acetaminophen as the internal standards for tracer amounts of [ 14 C] phenacetin and [ 3 H] acetaminophen. Again, they were able to quantiate the two tracer radiolabeled compounds simultaneously. (Auth.)

  11. Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vegetable samples.

    Science.gov (United States)

    Mukdasai, Siriboon; Thomas, Chunpen; Srijaranai, Supalax

    2014-03-01

    Dispersive liquid microextraction (DLME) combined with dispersive µ-solid phase extraction (D-µ-SPE) has been developed as a new approach for the extraction of four pyrethroids (tetramethrin, fenpropathrin, deltamethrin and permethrin) prior to the analysis by high performance liquid chromatography (HPLC) with UV detection. 1-Octanol was used as the extraction solvent in DLME. Magnetic nanoparticles (Fe3O4) functionalized with 3-aminopropyl triethoxysilane (APTS) were used as the dispersive in DLME and as the adsorbent in D-µ-SPE. The extracted pyrethroids were separated within 30 min using isocratic elution with acetonitrile:water (72:28). The factors affecting the extraction efficiency were investigated. Under the optimum conditions, the enrichment factors were in the range of 51-108. Linearity was obtained in the range 0.5-400 ng mL(-1) (tetramethrin) and 5-400 ng mL(-1) (fenpropathrin, deltamethrin and permethrin) with the correlation coefficients (R(2)) greater than 0.995. Detection limits were 0.05-2 ng mL(-1) (water samples) and 0.02-2.0 ng g(-1) (vegetable samples). The relative standard deviations of peak area varied from 1.8 to 2.5% (n=10). The extraction recoveries of the four pyrethroids in field water and vegetable samples were 91.7-104.5%. The proposed method has high potential for use as a sensitive method for determination of pyrethroid residues in water and vegetable samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

    Science.gov (United States)

    Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

    2014-09-12

    Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

    Science.gov (United States)

    Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

    2017-08-29

    With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

    Science.gov (United States)

    Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

    2015-07-01

    Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Effects of chromatographic fractions of Euphorbia hirta on the rat ...

    African Journals Online (AJOL)

    The effects of the chromatographic fractions of Euphorbia hirta Linn on the serum biochemical parameters in rats were investigated. The ethanolic extract of this plant was subjected to chromatographic separation using the vacuum liquid chromatographic technique, a modified form of classical column chromatography.

  16. [Detection of monoamine neurotransmitters and its metabolites by high performance liquid chromatograph after pre-column derivatization of dansyl chloride column].

    Science.gov (United States)

    Huang, Xiao; Chen, Jia-wen; He, Li-ping; Kang, Xue-jun

    2012-12-01

    To develop a high performance liquid chromatography (HPLC) for detection of monoamine neurotransmitters and its metabolites after pre-column derivatization with dansyl chloride. The C(18) chromatograph column (150 mm×4.6 mm×5 µm) was selected for detection, and derived by dansyl chloride (10 mg/ml) under the condition of 50°C water bath by pH11 buffer solution. 20 µl acetic acid acetone solution (1.0 mol/L) was then mixed in for termination of the reaction. Then the solution was cooling to room temperature, 0.1 mol/L acetic acid zinc-acetonitrile-tetrahydrofuran solution was adopted for mobile phrase, with the volume ratio at 62:35:3. The flow rate was 1.0 ml/min between 0-10 min, 2.0 ml/min between 10-35 min. The ultraviolet detection wavelength was 286 nm. The above method separately detected monoamine neurotransmitters and its metabolites and evaluated the limit of detection, accurate degree and accuracy degree. The linear relations between each component was good in the range of 1 - 20 µg/ml (r = 0.999). The lowest detection limit of norepinephrine, dopamine, 5-hydroxytryptamine and the metabolites 3-methoxy-4-benzoglycols, homovanillic acid and 5-heteroauxin were separately 0.60, 0.80, 0.41, 0.21, 0.19 and 0.1 µg/ml; while the average recovery rates were between 78.5% - 95.9%, and the relative standard deviation (RSD) was 6.62%, 7.64%, 2.98%, 3.60%, 5.09% and 3.09%, respectively. In the process of selection and optimization of the chromatographic conditions, we observed the importance of metal ions to discretion, and discussed the temperature, pH of the buffer solution and dosage of dansyl chloride in derivation. Under the above conditions, the reaction was perfect, and the baseline of the detected materials thoroughly separated. The method to detect monoamine neurotransmitters and its metabolites by HPLC and pre-column derivatization with dansyl chloride was established; and this method could provide reference for the detection of polyamine by HPLC.

  17. Multiplex real-time quantitative PCR, microscopy and rapid diagnostic immuno-chromatographic tests for the detection of Plasmodium spp: performance, limit of detection analysis and quality assurance

    Directory of Open Access Journals (Sweden)

    Ralevski Filip

    2009-12-01

    Full Text Available Abstract Background Accurate laboratory diagnosis of malaria species in returning travelers is paramount in the treatment of this potentially fatal infectious disease. Materials and methods A total of 466 blood specimens from returning travelers to Africa, Asia, and South/Central America with suspected malaria infection were collected between 2007 and 2009 at the reference public health laboratory. These specimens were assessed by reference microscopy, multipex real-time quantitative polymerase chain reaction (QPCR, and two rapid diagnostic immuno-chromatographic tests (ICT in a blinded manner. Key clinical laboratory parameters such as limit of detection (LOD analysis on clinical specimens by parasite stage, inter-reader variability of ICTs, staffing implications, quality assurance and cost analysis were evaluated. Results QPCR is the most analytically sensitive method (sensitivity 99.41%, followed by CARESTART (sensitivity 88.24%, and BINAXNOW (sensitivity 86.47% for the diagnosis of malaria in returning travelers when compared to reference microscopy. However, microscopy was unable to specifically identify Plasmodia spp. in 18 out of 170 positive samples by QPCR. Moreover, the 17 samples that were negative by microscopy and positive by QPCR were also positive by ICTs. Quality assurance was achieved for QPCR by exchanging a blinded proficiency panel with another reference laboratory. The Kappa value of inter-reader variability among three readers for BINAXNOW and CARESTART was calculated to be 0.872 and 0.898 respectively. Serial dilution studies demonstrated that the QPCR cycle threshold correlates linearly with parasitemia (R2 = 0.9746 in a clinically relevant dynamic range and retains a LOD of 11 rDNA copies/μl for P. falciparum, which was several log lower than reference microscopy and ICTs. LOD for QPCR is affected not only by parasitemia but the parasite stage distribution of each clinical specimen. QPCR was approximately 6-fold more

  18. High-performance liquid chromatographic determination of β-carotene content in four varieties of lotus stamens

    Directory of Open Access Journals (Sweden)

    Nithida Phonkot

    2010-08-01

    Full Text Available A high-performance liquid chromatography method was developed to determine -carotene content in lotus stamens.The stamens of four varieties of Nelumbo nucifera (Gaertn. and ten samples bought from traditional drug stores were determined.Validation of the method was carried out, the linearity of the -carotene concentrations range from 6.50-58.50 g.mL-1were 0.9997-0.9998. The repeatability and intermediate precision were 0.29 %CV (n=9 and 7.48 %CV (n=9, respectively; theaccuracy was 100.10 %w/w, the detection limit was 9.83 ng.mL-1 and the quantitation limit was 29.80 ng.mL-1. The -caroteneof the four varieties were 465.77-1150.80 mg% (n=3, and of the store samples were 4.70-41.73 mg% (n=3. The resultsdemonstrated that the contents varied according to the variety. The contents in the samples obtained from traditionaldrug stores were much lower that those dried in our laboratory, this might due to the source of the stamens, duration, andconditions of storages.

  19. Simultaneous high performance liquid chromatographic analysis of vitamins B1, B2 and B6 in royal jelly

    Directory of Open Access Journals (Sweden)

    Presoto Ana Elisa F

    2004-01-01

    Full Text Available Royal jelly is used as a food supplement, popularly known as rich in B vitamins. The present work has two objectives: firstly, to apply simultaneous quantitative determination by High Performance Liquid Chromatography of thiamin (vitamin B1, riboflavin (vitamin B2 and pyridoxine (vitamin B6 and secondly to compare the obtained data with the Dietary Reference Intake (DRI values. The values obtained showed no thiamin, a range from 20 to 171 ng g-1 of riboflavin and from 408 to 2 188 ng g-1 of pyridoxine in royal jelly. According to the Food and Nutrition Board (2000, the DRI of these vitamins varies from 0.2-1.4 mg for thiamin; 0.3-1.6 mg for riboflavin and 0.1-2.0 mg for pyridoxine, depending on age and sex. According to these recommendations, royal jelly is not a good source of vitamins B1, B2 or B6 as these vitamins appear only on order of ng g-1. The proposed method can be used in routine analysis for royal jelly, having the advantage of being simple, fast and reliable.

  20. Prediction of gradient retention data for hydrophilic interaction liquid chromatographic separation of native and fluorescently labeled oligosaccharides.

    Science.gov (United States)

    Vaňková, Nikola; Česla, Petr

    2017-02-17

    In this work, we have investigated the predictive properties of mixed-mode retention model and oligomeric mixed-mode model, taking into account the contribution of monomeric units to the retention, in hydrophilic interaction liquid chromatography. The gradient retention times of native maltooligosaccharides and their fluorescent derivatives were predicted in the oligomeric series with number of monomeric glucose units in the range from two to seven. The maltooligosaccharides were separated on a packed column with carbamoyl-bonded silica stationary phase and 15 gradient profiles with different initial and final mobile phase composition were used with the gradient times 5; 7.5 and 10min. The predicted gradient retention times were compared for calculations based on isocratic retention data and gradient retention data, which provided better accuracy of the results. By comparing two different mobile phase additives, the more accurate retention times were predicted in mobile phases containing ammonium acetate. The acidic derivatives, prepared by reaction of an oligosaccharide with 2-aminobenzoic acid or 8-aminonaphthalene-1,3,6-trisulfonic acid, provided more accurate predictions of the retention data in comparison to native oligosaccharides or their neutral derivatives. The oligomeric mixed-mode model allowed prediction of gradient retention times using only one gradient profile, which significantly speeded-up the method development. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Comparison of isocratic retention models for hydrophilic interaction liquid chromatographic separation of native and fluorescently labeled oligosaccharides.

    Science.gov (United States)

    Česla, Petr; Vaňková, Nikola; Křenková, Jana; Fischer, Jan

    2016-03-18

    In this work, we have investigated retention of maltooligosaccharides and their fluorescent derivatives in hydrophilic interaction liquid chromatography using four different stationary phases. The non-derivatized maltooligosaccharides (maltose to maltoheptaose) and their derivatives with 2-aminobenzoic acid, 2-aminobenzamide, 2-aminopyridine and 8-aminonaphthalene-1,3,6-trisulfonic acid were analyzed on silica gel, aminopropyl silica, amide (carbamoyl-bonded silica) and ZIC-HILIC zwitterionic sulfobetain bonded phase. The partitioning of the analytes between the bulk mobile phase and adsorbed water-rich layer, polar and ionic interactions of analytes with stationary phase have been evaluated and compared. The effects of the mobile phase additives (0.1% (v/v) of acetic acid and ammonium acetate in concentration range 5-30 mmol L(-1)) on retention were described. The suitability of different models for prediction of retention was tested including linear solvent strength model, quadratic model, mixed-mode model, and empirical Neue-Kuss model. The mixed-mode model was extended to the parameter describing the contribution of monomeric glucose unit to the retention of non-derivatized and derivatized maltooligosaccharides, which was used for evaluation of contribution of both, oligosaccharide backbone and end-group to retention. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Determination of descriptors for polycyclic aromatic hydrocarbons and related compounds by chromatographic methods and liquid-liquid partition in totally organic biphasic systems.

    Science.gov (United States)

    Ariyasena, Thiloka C; Poole, Colin F

    2014-09-26

    Retention factors on several columns and at various temperatures using gas chromatography and from reversed-phase liquid chromatography on a SunFire C18 column with various mobile phase compositions containing acetonitrile, methanol and tetrahydrofuran as strength adjusting solvents are combined with liquid-liquid partition coefficients in totally organic biphasic systems to calculate descriptors for 23 polycyclic aromatic hydrocarbons and eighteen related compounds of environmental interest. The use of a consistent protocol for the above measurements provides descriptors that are more self consistent for the estimation of physicochemical properties (octanol-water, air-octanol, air-water, aqueous solubility, and subcooled liquid vapor pressure). The descriptor in this report tend to have smaller values for the L and E descriptors and random differences in the B and S descriptors compared with literature sources. A simple atom fragment constant model is proposed for the estimation of descriptors from structure for polycyclic aromatic hydrocarbons. The new descriptors show no bias in the prediction of the air-water partition coefficient for polycyclic aromatic hydrocarbons unlike the literature values. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Development of a gas-liquid chromatographic method for the analysis of fatty acid tryptamides in cocoa products.

    Science.gov (United States)

    Hug, Bernadette; Golay, Pierre-Alain; Giuffrida, Francesca; Dionisi, Fabiola; Destaillats, Frédéric

    2006-05-03

    The determination of the occurrence and level of cocoa shells in cocoa products and chocolate is an important analytical issue. The recent European Union directive on cocoa and chocolate products (2000/36/EC) has not retained the former limit of a maximum amount of 5% of cocoa shells in cocoa nibs (based on fat-free dry matter), previously authorized for the elaboration of cocoa products such as cocoa mass. In the present study, we report a reliable gas-liquid chromatography procedure suitable for the determination of the occurrence of cocoa shells in cocoa products by detection of fatty acid tryptamides (FATs). The precision of the method was evaluated by analyzing nine different samples (cocoa liquors with different ranges of shells) six times (replicate repeatability). The variations of the robust coefficient of variation of the repeatability demonstrated that FAT(C22), FAT(C24), and total FATs are good markers for the detection of shells in cocoa products. The trueness of the method was evaluated by determining the FAT content in two spiked matrices (cocoa liquors and cocoa shells) at different levels (from 1 to 50 mg/100 g). A good relation was found between the results obtained and the spiking (recovery varied between 90 and 130%), and the linearity range was established between 1 and 50 mg/100 g in cocoa products. For total FAT contents of cocoa liquor containing 5% shells, the measurement uncertainty allows us to conclude that FAT is equal to 4.01 +/- 0.8 mg/100 g. This validated method is perfectly suitable to determine shell contents in cocoa products using FAT(C22), FAT(C24), and total FATs as markers. The results also confirmed that cocoa shells contain FAT(C24) and FAT(C22) in a constant ratio of nearly 2:1.

  4. Validation of a liquid chromatographic method for determination of related substances in a candidate certified reference material of captopril

    Directory of Open Access Journals (Sweden)

    Raquel Nogueira

    2011-06-01

    Full Text Available This paper describes the validation of a reversed-phase high performance liquid chromatography method (RP-HPLC with diode array detection (DAD for determination of related substances (impurities from organic synthesis and degradation products of captopril according to the Brazilian Pharmacopeia IV. The aim of this study was to guarantee the method accuracy for quantification of related substances, an essential requisite to determine, using the mass balance approach, the captopril content in the first Brazilian certified reference material (CRM of an active pharmaceutical ingredient (API, developed by Inmetro. The captopril instability in solution is discussed and the captopril content determined by mass balance is compared to the results from titration and differential scanning calorimetry (DSC.Este artigo descreve a validação de método de cromatografia líquida de alta eficiência em fase reversa (CLAE-RP com detector de fotodiodos (DAD para determinação de substâncias relacionadas (impurezas orgânicas de síntese e produtos de degradação de captopril segundo Farmacopéia Brasileira IV ed. Este estudo teve como objetivo garantir que o método é capaz de quantificar com exatidão o teor de substâncias relacionadas, um requisito essencial para que o teor de captopril seja determinado por balanço de massa no primeiro material de referência certificado (MRC de fármacos brasileiro, o qual foi desenvolvido pelo Inmetro. A instabilidade do captopril em solução é discutida em detalhes e o teor de captopril determinado por balanço de massa é comparado com aqueles obtidos por titulação e por calorimetria exploratória diferencial (DSC.

  5. High-performance liquid chromatographic method for the simultaneous determination of 24 fragrance allergens to study scented products.

    Science.gov (United States)

    Villa, C; Gambaro, R; Mariani, E; Dorato, S

    2007-07-27

    The European legislation on cosmetic products has recently required the declaration of 26 compounds (24 volatile chemicals and 2 natural extracts) on the label of final products when exceeding a stipulated cut-off level. In this work a rapid reliable and specific RP-HPLC method coupled with diode array detector (DAD) has been developed for the simultaneous determination and quantification of the 24 volatile chemicals: amyl cinnamal, benzyl alcohol, cinnamyl alcohol, citral, eugenol, hydroxy-citronellal, isoeugenol, amylcinnamyl alcohol, benzyl salicylate, cinnamal, coumarin, geraniol, Lyral (hydroxy-methylpentylcyclohexene carboxaldehyde), anisyl alcohol, benzyl cinnamate, farnesol, Lilial (2-(4-tert-butylbenzyl)propionaldehyde) linalool, benzyl benzoate, citronellol, hexyl cinnamal, limonene, methylheptin carbonate, alpha-isomethyl ionone (3-methyl-4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-3-buten-2-one). The 24 analytes were appropriately separated over a running time of 40 min, on a C18 column using a simple gradient elution (acetonitrile/water) with flow rate from 0.7 to 1.0 ml/min and UV acquisition at 210, 254 and 280 nm. All calibration curves showed good linearity (r2>0.99) within test ranges. The method was successfully applied to the qualitative and quantitative determination of the potential allergens in four commercial scented products, with satisfactory accuracy and precision. The results indicated that this simple and efficient method can be used for quality assessment of complex matrices such us cosmetic scented products.

  6. Liquid chromatographic-diode-array detection multiresidue determination of rice herbicides in drinking and paddy-field water.

    Science.gov (United States)

    Roehrs, Rafael; Zanella, Renato; Pizzuti, Ionara; Adaime, Martha B; Pareja, Lucía; Niell, Silvina; Cesio, María V; Heinzen, Horacio

    2009-01-01

    A sensitive, rapid, and simple multiresidue method for the simultaneous determination of six postemergence herbicides currently used in rice cultivation--metsulfuron methyl, bensulfuron methyl, pyrazosulfuron ethyl, bentazone, bispyribac sodium, and cyhalofop butyl--in drinking and paddy-field water is presented. Water samples were extracted with solid-phase extraction cartridges. Final determination was made by LC with diode-array detection. The extraction efficiencies of C18 and HLB cartridges were compared. The average recovery obtained for these compounds for the lowest spiked level (0.1 microg/L) varied from 70 to 122% for C18 and 75-119% for HLB, with RSDs of 11 and 8.3%, respectively. The method had good linearity, and the lower detection limit for the pesticides studied varied from 0.03 to 0.04 microg/L. The proposed method was also tested in paddy-field water, with recovery studies giving good results with low RSDs at 1.0 microg/L.

  7. Validated high-performance liquid chromatographic method for the standardisation of Ptychopetalum olacoides Benth., Olacaceae, commercial extracts

    Directory of Open Access Journals (Sweden)

    Renata Colombo

    2010-10-01

    Full Text Available Ptychopetalum olacoides Benth., Olacaceae, popularly known as marapuama or muirapuama or miriantã, is a species native to the Amazonian region of Brazil. Extracts of the bark of the plant have been used traditionally for its stimulating and aphrodisiac properties and currently commercialised by the herbal industry as constituents in a wide range of phytomedicines. Fractionation by open column chromatography followed by preparative HPLC-UV/PAD of the stem bark and of three commercial extracts of P. olacoides allowed the isolation of three components that were common to all extracts analysed, and these were identified by NMR to be vanillic acid, protocatechuic acid and theobromine. Vanillic acid, which has been proposed as a phytochemical marker for P. olacoides, was employed as an external standard in the development and validation of a rapid qualitative and quantitative HPLC assay for the analyte. The recoveries values of the developed method were 99.02% and the LOD and LOQ values were 0.033 and 0.11 mg.L-1, respectively. The described method may be applied to the standardisation of herbs, extracts or phytomedicines commercialised as marapuama.

  8. Liquid-liquid and solid-phase extractions of phenols from virgin olive oil and their separation by chromatographic and electrophoretic methods.

    Science.gov (United States)

    Bendini, Alessandra; Bonoli, Matteo; Cerretani, Lorenzo; Biguzzi, Barbara; Lercker, Giovanni; Toschi, Tullia Gallina

    2003-01-24

    The high oxidative stability of virgin olive oil is related to its high monounsaturated/polyunsaturated ratio and to the presence of antioxidant compounds, such as tocopherols and phenols. In this paper, the isolation of phenolic compounds from virgin olive oil, by different methods, was tested and discussed. Particularly liquid-liquid and solid-phase extraction methods were compared, assaying, for the latter, three stationary phases (C8, C18 and Diol) and several elution mixtures. Quantification of phenolic and o-diphenolic substances in the extracts was performed by the traditional Folin-Ciocalteau method and the sodium molybdate reaction, respectively. Furthermore, the quantification of phenolic compounds in the extracts and in a standard mixture was carried out both with diode array and mass spectrometric detection and capillary zone electrophoresis.

  9. Quality by Design approach in the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol and its impurities.

    Science.gov (United States)

    Jovanović, Marko; Rakić, Tijana; Tumpa, Anja; Jančić Stojanović, Biljana

    2015-06-10

    This study presents the development of hydrophilic interaction liquid chromatographic method for the analysis of iohexol, its endo-isomer and three impurities following Quality by Design (QbD) approach. The main objective of the method was to identify the conditions where adequate separation quality in minimal analysis duration could be achieved within a robust region that guarantees the stability of method performance. The relationship between critical process parameters (acetonitrile content in the mobile phase, pH of the water phase and ammonium acetate concentration in the water phase) and critical quality attributes is created applying design of experiments methodology. The defined mathematical models and Monte Carlo simulation are used to evaluate the risk of uncertainty in models prediction and incertitude in adjusting the process parameters and to identify the design space. The borders of the design space are experimentally verified and confirmed that the quality of the method is preserved in this region. Moreover, Plackett-Burman design is applied for experimental robustness testing and method is fully validated to verify the adequacy of selected optimal conditions: the analytical column ZIC HILIC (100 mm × 4.6 mm, 5 μm particle size); mobile phase consisted of acetonitrile-water phase (72 mM ammonium acetate, pH adjusted to 6.5 with glacial acetic acid) (86.7:13.3) v/v; column temperature 25 °C, mobile phase flow rate 1 mL min(-1), wavelength of detection 254 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. A validated stability-indicating high performance liquid chromatographic method for moxifloxacin hydrochloride and ketorolac tromethamine eye drops and its application in pH dependent degradation kinetics

    Directory of Open Access Journals (Sweden)

    Jayant B Dave

    2013-01-01

    Full Text Available Background and Aim: A fixed dose combination of moxifloxacin hydrochloride and ketorolac tromethamine is used in ratio of 1:1 as eye drops for the treatment of the reduction of post operative inflammatory conditions of the eye. A simple, precise, and accurate High Performance Liquid Chromatographic (HPLC method was developed and validated for determination of moxifloxacin hydrochloride and ketorolac tromethamine in eye drops. Materials and Methods: Isocratic HPLC separation was achieved on a ACE C 18 column (C 18 (5 μm, 150 mm×4.6 mm, i.d. using the mobile phase 10 mM potassium di-hydrogen phosphate buffer pH 4.6-Acetonitrile (75:25 v/v at a flow rate of 1.0 mL/min. The detection was performed at 307 nm. Drugs were subjected to acid, alkali and neutral hydrolysis, oxidation and photo degradation. Moreover, the proposed HPLC method was utilized to investigate the pH dependent degradation kinetics of moxifloxacin hydrochloride and ketorolac tromethamine in buffer solutions at different pH values like 2.0, 6.8 and 9.0. Results and Conclusion: The retention time (t R of moxifloxacin hydrochloride and ketorolac tromethamine were 3.81±0.01 and 8.82±0.02 min, respectively. The method was linear in the concentration range of 2-20 μ/mL each for moxifloxacin hydrochloride and ketorolac tromethamine with a correlation coefficient of 0.9996 and 0.9999, respectively. The method was validated for linearity, precision, accuracy, robustness, specificity, limit of detection and limit of quantitation. The drugs could be effectively separated from different degradation products and hence the method can be used for stability analysis. Different kinetics parameters like apparent first-order rate constant, half-life and t 90 (time for 90% potency left were calculated.

  11. Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

    Directory of Open Access Journals (Sweden)

    Serpil Sevim

    2015-12-01

    Full Text Available abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4 and acetonitrile (35:65 by volume. The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL and limit of quantification (50 ng/mL were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000. In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.

  12. Validated stability indicating liquid chromatographic determination of ebastine in pharmaceuticals after pre column derivatization: Application to tablets and content uniformity testing

    Directory of Open Access Journals (Sweden)

    Eid Manal

    2011-05-01

    Full Text Available Abstract An accurate, simple, sensitive and selective reversed phase liquid chromatographic method has been developed for the determination of ebastine in its pharmaceutical preparations. The proposed method depends on the complexation ability of the studied drug with Zn2+ ions. Reversed phase chromatography was conducted using an ODS C18 (150 × 4.6 mm id stainless steel column at ambient temperature with UV-detection at 260 nm. A mobile phase containing 0.025%w/v Zn2+ in a mixture of (acetonitril/methanol; 1/4 and Britton Robinson buffer (65:35, v/v adjusted to pH 4.2, has been used for the determination of ebastine at a flow rate of 1 ml/min. The calibration curve was rectilinear over the concentration range of 0.3 - 6.0 μg/ml with a detection limit (LOD of 0.13 μg/ml, and quantification limit (LOQ of 0.26 μg/ml. The proposed method was successfully applied for the analysis of ebastine in its dosage forms, the obtained results were favorably compared with those obtained by a comparison method. Furthermore, content uniformity testing of the studied pharmaceutical formulations was also conducted. The composition of the complex as well as its stability constant was also investigated. Moreover, the proposed method was found to be a stability indicating one and was utilized to investigate the kinetics of alkaline and ultraviolet induced degradation of the drug. The first-order rate constant and half life of the degradation products were calculated.

  13. A validated high-performance liquid chromatographic method for the determination of glibenclamide in human plasma and its application to pharmacokinetic studies.

    Science.gov (United States)

    Niopas, Ioannis; Daftsios, Athanasios C

    2002-05-15

    Glibenclamide is a potent second generation oral sulfonylurea antidiabetic agent widely used for the treatment of type II diabetes melitus. A rapid, sensitive, precise, accurate and specific HPLC assay for the determination of glibenclamide in human plasma was developed and validated. After addition of flufenamic acid as internal standard, the analytes were isolated from human plasma by liquid-liquid extraction. The method was linear in the 10-400 ng/ml concentration range (r > 0.999). Recovery for glibenclamide was greater than 91.5% and for internal standard was 93.5%. Within-day and between-day precision, expressed as the relative standard deviation (RSD%), ranged from 1.4 to 5.9% and 5.8 to 6.6%, respectively. Assay accuracy was better than 93.4%. The assay was used to estimate the pharmacokinetics of glibenclamide after oral administration of a 5 mg tablet of glibenclamide to 18 healthy volunteers.

  14. Ionic liquid-based single-drop microextraction/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene and xylene isomers in waters.

    Science.gov (United States)

    Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2008-08-01

    The direct coupling between ionic liquid-based single-drop microextraction and gas chromatography/mass spectrometry is proposed for the rapid and simple determination of benzene, toluene, ethylbenzene and xylenes isomers (BTEX) in water samples. The extraction procedure exploits not only the high affinity of the selected ionic liquid (1-methyl-3-octyl-imidazolium hexaflourophosphate) to these aromatic compounds but also its special properties like viscosity, low vapour pressure and immiscibility with water. All the variables involved in the extraction process have been studied in depth. The developed method allows the determination of these single-ring compounds in water under the reference concentration level fixed by the international legislation. In this case, limits of detection were in the range 20 ng L(-1) (obtained for benzene) and 91 ng L(-1) (for o-xylene). The repeatability of the proposed method, expressed as RSD (n=5), varied between 3.0% (o-xylene) and 5.2% (toluene).

  15. Rapid determination of methadone and its major metabolite in biological fluids by gas-liquid chromatography with thermionic detection for maintenance treatment of opiate addicts.

    Science.gov (United States)

    Chikhi-Chorfi, N; Pham-Huy, C; Galons, H; Manuel, N; Lowenstein, W; Warnet, J M; Claude, J R

    1998-11-06

    A rapid gas-liquid chromatographic assay is developed for the quantification of methadone (Mtd) and its major metabolite, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), in biological fluids of opiate addicts. After alkaline extraction from samples with lidocaine hydrochloride as internal standard, Mtd and EDDP are separated on SP-2250 column at 220 degrees C and detected with a thermionic detector. The chromatographic time is about 6 min. The relative standard deviations (R.S.D.) of Mtd and EDDP standards are between 1.5 and 5.5%. Most drugs of abuse (morphine, codeine, narcotine, cocaine, benzoylecgonine, cocaethylene, dextropropoxyphene etc) are shown not to interfere with this technique. The method has been applied to study the levels of Mtd and EDDP metabolite in serum, saliva and urine of patients under maintenance treatment for opiate dependence. EDDP levels were found higher than those of Mtd in urine samples from four treated patients, but lower in serum and undetectable in saliva. However, Mtd concentrations were higher in saliva than in serum.

  16. A simple and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method to determine plasma biotin in hemodialysis patients.

    Science.gov (United States)

    Yagi, Shigeaki; Nishizawa, Manabu; Ando, Itiro; Oguma, Shiro; Sato, Emiko; Imai, Yutaka; Fujiwara, Masako

    2016-08-01

    A simple, rapid, and selective method for determination of plasma biotin was developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After single-step protein precipitation with methanol, biotin and stable isotope-labeled biotin as an internal standard (IS) were chromatographed on a pentafluorophenyl stationary-phase column (2.1 × 100 mm, 2.7 μm) under isocratic conditions using 10 mm ammonium formate-acetonitrile (93:7, v/v) at a flow rate of 0.6 mL/min. The total chromatographic runtime was 5 min for each injection. Detection was performed in a positive electrospray ionization mode by monitoring selected ion transitions at m/z 245.1/227.0 and 249.1/231.0 for biotin and the IS, respectively. The calibration curve was linear in the range of 0.05-2 ng/mL using 300 μL of plasma. The intra- and inter-day precisions were all biotin concentrations in hemodialysis patients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction

    International Nuclear Information System (INIS)

    Chisvert, Alberto; Benedé, Juan L.; Anderson, Jared L.; Pierson, Stephen A.; Salvador, Amparo

    2017-01-01

    With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67–791), limits of detection (low ng L −1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87–113%, 91–117% and 89–115% for river, sea and swimming pool water samples, respectively). - Highlights: • A new microextraction method combining the

  18. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Vortex-assisted liquid-liquid microextraction for the rapid screening of short-chain chlorinated paraffins in water.

    Science.gov (United States)

    Chang, Chia-Yu; Chung, Wu-Hsun; Ding, Wang-Hsien

    2016-01-01

    The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Liquid chromatographic studies on the behaviour of Pu(III), Pu(IV) and Pu(VI) on a RP stationary phase in presence of α-hydroxyisobutyric acid as a chelating agent

    Energy Technology Data Exchange (ETDEWEB)

    Jaison, P.G.; Kumar, Pranaw; Telmore, Vijay M. [Bhabha Atomic Research Centre, Mumbai (India). Fuel Chemistry Division

    2017-06-01

    Since plutonium possesses multiple oxidation states which can coexist in solution, a method for the identification of these oxidation states is important to understand its chemical processes. Liquid chromatographic studies were carried out to compare the chromatographic behaviour of different oxidation states of Pu in presence of the eluent, α-hydroxyisobutyric acid (HIBA). The three oxidation states of Pu viz. Pu(III), Pu(IV) and Pu(VI) were separated under optimised conditions. It was seen that the presence of the complexing agent influences the equilibrium of Pu(III)/(IV) as well as Pu(IV)/(VI) systems. Pu(III) to Pu(IV) conversion was found to be enhanced by high pH and concentration of HIBA whereas a relatively low pH and high concentration of HIBA promotes the conversion of Pu(VI) to Pu(IV).

  1. Ionic Liquid-Bonded Fused Silica as a New Solid-Phase Microextraction Fiber for the Liquid Chromatographic Determination of Bisphenol A as an Endocrine Disruptor.

    Science.gov (United States)

    Mohammadnezhad, Nasim; Matin, Amir Abbas; Samadi, Naser; Shomali, Ashkan; Valizadeh, Hassan

    2017-01-01

    Linear ionic liquid bonded to fused silica and its application as a solid-phase microextraction fiber for the extraction of bisphenol A (BPA) from water samples were studied. After optimization of microextraction conditions (15 mL sample volume, extraction time of 40 min, extraction temperature of 30 ± 1°C, 300 μL acetonitrile as the desorption solvent, and desorption time of 7 min), the fiber was used to extract BPA from packed mineral water, followed by HPLC-UV on an XDB-C18 column (150 × 4.6 mm id, 3.5 μm particle) with a mobile phase of acetonitrile-water (45 + 55%, v/v) and flow rate of 1 mL . min-1). A low LOD (0.20 μg . L-1) and good linearity (0.9977) in the calibration graph indicated that the proposed method was suitable for the determination of BPA.

  2. Liquid chromatographic determination of water

    Science.gov (United States)

    Fortier, N.E.; Fritz, J.S.

    1990-11-13

    A sensitive method for the determination of water in the presence of common interferences is presented. The detection system is based on the effect of water on the equilibrium which results from the reaction aryl aldehydes, such as cinnamaldehyde and methanol in the eluent to form cinnamaldehyde dimethylacetal, plus water. This equilibrium is shifted in a catalytic atmosphere of a hydrogen ion form past column reactor. The extent of the shift and the resulting change in absorbance are proportional to the amount of water present. 1 fig.

  3. Rapid thin-layer chromatographic photodensitometric method for the determination of metoclopramide and clebopride in the presence of some of their metabolic products.

    Science.gov (United States)

    Huizing, G; Beckett, A H; Segura, J

    1979-04-21

    Metoclopramide and its newly developed analogue clebopride, together with some of their metabolic products are quantitated, following extraction from biological tissues and fluids, and subsequent separation on silica gel thin-layer chromatographic plates. Diazotisation, followed by coupling with N-(1-naphthyl)ethylenediammonium dichloride, carried out on the thin-layer plate, is utilised for visualisation. The intensity of the spots is measured by photodensitometric analysis. The effect of variation of various experimental conditions is studied. The method has proven to be satisfactory for the measurement of 20 ng/ml of these compounds in biological material; the results are well within the accepted limits of deviation.

  4. Study of matrix effects on the direct trace analysis of acidic pesticides in water using various liquid chromatographic modes coupled to tandem mass spectrometric detection.

    Science.gov (United States)

    Dijkman, E; Mooibroek, D; Hoogerbrugge, R; Hogendoorn, E; Sancho, J V; Pozo, O; Hernández, F

    2001-08-10

    This study investigated the effects of matrix interferences on the analytical performance of a triple quadrupole mass spectrometric (MS-MS) detector coupled to various reversed-phase liquid chromatographic (LC) modes for the on-line determination of various types of acidic herbicides in water using external calibration for quantification of the analytes tested at a level of 0.4 microg/l. The LC modes included (i) a single-column configuration (LC), (ii) precolumn switching (PC-LC) and (iii) coupled-column LC (LC-LC). As regards detection, electrospray (ESI) and atmospheric pressure chemical ionization (APCI) in both positive (PI) and negative (NI) ionization modes were examined. Salinity and dissolved organic carbon (DOC) were selected as interferences to study matrix effects in this type of analysis. Therefore, Milli-Q and tap water samples both fortified with 12 mg/l DOC and spiked with sulfometuron-methyl, bentazone, bromoxynil, 2-methyl-4-chlorophenoxyacetic acid, and 2-methyl-4-chlorophenoxypropionic acid at a level of about 0.4 microg/l were analyzed with the various LC-MS approaches. Direct sample injection was performed with volumes of 0.25 ml or 2.0 ml on a column of 2.1 mm I.D. or 4.6 mm I.D. for the ESI and APCI modes, respectively. The recovery data were used to compare and evaluate the analytical performance of the various LC approaches. As regards matrix effects, the salinity provided a dramatic decrease in response for early eluting analytes (k value of about 1) when using the LC mode. Both PC-LC and LC-LC efficiently eliminated this problem. The high DOC content hardly effected the responses of analytes in the ESI mode, while in most cases the responses increased when using APCI-MS-MS detection. Of all the tested configurations, LC-LC-ESI-MS-MS with the column combination Discovery C18/ABZ+ was the most favorable as regards elimination of matrix effects and provided reliable quantification of all compounds using external calibration at the tested

  5. Synthesis and application of a macroporous silica-based polymeric octyl(phenyl)-N,N-diisobutylcarbamoylmethylphoshine oxide composite for the chromatographic separation of high level liquid waste

    International Nuclear Information System (INIS)

    Zhang, A.

    2006-01-01

    The Minor Actinides Recovery from HLW by Extraction Chromatography (MAREC) process was used mainly for the separation of minor actinides (MAs) and some specific fission products (FPs) from highly active liquid waste (HLW) by the composite CMPO/SiO 2 -P of the macroporous silica based polymeric octyl(phenyl)-N,N-diisobutylcarbamoylmethylphoshine oxide (CMPO) and others. In this study a cascade of chromatographic separation was performed on a 3.0M HNO 3 solution containing 5.0 x 10 -3 M of 13 elements, at 323 K. The cascade consisted of three columns the first and second ones were packed with CMPO/SiO 2 -P and the third with SiO 2 -P particles. The first column was employed to prepare various eluents containing saturated CMPO. The second column was used for separation into groups. The CMPO of CMPO/SiO2-P was recovered from the effluent by the third column and a CMPO-free effluent containing minor actinides was obtained. The elements contained in the simulated HLW of 3.0M HNO 3 were separated into (1) a non-adsorption group (Sr, Cs, and Ru etc.), (2) a MA-hRE (heavy rare earth)-Mo-Zr group, and (3) a lRE (light rare earth) group by eluting with 3.0M HNO 3 , 0.05M DTPA (diethylenetriaminepentaacetic acid) (pH 2.0) and HNO 3 (pH 3.5), respectively. The resultant MA-hRE-Mo-Zr mixture containing minor actinides was then separated into the groups (1) Pd-Ru, (2) MA-hRE, and (3) Mo-Zr by utilizing 3.0M HNO 3 , distilled water, and 0.05M DTPA (pH 2.0) as eluents. More than 92% of CMPO in the MA-hRE containing effluent was adsorbed by SiO 2 -P particles. The effectivity and technical feasibility of MAREC process were demonstrated. (author)

  6. Homogeneous nucleation ahead of the solid-liquid interface during rapid solidification of binary alloys

    International Nuclear Information System (INIS)

    Smith, P.M.; Elmer, J.W.

    1996-01-01

    In recent rapid solidification experiments on Al-5%Be alloys, a Liquid Phase Nucleation (LPN) model was developed to explain the formation of periodic arrays of randomly-oriented Be-rich particles in an Al-rich matrix. In the LPN model, Be droplets were assumed to nucleate in the liquid ahead of the solid-liquid interface, but no justification for this was given. Here the authors present a model which considers the geometric constraints (imposed by proximity to the interface) on the number of solute atoms available to form a nucleus. Calculations based on this model predict that nucleation of second-phase particles can be most likely a short distance ahead of the interface in immiscible binary systems such as Al-Be. As part of the nucleation calculations, a semi-empirical method of calculating solid-liquid surface tensions in binary systems was developed, and is presented in the Appendix

  7. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Freese, R.; Cornett, C.

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved...

  8. Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

    2011-04-01

    In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Development of a validated liquid chromatographic method for quantification of sorafenib tosylate in the presence of stress-induced degradation products and in biological matrix employing analytical quality by design approach.

    Science.gov (United States)

    Sharma, Teenu; Khurana, Rajneet Kaur; Jain, Atul; Katare, O P; Singh, Bhupinder

    2018-05-01

    The current research work envisages an analytical quality by design-enabled development of a simple, rapid, sensitive, specific, robust and cost-effective stability-indicating reversed-phase high-performance liquid chromatographic method for determining stress-induced forced-degradation products of sorafenib tosylate (SFN). An Ishikawa fishbone diagram was constructed to embark upon analytical target profile and critical analytical attributes, i.e. peak area, theoretical plates, retention time and peak tailing. Factor screening using Taguchi orthogonal arrays and quality risk assessment studies carried out using failure mode effect analysis aided the selection of critical method parameters, i.e. mobile phase ratio and flow rate potentially affecting the chosen critical analytical attributes. Systematic optimization using response surface methodology of the chosen critical method parameters was carried out employing a two-factor-three-level-13-run, face-centered cubic design. A method operable design region was earmarked providing optimum method performance using numerical and graphical optimization. The optimum method employed a mobile phase composition consisting of acetonitrile and water (containing orthophosphoric acid, pH 4.1) at 65:35 v/v at a flow rate of 0.8 mL/min with UV detection at 265 nm using a C 18 column. Response surface methodology validation studies confirmed good efficiency and sensitivity of the developed method for analysis of SFN in mobile phase as well as in human plasma matrix. The forced degradation studies were conducted under different recommended stress conditions as per ICH Q1A (R2). Mass spectroscopy studies showed that SFN degrades in strongly acidic, alkaline and oxidative hydrolytic conditions at elevated temperature, while the drug was per se found to be photostable. Oxidative hydrolysis using 30% H 2 O 2 showed maximum degradation with products at retention times of 3.35, 3.65, 4.20 and 5.67 min. The absence of any

  10. Experimental observations of flow instabilities and rapid mixing of two dissimilar viscoelastic liquids

    Directory of Open Access Journals (Sweden)

    Hiong Yap Gan

    2012-12-01

    Full Text Available Viscoelastically induced flow instabilities, via a simple planar microchannel, were previously used to produce rapid mixing of two dissimilar polymeric liquids (i.e. at least a hundredfold different in shear viscosity even at a small Reynolds number. The unique advantage of this mixing technology is that viscoelastic liquids are readily found in chemical and biological samples like organic and polymeric liquids, blood and crowded proteins samples; their viscoelastic properties could be exploited. As such, an understanding of the underlying interactions will be important especially in rapid microfluidic mixing involving multiple-stream flow of complex (viscoelastic fluids in biological assays. Here, we use the same planar device to experimentally show that the elasticity ratio (i.e. the ratio of stored elastic energy to be relaxed between two liquids indeed plays a crucial role in the entire flow kinematics and the enhanced mixing. We demonstrate here that the polymer stretching dynamics generated in the upstream converging flow and the polymer relaxation events occurring in the downstream channel are not exclusively responsible for the transverse flow mixing, but the elasticity ratio is also equally important. The role of elasticity ratio for transverse flow instability and the associated enhanced mixing were illustrated based on experimental observations. A new parameter Deratio = Deside / Demain (i.e. the ratio of the Deborah number (De of the sidestream to the mainstream liquids is introduced to correlate the magnitude of energy discontinuity between the two liquids. A new Deratio-Demain operating space diagram was constructed to present the observation of the effects of both elasticity and energy discontinuity in a compact manner, and for a general classification of the states of flow development.

  11. Liquid chromatographic-tandem mass spectrometric method for the simultaneous determination of alkylphenols polyethoxylates, alkylphenoxy carboxylates and alkylphenols in wastewater and surface-water.

    Science.gov (United States)

    Ciofi, L; Ancillotti, C; Chiuminatto, U; Fibbi, D; Checchini, L; Orlandini, S; Del Bubba, M

    2014-10-03

    Four different pellicular stationary phases (i.e. octadecylsilane, octasilane, Phenyl-Hexyl and pentafluorophenyl) were investigated for the chromatographic resolution of alkylphenols (APs), alkylphenols polyethoxylates (APnEOs) and alkylphenoxy carboxylates (APECs) using mixtures of water and organic solvents (i.e. methanol, acetonitrile and tetrahydrofuran) as eluents, in order to obtain their determination by a single LC-MS/MS run. In fact, alkylphenols and alkylphenoxy carboxylates must be analysed in negative ion mode, whereas alkylphenols polyethoxylates undergo ionisation only in positive ion mode, and therefore, two distinct LC-MS/MS analysis are commonly adopted. The best resolution among the aforementioned target analytes was achieved on the pentafluorophenyl column, eluting with an acidified water-acetonitrile-tetrahydrofuran mixture and using the post column addition of an ammonia solution in methanol for the detection of positively ionisable compounds. Under these optimized chromatographic conditions the investigated compounds were determined via a single chromatographic run, with only one polarity switch, in 15min, achieving the following instrumental detection limits: 600pg for AP1EOs, 0.8-14pg for AP2EOs, 10.4-150pg for APs and 4.4-4.8pg for APECs. The chromatographic method was coupled with solid-phase extraction and clean-up procedures and successfully applied to the analysis of wastewater and surface water samples, highlighting mean concentration ranging from 6ng/L for 4-t-OP1EC to 1434ng/L for 4-NP1121EC, depending on the sample analysed. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

    2017-05-01

    Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. A new modeling strategy for third-order fast high-performance liquid chromatographic data with fluorescence detection. Quantitation of fluoroquinolones in water samples.

    Science.gov (United States)

    Alcaráz, Mirta R; Bortolato, Santiago A; Goicoechea, Héctor C; Olivieri, Alejandro C

    2015-03-01

    Matrix augmentation is regularly employed in extended multivariate curve resolution-alternating least-squares (MCR-ALS), as applied to analytical calibration based on second- and third-order data. However, this highly useful concept has almost no correspondence in parallel factor analysis (PARAFAC) of third-order data. In the present work, we propose a strategy to process third-order chromatographic data with matrix fluorescence detection, based on an Augmented PARAFAC model. The latter involves decomposition of a three-way data array augmented along the elution time mode with data for the calibration samples and for each of the test samples. A set of excitation-emission fluorescence matrices, measured at different chromatographic elution times for drinking water samples, containing three fluoroquinolones and uncalibrated interferences, were evaluated using this approach. Augmented PARAFAC exploits the second-order advantage, even in the presence of significant changes in chromatographic profiles from run to run. The obtained relative errors of prediction were ca. 10 % for ofloxacin, ciprofloxacin, and danofloxacin, with a significant enhancement in analytical figures of merit in comparison with previous reports. The results are compared with those furnished by MCR-ALS.

  14. Validated determination of losartan and valsartan in human plasma by stir bar sorptive extraction based on acrylate monolithic polymer, liquid chromatographic analysis and experimental design methodology.

    Science.gov (United States)

    Babarahimi, Vida; Talebpour, Zahra; Haghighi, Farideh; Adib, Nuoshin; Vahidi, Hamed

    2018-05-10

    In our previous work, a new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The formulation of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer was optimized and the satisfactory quality of prepared coated stir bar was demonstrated. In this work, the prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of losartan (LOS) and valsartan (VAS) in human plasma samples. In a comparison study, the extraction efficiency of the prepared stir bar was accompanied much higher extraction efficiency than the two commercial stir bars (polydimethylsiloxand and polyacrylate) for both target compounds. In order to improve the desorption efficiency of LOS and VAS, the best values for effective parameters on desorption step were selected systematically. Also, the effective parameters on extraction step were optimized using a Box-Behnken design. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for LOS (24-1000 ng mL -1 ) and VAS (91-1000 ng mL -1 ), with correlation coefficients of 0.9998 and 0.9971 and detection limits of 7 and 27 ng mL -1 , respectively. The intra- and inter-day recovery ranged from 98 to 117%, and the relative standard deviations were less than 8%. Finally, the proposed technique was successfully applied to the analysis of LOS and VAS at their therapeutic levels in volunteer patient plasma sample. The obtained results were confirmed using liquid chromatography-mass spectrometry. The proposed technique was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of LOS and VLS in

  15. Development and validation of ultra-performance liquid chromatographic method with tandem mass spectrometry for determination of lenalidomide in rabbit and human plasma

    Directory of Open Access Journals (Sweden)

    Iqbal Muzaffar

    2013-01-01

    Full Text Available Abstract Background Lenalidomide (LND is a potent novel thalidomide analog which demonstrated remarkable clinical activity in treatment of multiple myeloma disease via a multiple-pathways mechanism. Validated sensitive method with high throughput is required for the determination of lenalidomide for pharmacokinetics and toxicokinetic studies. Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS is a preeminent analytical tool for rapid biomedical analysis. Results A simple, highly sensitive UPLC-MS/MS method was developed and validated for the determination of LND in rabbit and human plasma. After a simple protein precipitation using methanol, LND and carbamazepine (IS were separated on Acquity UPLC BEH™ C18 column (50 × 2.1 mm, i.d. 1.7 μm, Waters, USA using a mobile phase consisted of acetonitrile:water:formic acid (65:35:0.1%, v/v/v pumped at a flow rate of 0.2 mL/min. LND and IS were eluted at 0.71 and 1.92 min, respectively. The mass spectrometric determination was carried out using an electrospray interface operated in the positive mode with multiple reaction monitoring (MRM mode. The precursor to product ion transitions of m/z 260.1 > 149.0 and m/z 237.0 > 179.0 were used to quantify LND and IS, respectively. The method was linear in the concentration range of 0.23–1000 ng/mL with a limit of quantitation of 0.23 ng/mL. All the validation parameters were in the ranges acceptable by the guidelines of analytical method validation. Conclusion The proposed UPLC-MS/MS method is simple, rapid and highly sensitive, and hence it could be reliable for pharmacokinetic and toxicokinetic study in both animals and humans.

  16. Rapid hydrogen hydrate growth from non-stoichiometric tuning mixtures during liquid nitrogen quenching.

    Science.gov (United States)

    Grim, R Gary; Kerkar, Prasad B; Sloan, E Dendy; Koh, Carolyn A; Sum, Amadeu K

    2012-06-21

    In this study the rapid growth of sII H(2) hydrate within 20 min of post formation quenching towards liquid nitrogen (LN(2)) temperature is presented. Initially at 72 MPa and 258 K, hydrate samples would cool to the conditions of ~60 MPa and ~90 K after quenching. Although within the stability region for H(2) hydrate, new hydrate growth only occurred under LN(2) quenching of the samples when preformed hydrate "seeds" of THF + H(2) were in the presence of unconverted ice. The characterization of hydrate seeds and the post-quenched samples was performed with confocal Raman spectroscopy. These results suggest that quenching to LN(2) temperature, a common preservation technique for ex situ hydrate analysis, can lead to rapid unintended hydrate growth. Specifically, guest such as H(2) that may otherwise need sufficiently long induction periods to nucleate, may still experience rapid growth through an increased kinetic effect from a preformed hydrate template.

  17. Simultaneous high-performance liquid chromatographic determination of nitrate, nitrite, and organic pesticides in soil solution using a multidimensional column with ultraviolet detection

    International Nuclear Information System (INIS)

    Nkedi-Kizza, P.; Owusu-Yaw, J.

    1992-01-01

    In many fertilizer trials, the amount of nitrate-nitrogen in soil solution must be quantified frequently because nitrate is easily leached. Because pesticides are generally applied to cropland with fertilizers, quantitative information is needed on the concentration of these chemicals still available in the soil. Information on nitrite, nitrate and pesticide concentrations in food, water and environmental samples is essential because of their toxicity and potential for groundwater and surface water contamination. Most of the methods currently used for nitrate determination also account for nitrite, because nitrite and some organics act as interferences. Some of the existing analytical methods require sample reduction or derivatization, complex solvent mixtures or large sample volumes which make analysis times long. A High-Performance Liquid Chromatography (HPLC) method has been developed for the simultaneous determination of nitrate, nitrite and organic pesticides in soil solution samples and extracts using a multidimensional separator column with ultraviolet detection at 220 nm. The method is rapid and requires small sample volumes (20 μL). It is a sensitive method which is suitable for routine analyses of up to 100 samples per day. A comparison of this method with standard ion chromatography with conductivity detection showed very good agreement between the two methods for the analysis of NO3- and NO2-

  18. Simultaneous high-performance liquid chromatographic analysis of pregabalin, gabapentin and vigabatrin in human serum by precolumn derivatization with o-phtaldialdehyde and fluorescence detection.

    Science.gov (United States)

    Vermeij, T A C; Edelbroek, P M

    2004-10-25

    A rapid, simple and robust method is presented for the simultaneous determination of the gamma-amino-n-butyric acid (GABA) derivatives pregabalin (PGB), gabapentin (GBP) and vigabatrin (VGB) in human serum by high-performance liquid chromatography (HPLC). Serum is deproteinized with trichloroacetic acid and aliquots of the supernatant are precolumn derivatized with o-phtaldialdehyde (OPA) and 3-mercaptopropionic acid. Separation is achieved on a Alltima 3C18 column using isocratic elution; the drugs are monitored using fluorescence detection. Norvaline is used as an internal standard. Within-day precision (COV; n = 10) is 1.2% for PGB (serum concentration 10.0 mg/l), 1.1% for GBP (serum concentration 15.8 mg/l) and 0.3% for VGB (serum concentration 15.5 mg/l). The method is linear up to at least 63 mg/l for PGB, 40 mg/l for GBP and 62 mg/l for VGB. Lower limits of quantitation (LOQ) are 0.13 mg/l for PGB, 0.53 mg/l for GBP and 0.06 mg/l for VGB. No interferences were found from commonly coadministered antiepileptic drugs (AEDs) and from endogenous amino acids. Experimental design in combination with statistical evaluation (ANOVA) was used to study the robustness of chromatography and sample preparation. The method is very suitable for routine therapeutic drug monitoring and for pharmacokinetic studies.

  19. Rapid Screening and Characterization of Acetylcholinesterase Inhibitors from Yinhuang Oral Liquid Using Ultrafiltration-liquid Chromatography-electrospray Ionization Tandem Mass Spectrometry.

    Science.gov (United States)

    Zhang, Haomin; Guo, Yinan; Meng, Lingwen; Sun, Hui; Yang, Yinping; Gao, Ying; Sun, Jiaming

    2018-01-01

    At present, approximately 17-25 million people in the world suffer from Alzheimer's disease (AD). The most efficacious and acceptable therapeutic drug clinically are the acetylcholinesterase inhibitors (AChEIs). Yinhuang oral liquid is a Chinese medicine preparation which contains AChEIs according to the literatures. However, no strategy has been presented for rapid screening and identification of AChEIs from Yinhuang oral liquid. To develop a method for rapid screening and identification of AChEIs from Yinhuang oral liquid using ultrafiltration-liquid chromatography-electrospray ionization tandem mass spectrometry (UF-LC-ESI-MS/MS). In this study, UF incubation conditions such as enzyme concentration, incubation time, and incubation temperature were optimized so as to get better screening results. The AChEIs from Yinhuang oral liquid were identified by high-performance liquid chromatography-ESI-MS and the improved Ellman method was used for the AChE inhibitory activity test in vitro . The results showed that Yinhuang oral liquid can inhibit the activity of AChE. We screened and identified seven compounds with potential AChE inhibitory activity from Yinhuang oral liquid, which provided experimental basis for the treatment and prevention of AD. The current technique was used to directly screen the active ingredients with acetylcholinesterase inhibition from complex traditional Chinese medicine, which was simple, rapid, accurate, and suitable for high-throughput screening of AChEI from complex systems. A UF-LC-ESI-MS/MS method for rapid screening and identification of AChEIs from Yinhuang oral liquid was developedSeven compounds were screened and identified with potential AChE inhibitory activity from Yinhuang oral liquidIt provided experimental basis of Yinhuang oral liquid for the treating and preventing AD. Abbreviations used: (AD): Alzheimer's disease; (UF-LC-ESI-MS/MS): ultrafiltration-liquid chromatography-electrospray ionization tandem mass spectrometry; (ACh

  20. Rapid Screening and Characterization of Acetylcholinesterase Inhibitors from Yinhuang Oral Liquid Using Ultrafiltration-liquid Chromatography-electrospray Ionization Tandem Mass Spectrometry

    Science.gov (United States)

    Zhang, Haomin; Guo, Yinan; Meng, Lingwen; Sun, Hui; Yang, Yinping; Gao, Ying; Sun, Jiaming

    2018-01-01

    Background: At present, approximately 17–25 million people in the world suffer from Alzheimer's disease (AD). The most efficacious and acceptable therapeutic drug clinically are the acetylcholinesterase inhibitors (AChEIs). Yinhuang oral liquid is a Chinese medicine preparation which contains AChEIs according to the literatures. However, no strategy has been presented for rapid screening and identification of AChEIs from Yinhuang oral liquid. Objective: To develop a method for rapid screening and identification of AChEIs from Yinhuang oral liquid using ultrafiltration–liquid chromatography–electrospray ionization tandem mass spectrometry (UF-LC-ESI-MS/MS). Materials and Methods: In this study, UF incubation conditions such as enzyme concentration, incubation time, and incubation temperature were optimized so as to get better screening results. The AChEIs from Yinhuang oral liquid were identified by high-performance liquid chromatography-ESI-MS and the improved Ellman method was used for the AChE inhibitory activity test in vitro. Results: The results showed that Yinhuang oral liquid can inhibit the activity of AChE. We screened and identified seven compounds with potential AChE inhibitory activity from Yinhuang oral liquid, which provided experimental basis for the treatment and prevention of AD. Conclusion: The current technique was used to directly screen the active ingredients with acetylcholinesterase inhibition from complex traditional Chinese medicine, which was simple, rapid, accurate, and suitable for high-throughput screening of AChEI from complex systems. SUMMARY A UF-LC-ESI-MS/MS method for rapid screening and identification of AChEIs from Yinhuang oral liquid was developedSeven compounds were screened and identified with potential AChE inhibitory activity from Yinhuang oral liquidIt provided experimental basis of Yinhuang oral liquid for the treating and preventing AD. Abbreviations used: (AD): Alzheimer's disease; (UF

  1. UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

    Science.gov (United States)

    Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

    2012-10-01

    The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

  2. An assessment of the usefulness of a rapid immuno-chromatographic test, "Determine™ malaria pf" in evaluation of intervention measures in forest villages of central India

    Directory of Open Access Journals (Sweden)

    Shukla Manmohan

    2001-08-01

    Full Text Available Abstract Background Plasmodium falciparum malaria, is a major health problem in forested tribal belt of central India. Rapid and accurate methods are needed for the diagnosis of P. falciparum. We performed a blinded evaluation of the recently introduced Determine™ malaria pf test (Abbott, Laboratories, Japan compared with microscopy and splenomegaly in children in epidemic prone areas of district Mandla to assess the impact of intervention measures. Methods Children aged 2–10 yrs with and without fever were examined for spleen enlargement by medical specialist by establishing a mobile field clinic. From these children thick blood smears were prepared from finger prick and read by a technician. Simultaneously, rapid tests were performed by a field lab attendant. The figures for specificity, sensitivity and predictive values were calculated using microscopy as gold standard. Results In all 349 children were examined. The sensitivity and specificity for Determine rapid diagnostic test were 91 and 80% respectively. The positive predictive values (PPV, negative predictive values (NPV and accuracy of the test were respectively 79, 91 and 85%. On the contrary, the sensitivity and specificity of spleen in detecting malaria infection were 57 and 74 % respectively with PPV of 73%, NPV 59 % and an accuracy of 65%. Conclusions Determine™ malaria rapid diagnostic test is easier and quicker to perform and has other advantages over microscopy in not requiring prior training of personnel or quality control. Thus, highlighting the usefulness of a rapid antigen test in assessing prevailing malaria situation in remote areas.

  3. Validation and optimization of a chromatographic method for the quantitative and qualitative determination of cocaine and heroin through liquid chromatography of high resolution

    International Nuclear Information System (INIS)

    Montero Aguilar, A.L.

    1997-01-01

    A (HPLC) chromatographic method was optimized in this work, for the determination of cocaine and heroin in seizures, through the application of the factorial and the simplex design. It applied the developed methodology in the determination of the content of cocaine and of heroin in nine different samples. The application of this methodology in abuse drugs seizures samples, turned out analytically satisfactory for the time of analysis and the veracity of the results. It also complements efficiently the qualitative analysis of cocaine and heroin, that the Laboratory of Physical and Chemical Investigations of the Department of Forensic Sciences of the Agency of Judicial Investigation carries out. (S. Grainger) [es

  4. Rapid and selective derivatizatin method for the nitrogen-sensitive detection of carboxylic acids in biological fluids prior to gas chromatographic analysis

    NARCIS (Netherlands)

    Lingeman, H.; Haan, H.B.P.; Hulshoff, A.

    1984-01-01

    A rapid and selective derivatization procedure is described for the pre-column labelling of carboxylic acids with a nitrogen-containing label. The carboxylic acid function is activated with 2-bromo-1-methylpyridinium iodide and the activated carboxylic acid function reacts with a primary or a

  5. Simultaneous determination of related substances of telmisartan and hydrochlorothiazide in tablet dosage form by using reversed phase high performance liquid chromatographic method

    Directory of Open Access Journals (Sweden)

    Sutirtho Mukhopadhyay

    2011-01-01

    Full Text Available Objective : Telmisartan is a potent, long-lasting, nonpeptide antagonist of the angiotensin II type-1 (AT 1 receptor that is indicated for the treatment of essential hypertension. Hydrochlorothiazide is a widely prescribed diuretic and it is indicated for the treatment of edema, control of essential hypertension and management of diabetes insipidus. In the current article a new, accurate, sensitive, precise, rapid, reversed phase high performance liquid chromatography (RP-HPLC method was developed for determination of related substances of Telmisartan and Hydrochlorthiazide in tablet dosage form. Materials and Methods : Simultaneous determination of related substances was performed on Kromasil C 18 analytical column (250 × 4.6 mm; 5΅m pertical size column at 40°C employing a gradient elution. Mobile phase consisting of solvent A (solution containing 2.0 g of potassium dihydrogen phosphate anhydrous and 1.04 g of Sodium 1- Hexane sulphonic acid monohydrate per liter of water, adjusted to pH 3.0 with orthophosphoric acid and solvent B (mixture of Acetonitrile: Methanol in the ratio 80:20 v/v was used at a flow rate of 1.0 ml min−1 . UV detection was performed at 270 nm. Results : During method validation parameter such as precision, linearity, accuracy, specificity, limit of detection and quantification were evaluated, which remained within acceptable limits. Conclusions : HPLC analytical method is linear, accurate, precise, robust and specific, being able to separate the main drug from its degradation products. It may find application for the routine analysis of the related substances of both Telmisartan and Hydrochlorthiazide in this combination tablets.

  6. Covalent triazine framework-1 as adsorbent for inline solid phase extraction-high performance liquid chromatographic analysis of trace nitroimidazoles in porcine liver and environmental waters.

    Science.gov (United States)

    Zhong, Cheng; Chen, Beibei; He, Man; Hu, Bin

    2017-02-03

    In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

    Science.gov (United States)

    Hemmati, Maryam; Asghari, Alireza; Bazregar, Mohammad; Rajabi, Maryam

    2016-11-01

    In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL -1 for metoprolol and 2.5-2500 ng mL -1 for propranolol with the correlation of determinations (R 2 s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL -1 for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.

  8. Development of high performance liquid chromatography for rapid determination of burn-up of nuclear fuels

    International Nuclear Information System (INIS)

    Joseph, M.; Karunasagar, D.; Saha, B.

    1996-01-01

    Burn-up an important parameter during evaluation of the performance of any nuclear fuel. Among the various techniques available, the preferred one for its determination is based on accurate measurement of a suitable fission product monitor and the residual heavy elements. Since isotopes of rare earth elements are generally used as burn-up monitors, conditions were standardized for rapid separation (within 15 minutes) of light rare earths using high performance liquid chromatography based on either anion exchange (Partisil 10 SAX) in methanol-nitric acid medium or by cation exchange on a reverse phase column (Spherisorb 5-ODS-2 or Supelcosil LC-18) dynamically modified with 1-octane sulfonate or camphor-10-sulfonic acid (β). Both these methods were assessed for separation of individual fission product rare earths from their mixtures. A new approach has been examined in detail for rapid assay of neodymium, which appears promising for faster and accurate measurement of burn-up. (author)

  9. Rapid Immuno-Chromatographic Assay for the Detection of Antibodies to HIV Compare with Elisa among Voluntary and Replacement Blood Donor of Mymensingh Medical College Hospital.

    Science.gov (United States)

    Chakrabarty, P; Rudra, S; Hossain, M A; Begum, S A; Mirza, T T; Rudra, M

    2015-04-01

    Suitable algorithms based on a combination of two or more simple rapid HIV assays have been shown to have a diagnostic accuracy comparable to double enzyme-linked immunosorbent assay (ELISA) or double ELISA with Western Blot strategies. The aims of this study were to evaluate the performance of five simple rapid HIV assays using whole blood samples from voluntary and replacement blood donors & HIV-infected patients (positive samples from BSMMU, Dhaka). Five rapid HIV assays: Determine™ HIV-1/2 (Inverness Medical), SD Bioline HIV 1/2 3.0 (Standard Diagnostics Inc.), First Response HIV Card 1-2.0 (PMC Medical India Pvt Ltd.), HIV1/2 Stat-Pak Dipstick (Chembio Diagnostic System, Inc) and Uni-Gold™ HIV-1/2 (Biotech) were evaluated between 1st February to 30th June, 2013 using 400 whole blood samples from voluntary and replacement blood donors. All samples that were reactive on all or any of the five rapid assays and 10% of non-reactive samples were tested on a confirmatory Inno-Lia HIV I/II immunoblot assay (Immunogenetics). Only 01 sample including ten positive samples from BSMMU were confirmed HIV-1 antibody positive, while 399 were HIV negative. The sensitivity at initial testing of Determine, SD Bioline and Uni-Gold™ was 100% (95% CI; 99.1-100) while First Response and Stat-Pak had sensitivity of 99.5% (95% CI; 98.2-99.9) and 97.7% (95% CI; 95.7-98.9) respectively, which increased to 100% (95% CI; 99.1-100) on repeat testing. The initial specificity of the Uni-Gold™ assay was 100% (95% CI; 99.6-100) while specificities were 99.6% (95% CI; 99-99.9), 99.4% (95% CI; 98.8-99.7), 99.6% (95% CI; 99-99.9) and 99.8% (95% CI; 99.3-99.9) for Determine, SD Bioline, First Response and Stat-Pak assays, respectively. There was no any sample which was concordantly false positive in Uni-Gold™, Determine and SD Bioline assays. An alternative confirmatory HIV testing strategy based on initial testing on either SD Bioline or Determine assays followed by testing of reactive

  10. Simple and rapid method on High Performance Liquid Chromatography for simultaneous determination of benzylpenicillin potassium, streptomycin sulphate and related substances in Ascomicin – a veterinary use ointment

    Directory of Open Access Journals (Sweden)

    Neagu Maria

    2015-06-01

    Full Text Available A new simple, rapid, accurate and precise High – Performance Liquid Chromatography (HPLC method for determination of benzylpenicillin potassium and streptomycin sulphate in Ascomicin ointment was developed and validated. The method can be used for the detection and quantification of known and unknown impurities and degradation products in this pharmaceutical product during routine analysis and also for stability studies in view of its capability to separate degradation products. The method was validated for accuracy, precision, specificity, robustness and quantification limits according to ICH Guidelines. The estimation of benzylpenicillin potassium and streptomycin sulphate was done by Waters HPLC 2695. The chromatographic conditions comprised a reverse-phased C18 column (5 µm particle size, 250 mm×4.6 mm i.d. with a mobile phase consisting of a mixture of solution in water containing 0.025 M of sodium phosphate dibasic and 0.02 of sodium hexansulfonate adjusted to pH 6.0 with 22.5 g/lsolution of phosphoric acid and acetonitrile in gradient elution. The flow rate was 0.8 ml/min. Standard curves were linear over the concentration range of 5.00 µg/ml to 5.00 mg/ml for streptomycin sulphate and 3.26 µg/ml to 3.26 mg/ml for benzylpenicillin potassium. Statistical analyses proved the method was precise, reproducible, selective, specific and accurate for analysis of benzylpenicillin potassium, streptomycin sulphate and related substances.

  11. Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

    International Nuclear Information System (INIS)

    Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

    1989-01-01

    We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

  12. Comparison of two validated gas-chromatographic methods for the determination of trihalomethanes in drinking water Comparação de dois métodos cromatográficos validados para a dosagem de trialometanos em água potável

    OpenAIRE

    Maria Yumiko Tominaga; Antonio Flavio Mídio

    2003-01-01

    In this paper the results obtained using two validated gas-chromatographic procedures on drinking water for the determination of trihalomethanes are compared. The volatile compounds, chloroform (CF), bromodichloromethane (BDCM), dibromochloromethane (DBCM) and bromoform (BF) were detected by purge and trap capillary column gas-chromatography with electrolytic conductivity detector ( ELCD) and the simple and rapid gas-chromatographic method by electron capture detector (ECD) after liquid-liqui...

  13. A rapid, solid phase extraction (SPE technique for the extraction and gas chromatographic determination lindane pesticide residue in tissue and milk

    Directory of Open Access Journals (Sweden)

    Yuningsih

    2006-03-01

    Full Text Available Organochlorine pesticide contamination in feed can cause residue in animal product (tissue and milk, so its become a problem in food safety. Solid phase extraction (SPE has been carried out for determination organochlorine pesticide residues in food animal production. The technique was rapid, not costly and produce limited amount of hazardous-waste. Samples were homogenized with acetonitrile trough cartridge C18, eluted in fluorocyl column with 2% ether-petroleum or acetonitrile fortissue and milk samples respectively. The recoveries of tissue sample by addition lindane standard solution: 0.50 and 1.00 μg are 85.10 and 103.10% respectively, while that of milk with the addition of 0.50, 1.00 and 1.50 μg are 83.80, 88.69 and 91.24% respectively. Three replicates were carried out for every sample. According of validation criteria of FAO/IAEA the recovery for analysis of pesticide residues was 70-110%. Therefore, the method is applicable.

  14. Miniaturized Planar Room Temperature Ionic Liquid Electrochemical Gas Sensor for Rapid Multiple Gas Pollutants Monitoring.

    Science.gov (United States)

    Wan, Hao; Yin, Heyu; Lin, Lu; Zeng, Xiangqun; Mason, Andrew J

    2018-02-01

    The growing impact of airborne pollutants and explosive gases on human health and occupational safety has escalated the demand of sensors to monitor hazardous gases. This paper presents a new miniaturized planar electrochemical gas sensor for rapid measurement of multiple gaseous hazards. The gas sensor features a porous polytetrafluoroethylene substrate that enables fast gas diffusion and room temperature ionic liquid as the electrolyte. Metal sputtering was utilized for platinum electrodes fabrication to enhance adhesion between the electrodes and the substrate. Together with carefully selected electrochemical methods, the miniaturized gas sensor is capable of measuring multiple gases including oxygen, methane, ozone and sulfur dioxide that are important to human health and safety. Compared to its manually-assembled Clark-cell predecessor, this sensor provides better sensitivity, linearity and repeatability, as validated for oxygen monitoring. With solid performance, fast response and miniaturized size, this sensor is promising for deployment in wearable devices for real-time point-of-exposure gas pollutant monitoring.

  15. Rapid bioassay method for estimation of 90Sr in urine samples by liquid scintillation counting

    International Nuclear Information System (INIS)

    Wankhede, Sonal; Chaudhary, Seema; Sawant, Pramilla D.

    2018-01-01

    Radiostrontium (Sr) is a by-product of the nuclear fission of uranium and plutonium in nuclear reactors and is an important radionuclide in spent nuclear fuel and radioactive waste. Rapid bioassay methods are required for estimating Sr in urine following internal contamination. Decision regarding medical intervention, if any can be based upon the results of urinalysis. The present method used at Bioassay Laboratory, Trombay is by Solid Extraction Chromatography (SEC) technique. The Sr separated from urine sample is precipitated as SrCO 3 and analyzed gravimetrically. However, gravimetric procedure is time consuming and therefore, in the present study, feasibility of Liquid Scintillation Counting for direct detection of radiostrontium in effluent was explored. The results obtained in the present study were compared with those obtained using gravimetric method

  16. Optimization of Forced Degradation Using Experimental Design and Development of a Stability-Indicating Liquid Chromatographic Assay Method for Rebamipide in Bulk and Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    Sandeep SONAWANE

    2016-09-01

    Full Text Available A novel stability-indicating RP-HPLC assay method was developed and validated for quantitative determination of rebamipide in bulk and tablet dosage form. Rebamipide (drug and drug product solutions were exposed to acid and alkali hydrolysis, thermal stress, oxidation by hydrogen peroxide and photodegradation. Experimental design has been used during forced degradation to determine significant factors responsible for degradation and to obtain optimal degradation conditions. In addition, acid and alkali hydrolysis was performed using a microwave oven. The chromatographic method employed the HiQ sil C-18HS (250 × 4.6 mm; 5 μm column with mobile phase consisting of 0.02 M potassium phosphate (pH adjusted to 6.8 and methanol (40:60, v/v and the detection was performed at 230 nm. The procedure was validated for specificity, linearity, accuracy, precision and robustness. There was no interference observed of excipients and degradation products in the determination of the active pharmaceutical ingredient. The method showed good accuracy and precision (intra and inter day and the response was linear in a range from 0.5 to 5 μg mL−1. The method was found to be simple and fast with less trial and error experimentation by making use of experimental design. Also, it proved that microwave energy can be used to expedite hydrolysis of rebamipide.

  17. Liquid chromatographic determination of aniline and derivatives in environmental waters at nanogram per litre levels using fluorescamine pre-column derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Djozan, D. [Univ. of Tabriz (Iran, Islamic Republic of). Dept. of Analytical Chemistry; Faraj-Zadeh, M.A. [Univ. of Tabriz (Iran, Islamic Republic of). Dept. of Analytical Chemistry

    1995-11-01

    Fluorescamine (fluram) has been used as a fluorogenic compound for pre-column derivatization of aniline and some derivatives. Anilines were derivatized with fluram in citrate buffer media (pH 5.5) to form pyrrolinones. The highly fluorescence pyrrolinones were isolated and pre-concentrated by solid phase extraction. A reversed phase, Spherisorb RP-8 column and tetrahydrofuran: Water:formic acid (42:56:2) mobile phase was used for separation. Detection method was by a sensitive fluorimetric method and quantitation was at 395 and 495 nm. The various parameters such as reaction conditions between anilines and fluram, solid phase extraction and chromatographic separation were optimized. Calibrations were linear over the range considered with excellent correlation coefficients (r>0.999). Relative standard deviations are less than 2.5% and detection limits for aniline, p-toluidine, 4-chloroaniline and 4-bromoaniline were 6, 30, 6 and 8 ng L{sup -1}, respectively. This method has been used successfully for the determination of anilines in environmental waters. (orig.)

  18. High-performance liquid chromatographic method for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma.

    Science.gov (United States)

    Xie, Ying; Chen, Yi; Lin, Mei; Wen, Jun; Fan, Guorong; Wu, Yutian

    2007-05-09

    A high-performance liquid chromatographic method was developed and validated for the determination and pharmacokinetic study of oxypeucedanin hydrate and byak-angelicin after oral administration of Angelica dahurica extracts in mongrel dog plasma. The coumarin components and the internal standard isopsoralen were extracted from plasma samples with the mixture of tert-butyl methyl ether and n-hexane (4:1, v/v). Chromatographic separation was performed on a C(18) column (200 mm x 4.6mm, 5 microm) with the mobile phase acetonitrile-methanol-water-acetic acid (20:15:65:2, v/v/v/v) at a flow-rate of 1.0 ml/min. Only the peak of oxypeucedanin hydrate and byak-angelicin could be detected in dog plasma after oral administration of ethanol extracts of A. dahurica mainly containing xanthotoxol, osthenol, imperatorin, oxypeucedanin hydrate and byak-angelicin. The calibration curves of oxypeucedanin hydrate and byak-angelicin were linear over a range of 22.08-8830.00 and 6.08-2430.00 ng/ml in dog plasma, respectively. The quantification limit of oxypeucedanin hydrate and byak-angelicin in dog plasma was 22.08 and 6.08 ng/ml, respectively. The intra- and inter-day precision was less than 7.6% and 8.5% and the accuracy was from 91.9% to 106.1%. The lowest absolute recoveries of oxypeucedanin hydrate and byak-angelicin were 85.7% and 87.0%, respectively. The method was successfully applied to the pharmacokinetic studies of oxypeucedanin hydrate and byak-angelicin in dog plasma after oral administration of ethanol extracts from A. dahurica.

  19. Rapid profiling of antimicrobial compounds characterising B. subtilis TR50 cell-free filtrate by high-performance liquid chromatography coupled to high-resolution Orbitrap™ mass spectrometry.

    Science.gov (United States)

    Monaci, Linda; Quintieri, Laura; Caputo, Leonardo; Visconti, Angelo; Baruzzi, Federico

    2016-01-15

    Several Bacillus strains, typically isolated from different food sources, represent renowned producers of a multitude of low and high molecular weight compounds, including lipopeptides and macrolactones, with an importance for their antimicrobial activity. The high homology shared by many of these compounds also occurring as closely related isoforms poses a challenge in their prompt detection. Identification and structural elucidation is generally achieved by matrix-assisted laser desorption/ionization (MALDI) or liquid chromatography (LC) coupled to mass spectrometry (MS) after a pre-fractionation and/or purification step of the extract. In this paper we report the application of a method based on LC separation and high-resolution Orbitrap™-based MS for the rapid screening of raw filtrate of the strain Bacillus subtilis TR50 endowed with antimicrobial activity, without requiring any sample pre-treatment. Upon direct analysis of the cell-free filtrate of Bacillus subtilis TR50 by high-resolution mass spectrometry (HRMS), different compounds families, that proved to exert a remarked antimicrobial activity against several foodborne pathogens, can be readily displayed along the chromatographic run. Among them, three different classes were identified and characterized belonging to the iturin, fengycin and surfactin groups. The high resolving power and accurate mass accuracy provided by the HRMS system in use ensured an enhanced selectivity compared to other mass spectrometers. In addition, after activation of the HCD cell, the HR-MS/MS spectra can provide insights in the structural elucidation of several compounds. The acquisition of HRMS spectra of raw filtrates of subtilis strains allows untargeted analysis of the major classes of compounds produced to be performed, thus facilitating identification of other unknown bioactive molecules after retrospective analysis. These features make this approach a fast tool applicable to the rapid screening and further

  20. Diffusion-stress coupling in liquid phase during rapid solidification of binary mixtures

    International Nuclear Information System (INIS)

    Sobolev, S.L.

    2014-01-01

    An analytical model has been developed to describe the diffusion-viscous stress coupling in the liquid phase during rapid solidification of binary mixtures. The model starts with a set of evolution equations for diffusion flux and viscous pressure tensor, based on extended irreversible thermodynamics. It has been demonstrated that the diffusion-stress coupling leads to non-Fickian diffusion effects in the liquid phase. With only diffusive dynamics, the model results in the nonlocal diffusion equations of parabolic type, which imply the transition to complete solute trapping only asymptotically at an infinite interface velocity. With the wavelike dynamics, the model leads to the nonlocal diffusion equations of hyperbolic type and describes the transition to complete solute trapping and diffusionless solidification at a finite interface velocity in accordance with experimental data and molecular dynamic simulation. -- Highlights: •We propose the diffusion-stress coupling model for binary solidification. •The coupling arises at deep undercooling. •With diffusive dynamics, the models result in parabolic transfer equations. •With the wavelike dynamics, the models lead to hyperbolic transfer equations. •The coupling strongly affects the solute partition coefficient

  1. Subcritical thermal convection of liquid metals in a rapidly rotating sphere

    Science.gov (United States)

    Cardin, P.; Schaeffer, N.; Guervilly, C.; Kaplan, E.

    2017-12-01

    Planetary cores consist of liquid metals (low Prandtl number Pr) that convect as the core cools. Here we study nonlinear convection in a rotating (low Ekman number Ek) planetary core using a fully 3D direct (down to Ek=10-7) and a quasi geostrophic (down to Ek=10-10) numerical simulations. Near the critical thermal forcing (Rayleigh number Ra), convection onsets as thermal Rossby waves, but as Ra increases, this state is superceded by one dominated by advection. At moderate rotation, these states (here called the weak branch and strong branch, respectively) are continuously connected. As the planetary core rotates faster, the continuous transition is replaced by hysteresis cycles and subcriticality until the weak branch disappears entirely and the strong branch onsets in a turbulent state at Ekforcing decreases well below the linear onset of convection (Ra 0.4Racrit in this study for Ek=10-10 and Pr=0.01). We highlight the importance of the Reynolds stress, which is required for convection to persist below the linear onset. We further note the presence of a strong zonal flow that is nonetheless unimportant to the convective subcritical state. Our study suggests that, in the asymptotic regime of rapid rotation relevant for planetary interiors, thermal convection of liquid metals in a sphere onsets and shuts down through a subcritical bifurcation. This scenario may be relevant to explain the lunar and martian dynamo extinctions.

  2. Assessment of disintegration of rapidly disintegrating tablets by a visiometric liquid jet-mediated disintegration apparatus.

    Science.gov (United States)

    Desai, Parind M; Liew, Celine V; Heng, Paul W S

    2013-02-14

    The aim of this study was to develop a responsive disintegration test apparatus that is particularly suitable for rapidly disintegrating tablets (RDTs). The designed RDT disintegration apparatus consisted of disintegration compartment, stereomicroscope and high speed video camera. Computational fluid dynamics (CFD) was used to simulate 3 different designs of the compartment and to predict velocity and pressure patterns inside the compartment. The CFD preprocessor established the compartment models and the CFD solver determined the numerical solutions of the governing equations that described disintegration medium flow. Simulation was validated by good agreement between CFD and experimental results. Based on the results, the most suitable disintegration compartment was selected. Six types of commercial RDTs were used and disintegration times of these tablets were determined using the designed RDT disintegration apparatus and the USP disintegration apparatus. The results obtained using the designed apparatus correlated well to those obtained by the USP apparatus. Thus, the applied CFD approach had the potential to predict the fluid hydrodynamics for the design of optimal disintegration apparatus. The designed visiometric liquid jet-mediated disintegration apparatus for RDT provided efficient and precise determination of very short disintegration times of rapidly disintegrating dosage forms. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Rapid Quantitation of Furanocoumarins and Flavonoids in Grapefruit Juice using Ultra-Performance Liquid Chromatography.

    Science.gov (United States)

    Vandermolen, Karen M; Cech, Nadja B; Paine, Mary F; Oberlies, Nicholas H

    2013-01-01

    Grapefruit juice can increase or decrease the systemic exposure of myriad oral medications, leading to untoward effects or reduced efficacy. Furanocoumarins in grapefruit juice have been established as inhibitors of cytochrome P450 3A (CYP3A)-mediated metabolism and P-glycoprotein (P-gp)-mediated efflux, while flavonoids have been implicated as inhibitors of organic anion transporting polypeptide (OATP)-mediated absorptive uptake in the intestine. The potential for drug interactions with a food product necessitates an understanding of the expected concentrations of a suite of structurally diverse and potentially bioactive compounds. Develop methods for the rapid quantitation of two furanocoumarins (bergamottin and 6',7'-dihydroxybergamottin) and four flavonoids (naringin, naringenin, narirutin and hesperidin) in five grapefruit juice products using ultra-performance liquid chromatography (UPLC). Grapefruit juice products were extracted with ethyl acetate; the concentrated extract was analysed by UPLC using acetonitrile:water gradients and a C18 -column. Analytes were detected using a photodiode array detector, set at 250 nm (furanocoumarins) and 310 nm (flavonoids). Intraday and interday precision and accuracy and limits of detection and quantitation were determined. Rapid (0.999. Considerable between-juice variation in the concentrations of these compounds was observed, and the quantities measured were in agreement with the concentrations published in HPLC studies. These analytical methods provide an expedient means to quantitate key furanocoumarins and flavonoids in grapefruit juice and other foods used in dietary substance-drug interaction studies. Copyright © 2013 John Wiley & Sons, Ltd.

  4. Isotope separations using chromatographic methods

    International Nuclear Information System (INIS)

    Leseticky, L.

    1985-01-01

    A survey is given of chromatographic separations of compounds only differing in isotope composition. Isotope effects on physical properties which allow chromatographic separation (vapour tension, adsorption heat, partition coefficient) are very small, with the exception of the simplest molecules. Therefore, separation factors only assume the value of several per cent. From this ensues the necessity of using columns which are specially and very carefully prepared and have a separation efficiency of the order of 10 4 theoretical plates. Briefly discussed is liquid chromatography on ion exchangers which with a varied degree of success was used for separating simple inorganic compounds or ions. Ion exchange chromatography of amino acids labelled with tritium, and chromatography of tritium labelled steroids also provided only a certain degree of separation. A detailed analysis is presented of gas chromatography separation of various deuterium and tritium labelled low-molecular compounds, to which a number of studies has been devoted in the literature. Very promising is the method of complexation gas chromatography based on the reversible formation of a complex of the ligand (the compound being separated) and the compound of the (transition) metal as the steady-state phase. (author)

  5. Simple and rapid determination of norethindrone in human plasma by supported liquid extraction and ultra performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Gong, Zhilong; Chandler, Kiresha; Webster, Stephen; Kerley, Remy; Buist, Susan; McCort-Tipton, Melanie

    2012-03-15

    We report for the first time an ultra performance liquid chromatographic method with tandem mass spectrometric detection (UPLC/MS/MS) for the determination of norethindrone alone in human plasma over the concentration range of 50.0-25000 pg mL(-1) using a sample volume of 0.250 mL. Norethindrone and its internal standard (ISTD), norethindrone-(13)C(2), were extracted from human plasma by supported liquid extraction (SLE). After evaporation of the organic solvent, samples were reconstituted and analyzed on an UPLC/MS/MS system. The UPLC system used a Waters BEH C18 (100 mm × 2.1mm, 1.7 μm) column with mobile phase A of 0.05% formic acid in water:acetonitrile (65:35, v/v) and mobile phase B of 0.05% formic acid in methanol:acetonitrile (50:50, v/v). The flow rate was 0.500 mL min(-1). The method was fully validated. The inter-run accuracy and precision at the lower limit of quantitation (LLOQ), low, mid and high quality control (QC) concentration levels were 99.2-108.4% with a <8.1% CV (coefficient of variation), respectively. The validated method has been successfully applied to analysis of thousands of pharmacokinetic samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Rapid quantification of imidazolium-based ionic liquids by hydrophilic interaction liquid chromatography: Methodology and an investigation of the retention mechanisms.

    Science.gov (United States)

    Hawkins, Cory A; Rud, Anna; Guthrie, Margaret L; Dietz, Mark L

    2015-06-26

    The separation of nine N,N'-dialkylimidazolium-based ionic liquids (ILs) by an isocratic hydrophilic interaction high-performance liquid chromatographic method using an unmodified silica column was investigated. The chosen analytical conditions using a 90:10 acetonitrile-ammonium formate buffer mobile phase on a high-purity, unmodified silica column were found to be efficient, robust, and sensitive for the determination of ILs in a variety of solutions. The retention window (k' = 2-11) was narrower than that of previous methods, resulting in a 7-min runtime for the nine IL homologues. The lower limit of quantification of the method, 2-3 μmol L(-1), was significantly lower than those reported previously for HPLC-UV methods. The effects of systematically modifying the IL cation alkyl chain length, column temperature, and mobile-phase water and buffer content on solute retention were examined. Cation exchange was identified as the dominant retention mechanism for most of the solutes, with a distinct (single methylene group) transition to a dominant partitioning mode at the highest solute polarity. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Chromatographic selectivity of poly(alkyl methacrylate-co-divinylbenzene) monolithic columns for polar aromatic compounds by pressure-driven capillary liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2016-10-05

    In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16–1.20%, RSD; n = 3) and column-to-column (0.26–2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns. - Highlights: • First investigation on chromatographic selectivity of AlMA-DVB monolithic columns. • Good run-to-run/column-to-column repeatability (<3%) on AlMA-DVB monolithic columns. • Efficient separation of phenylurea herbicides and sulfonamides on AlMA-DVB columns.

  8. Chromatographic hydrogen isotope separation

    International Nuclear Information System (INIS)

    Aldridge, F.T.

    1983-01-01

    Intermetallic compounds with the CaCu5 type of crystal structure, particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

  9. Chromatographic hydrogen isotope separation

    International Nuclear Information System (INIS)

    Aldridge, F.T.

    1981-01-01

    Intermetallic compounds with the CaCu5 type of crystal structure , particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

  10. Development and validation of a rapid ultra-high performance liquid chromatography diode array detector method for Vitex agnus-castus.

    Science.gov (United States)

    Högner, C; Sturm, S; Seger, C; Stuppner, H

    2013-05-15

    A rapid ultra-high performance liquid chromatography diode array detector (UHPLC-DAD) method was developed and validated for the simultaneous determination of all classes of non-volatile phytochemicals (iridoids, flavonoids and diterpenes) in Vitex agnus-castus (Lamiaceae) fruits, a traditional medicinal plant used against premenstrual symptoms (PMS) and other disorders. Seven marker compounds, 3,4-dihydroxybenzoic acid, p-hydroxybenzoic acid, agnuside, 5-hydroxykaempferol-3,6,7,4'-tetramethylether, 1,2-dibenzoic acid glucose, methoxy-vitexilactone, and vitetrifolin D were isolated from the methanol extract of V. agnus-castus to be used as reference substances. Chromatographic separation was performed on a Zorbax Eclipse XDB-C18 (50mm×2.1mm) UHPLC column with 1.8μm particle size, within 20min. A solvent gradient from 0.5% acetic acid to acetonitrile at a flow rate of 0.6mL/min was used as mobile phase. Analyte detection and quantification was realized at 210nm and 260nm. The UHPLC-DAD assay was validated for the quantitative analysis of agnuside, isovitexin, casticin, 5-hydroxykaempferol-3,6,7,4'-tetramethylether and vitetrifolin D. It was found to be specific, accurate, precise, and reproducible for the quantification of these compound within a concentration range of 0.7-500.0μg/mL for casticin and 5-hydroxykaempferol-3,6,7,4'-tetramethylether, 1.4-1000.0μg/mL for isovitexin and agnuside, and 12.4-1000.0μg/mL for vitetrifolin D. Intra- and inter-day variations showed relative standard deviations (RSD) of less than 3.9% and 6.4%, respectively. Tentatively assignment of 62 chromatographic features found in the UHPLC-DAD assay was carried out by coupling the UHPLC instrument to a quadrupole time-of-flight mass spectrometer via an electrospray ionization interface (ESI-QTOF-MS) operated in positive and negative ion mode. By using the established quantitative UHPLC-DAD assay to asses agnuside, isovitexin, casticin, 5-hydroxykaempferol-3,6,7,4'-tetramethylether and

  11. Additional band broadening of peptides in the first size-exclusion chromatographic dimension of an automated stop-flow two-dimensional high performance liquid chromatography.

    Science.gov (United States)

    Xu, Jucai; Sun-Waterhouse, Dongxiao; Qiu, Chaoying; Zhao, Mouming; Sun, Baoguo; Lin, Lianzhu; Su, Guowan

    2017-10-27

    The need to improve the peak capacity of liquid chromatography motivates the development of two-dimensional analysis systems. This paper presented a fully automated stop-flow two-dimensional liquid chromatography system with size exclusion chromatography followed by reversed phase liquid chromatography (SEC×RPLC) to efficiently separate peptides. The effects of different stop-flow operational parameters (stop-flow time, peak parking position, number of stop-flow periods and column temperature) on band broadening in the first dimension (1 st D) SEC column were quantitatively evaluated by using commercial small proteins and peptides. Results showed that the effects of peak parking position and the number of stop-flow periods on band broadening were relatively small. Unlike stop-flow analysis of large molecules with a long running time, additional band broadening was evidently observed for small molecule analytes due to the relatively high effective diffusion coefficient (D eff ). Therefore, shorter analysis time and lower 1 st D column temperature were suggested for analyzing small molecules. The stop-flow two-dimensional liquid chromatography (2D-LC) system was further tested on peanut peptides and an evidently improved resolution was observed for both stop-flow heart-cutting and comprehensive 2D-LC analysis (in spite of additional band broadening in SEC). The stop-flow SEC×RPLC, especially heart-cutting analysis with shorter analysis time and higher 1 st D resolution for selected fractions, offers a promising approach for efficient analysis of complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Warping methods for spectroscopic and chromatographic signal alignment: A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Bloemberg, Tom G., E-mail: T.Bloemberg@science.ru.nl [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Radboud University Nijmegen, Education Institute for Molecular Sciences, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Gerretzen, Jan; Lunshof, Anton [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands); Wehrens, Ron [Centre for Research and Innovation, Fondazione Edmund Mach, Via E. Mach, 1, 38010 San Michele all’Adige, TN (Italy); Buydens, Lutgarde M.C. [Radboud University Nijmegen, Institute for Molecules and Materials, Heyendaalseweg 135, 6525 AJ Nijmegen (Netherlands)

    2013-06-05

    Highlights: •The concepts of warping and alignment are introduced. •The most important warping methods are critically reviewed and explained. •Reference selection, evaluation and place of warping in preprocessing are discussed. •Some pitfalls, especially for LC–MS and similar data, are addressed. •Examples are provided, together with programming scripts to rework and extend them. -- Abstract: Warping methods are an important class of methods that can correct for misalignments in (a.o.) chemical measurements. Their use in preprocessing of chromatographic, spectroscopic and spectrometric data has grown rapidly over the last decade. This tutorial review aims to give a critical introduction to the most important warping methods, the place of warping in preprocessing and current views on the related matters of reference selection, optimization, and evaluation. Some pitfalls in warping, notably for liquid chromatography–mass spectrometry (LC–MS) data and similar, will be discussed. Examples will be given of the application of a number of freely available warping methods to a nuclear magnetic resonance (NMR) spectroscopic dataset and a chromatographic dataset. As part of the Supporting Information, we provide a number of programming scripts in Matlab and R, allowing the reader to work the extended examples in detail and to reproduce the figures in this paper.

  13. Rapid screening of oxytetracycline residue in catfish muscle by dispersive liquid-liquid microextraction and europium-sensitized luminescence

    Science.gov (United States)

    Oxytetracycline (OTC) residue in catfish muscle was screened by dispersive liquid-liquid microextraction (DLLME) and europium-sensitized luminescence (ESL). After extraction in EDTA, HCl, and acetonitrile, cleanup was carried out by DLLME, and ESL was measured at microgram = 385 nm and wavelength = ...

  14. Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

    Science.gov (United States)

    Steinheimer, T.R.; Brooks, M.G.

    1984-01-01

    A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

  15. Identification of dominant flow structures in rapidly rotating convection of liquid metals using Dynamic Mode Decomposition

    Science.gov (United States)

    Horn, S.; Schmid, P. J.; Aurnou, J. M.

    2016-12-01

    The Earth's metal core acts as a dynamo whose efficiency in generating and maintaining the magnetic field is essentially determined by the rotation rate and the convective motions occurring in its outer liquid part. For the description of the primary physics in the outer core the idealized system of rotating Rayleigh-Bénard convection is often invoked, with the majority of studies considering only working fluids with Prandtl numbers of Pr ≳ 1. However, liquid metals are characterized by distinctly smaller Prandtl numbers which in turn result in an inherently different type of convection. Here, we will present results from direct numerical simulations of rapidly rotating convection in a fluid with Pr ≈ 0.025 in cylindrical containers and Ekman numbers as low as 5 × 10-6. In this system, the Coriolis force is the source of two types of inertial modes, the so-called wall modes, that also exist at moderate Prandtl numbers, and cylinder-filling oscillatory modes, that are a unique feature of small Prandtl number convection. The obtained flow fields were analyzed using the Dynamic Mode Decomposition (DMD). This technique allows to extract and identify the structures that govern the dynamics of the system as well as their corresponding frequencies. We have investigated both the regime where the flow is purely oscillatory and the regime where wall modes and oscillatory modes co-exist. In the purely oscillatory regime, high and low frequency oscillatory modes characterize the flow. When both types of modes are present, the DMD reveals that the wall-attached modes dominate the flow dynamics. They precess with a relatively low frequency in retrograde direction. Nonetheless, also in this case, high frequency oscillations have a significant contribution.

  16. Sensitivity enhancement by chromatographic peak concentration with ultra-high performance liquid chromatography-nuclear magnetic resonance spectroscopy for minor impurity analysis.

    Science.gov (United States)

    Tokunaga, Takashi; Akagi, Ken-Ichi; Okamoto, Masahiko

    2017-07-28

    High performance liquid chromatography can be coupled with nuclear magnetic resonance (NMR) spectroscopy to give a powerful analytical method known as liquid chromatography-nuclear magnetic resonance (LC-NMR) spectroscopy, which can be used to determine the chemical structures of the components of complex mixtures. However, intrinsic limitations in the sensitivity of NMR spectroscopy have restricted the scope of this procedure, and resolving these limitations remains a critical problem for analysis. In this study, we coupled ultra-high performance liquid chromatography (UHPLC) with NMR to give a simple and versatile analytical method with higher sensitivity than conventional LC-NMR. UHPLC separation enabled the concentration of individual peaks to give a volume similar to that of the NMR flow cell, thereby maximizing the sensitivity to the theoretical upper limit. The UHPLC concentration of compound peaks present at typical impurity levels (5.0-13.1 nmol) in a mixture led to at most three-fold increase in the signal-to-noise ratio compared with LC-NMR. Furthermore, we demonstrated the use of UHPLC-NMR for obtaining structural information of a minor impurity in a reaction mixture in actual laboratory-scale development of a synthetic process. Using UHPLC-NMR, the experimental run times for chromatography and NMR were greatly reduced compared with LC-NMR. UHPLC-NMR successfully overcomes the difficulties associated with analyses of minor components in a complex mixture by LC-NMR, which are problematic even when an ultra-high field magnet and cryogenic probe are used. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. High-performance liquid chromatographic separation of biologically important arsenic species utilizing on-line inductively coupled argon plasma atomic emission spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Spall, W.D.; Lynn, J.G.; Andersen, J.L.; Valdez, J.G.; Gurley, L.R.

    1986-06-01

    An anion exchange, high-performance liquid chromatography technique using a 15-min linear gradient from water to 0.5 M ammonium carbonate to separate arsenite, arsenate, methylarsonic acid, and dimethylarsinic acid from neutral arsenic containing compounds was developed for application to a study of arsenic metabolism in cultured cell suspensions. Arsenic detection was accomplished by the direct coupling of the column effluent to an inductively coupled argon plasma atomic emission spectrometer (ICAP-AES) set to monitor the arsenic emission line at 197.19 nm. The analysis requires 20 min and is sensitive to as low as 60 ng of arsenic injected to the column.

  18. Rapid Quantitation of Furanocoumarins and Flavonoids in Grapefruit Juice using Ultra Performance Liquid Chromatography

    Science.gov (United States)

    VanderMolen, Karen M.; Cech, Nadja B.; Paine, Mary F.

    2013-01-01

    Introduction Grapefruit juice can increase or decrease the systemic exposure of myriad oral medications, leading to untoward effects or reduced efficacy. Furanocoumarins in grapefruit juice have been established as inhibitors of cytochrome P450 3A (CYP3A)-mediated metabolism and P-glycoprotein (P-gp)-mediated efflux, while flavonoids have been implicated as inhibitors of organic anion transporting polypeptide (OATP)-mediated absorptive uptake in the intestine. The potential for drug interactions with a food product necessitates an understanding of the expected concentrations of a suite of structurally diverse and potentially bioactive compounds. Objective Develop methods for the rapid quantitation of two furanocoumarins (bergamottin and 6′,7′-dihydroxybergamottin) and four flavonoids (naringin, naringenin, narirutin, and hesperidin) in five grapefruit juice products using ultra performance liquid chromatography (UPLC). Methodology Grapefruit juice products were extracted with ethyl acetate; the concentrated extract was analyzed by UPLC using acetonitrile:water gradients and a C18 column. Analytes were detected using a photodiode array detector, set at 250 nm (furanocoumarins) and 310 nm (flavonoids). Intraday and interday precision and accuracy and limits of detection and quantitation were determined. Results Rapid (flavonoids. R2 values for the calibration curves of all analytes were >0.999. Considerable between-juice variation in the concentrations of these compounds was observed, and the quantities measured were in agreement with the concentrations published in HPLC studies. Conclusion These analytical methods provide an expedient means to quantitate key furanocoumarins and flavonoids in grapefruit juice and other foods used in dietary substance-drug interaction studies. PMID:23780830

  19. LIQUID CHROMATOGRAPHIC / MASS SPECTROMETRIC DETERMINATION OF MORPHINE, CODEINE AND COCAINE IN HUMAN SERA USING A NEW INTERNAL SURFACE REVERSED PHASE COLUMN

    OpenAIRE

    Hattori, Hideki; Arinobu, Tetsuya; Iwai, Masae; Suzuki, Osamu; Seno, Hiroshi

    2003-01-01

    A new internal surface reversed phase column (Shim-pack MAYI-ODS) was used for analysis of morphine, codeine and cocaine in human sera by LC/MS/MS. The column enabled direct injection of crude biological samples without pretreatment realizing a rapid analytical procedure. Therecoveries of morphine, codeine and cocaine spiked into human sera were 50-60 %. The regression equations for morphine, codeine and cocaine in sera, using atropine as internal standard, showed good linearity in the ranges...

  20. Coal liquefaction process streams characterization and evaluation: Application of liquid chromatographic separation methods to THF-soluble portions of integrated two-stage coal liquefaction resids

    Energy Technology Data Exchange (ETDEWEB)

    Green, J.B.; Pearson, C.D.; Young, L.L.; Green, J.A. [National Inst. for Petroleum and Energy Research, Bartlesville, OK (United States)

    1992-05-01

    This study demonstrated the feasibility of using non-aqueous ion exchange liquid chromatography (NIELC) for the examination of the tetrahydrofuran (THF)-soluble distillation resids and THF-soluble whole oils derived from direct coal liquefaction. The technique can be used to separate the material into a number of acid, base, and neutral fractions. Each of the fractions obtained by NIELC was analyzed and then further fractionated by high-performance liquid chromatography (HPLC). The separation and analysis schemes are given in the accompanying report. With this approach, differences can be distinguished among samples obtained from different process streams in the liquefaction plant and among samples obtained at the same sampling location, but produced from different feed coals. HPLC was directly applied to one THF-soluble whole process oil without the NIELC preparation, with limited success. The direct HPLC technique used was directed toward the elution of the acid species into defined classes. The non-retained neutral and basic components of the oil were not analyzable by the direct HPLC method because of solubility limitations. Sample solubility is a major concern in the application of these techniques.

  1. The Validation of an Analytical Method for Sulfentrazone Residue Determination in Soil Using Liquid Chromatography and a Comparison of Chromatographic Sensitivity to Millet as a Bioindicator Species

    Directory of Open Access Journals (Sweden)

    Marcelo Antonio de Oliveira

    2014-07-01

    Full Text Available Commonly used herbicides, such as sulfentrazone, pose the risk of soil contamination due to their persistence, bioaccumulation and toxicity. Phytoremediation by green manure species has been tested using biomarkers, but analytical data are now required to confirm the extraction of sulfentrazone from soil. Thus, the present work was carried out to analyze sulfentrazone residues in soil based on liquid chromatography with a comparison of these values to the sensitivity of the bioindicator Pennisetum glaucum. The soil samples were obtained after cultivation of Crotalaria juncea and Canavalia ensiformis at four seeding densities and with three doses of sulfentrazone. The seedlings were collected into pots, at two different depths, after 75 days of phytoremediator sowing and then were used to determine the herbicide persistence in the soil. A bioassay with P. glaucum was carried out in the same pot. High-performance liquid chromatography (HPLC, using UV-diode array detection (HPLC/UV-DAD, was used to determine the herbicide residues. The HPLC determination was optimized and validated according to the parameters of precision, accuracy, linearity, limit of detection and quantification, robustness and specificity. The bioindicator P. glaucum was more sensitive to sulfentrazone than residue determination by HPLC. Changes in sulfentrazone concentration caused by green manure phytoremediation were accurately identified by the bioindicator. However, a true correlation between the size of the species and the analyte content was not identified.

  2. Determination of multiresidue analysis of β-agonists in muscle and viscera using liquid chromatograph/tandem mass spectrometry with Quick, Easy, Cheap, Effective, Rugged, and Safe methodologies

    Directory of Open Access Journals (Sweden)

    Yen-Ping Lin

    2017-04-01

    Full Text Available The official analytical method of the Taiwan Food and Drug Administration, Ministry of Health and Welfare for testing for veterinary drug residues in foods is the multiresidue analysis of β-agonists. Samples are pretreated through liquid–liquid extraction and solid-phase extraction. This method is time consuming and requires the intensive use of solvents. To improve analytical efficiency and reduce costs, our study incorporated QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe techniques to establish a new method of multiresidue analysis of β-agonists in animal muscle and viscera. The pretreatment time was shortened and solvent usage was minimized. The modified analysis was conducted using liquid chromatography/tandem mass spectrometry (LC–MS/MS and quantification was performed using multiple reaction monitoring. The results demonstrated that the correlation coefficients of the tissue calibration curve were higher than 0.99 and the limit of quantification (LOQ was 1 ppb. The average recoveries in spiked samples varied from 70% to 120%, and the relative difference between duplicated analysis results was lower than 10%. On the basis of the results, the proposed method was concluded to be an appropriate procedure for determining the presence of β-agonists, and demonstrated the advantages of high recovery rates in spiked samples, high precision, reduced analysis time and solvent usage, and lower costs.

  3. Evaluation of phenolic content, total flavonoid and survey of antioxidant activity of leaves of Ficus carica and Pterocarya fraxinifolia trees using spectrophotometry and high performance liquid chromatograph methods

    Directory of Open Access Journals (Sweden)

    Naser Jafari

    2015-09-01

    Full Text Available In this research, to evaluate the antioxidant activity of leaf Pterocarya fraxinifolia (Juglandaceae and Ficus carica (Moraceae extract were carried out by spectrophotometry and high performance liquid chromatography methods. The leaves of P. fraxinifolia and F. carica were collected from Whitney and Shast Kalate (Golestan, Noor (Mazandaran and Asalem (Guilan forests in Iran. Methanolc extract was used in different experiments. The phenolic compounds (gallic acid, coumaric acid and quercetin were also measured by using high performance liquid chromatography (HPLC method.The maximum IC50 for DPPH radical-scavenging activity (595.12±21.4 μg ml-1 were observed in P. fraxinifolia leaves. According to the inhibition time, phenolic compound (gallic acid, coumaric acid and quercetin in F. carica leaves and gallic acid and coumaric acid were detected of Pterocarya leaves methanol extracts. The maximum amount of gallic acid (78.93 and coumaric acid (8.14 in extracts Pterocarya leaves Asalem and the lowest gallic acid (8.56 and coumaric acid (0.89 milligrams per gram was observed in Ficus leaf of Noor forest. Based on the standard chromatogram retention time of gallic acid (2.383, coumaric acid (3.817 and quercetin (7.217 mg/g was reported. This study showed that soil factors, such as potassium, sodium, phosphorus and nitrogen compounds with antioxidant phenolic extracts of the leaves of both plants there is a significant correlation.

  4. MultiSimplex optimization of chromatographic separation and dansyl derivatization conditions in the ultra performance liquid chromatography-tandem mass spectrometry analysis of risperidone, 9-hydroxyrisperidone, monoamine and amino acid neurotransmitters in human urine.

    Science.gov (United States)

    Cai, Hua-Lin; Zhu, Rong-Hua; Li, Huan-De; Zhang, Jun; Li, Lan-Fang

    2011-07-01

    A pre-column dansylated ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS/MS) method for simultaneous determination of risperidone (RIP), 9-hydroxyrisperidone (9-OH-RIP), monoamine and amino acid neurotransmitters in human urine was developed with the aim of providing data on how neurotransmitters may influence each other or change simultaneously in response to risperidone treatment. MultiSimplex based on the simplex algorithm and the fuzzy set theory was applied to the optimization of chromatographic separation and dansyl derivatization conditions during method development. This method exhibited excellent linearity for all the analytes with regression coefficients higher than 0.997. The lower limit of quantification (LLOQ) values for 9-OH-RIP and RIP were 0.11 and 0.06 ng/ml, respectively, and for neurotrasmitters ranged from 0.31 to 12.8 nM. The mean accuracy ranged from 94.7% to 108.5%. The mean recovery varied between 81.6% and 97.5%. All the RSD of precision and stability were below 9.7%. Finally, the optimized method was applied to analyze the first morning urine samples of schizophrenic patients treated with risperidone and healthy volunteers. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Rapid response sensor to monitor the temperature and flow of liquid metals

    International Nuclear Information System (INIS)

    McCann, J.D.

    1980-01-01

    Two forms of a sensor capable of simultaneously monitoring the temperature and flow of liquid metal coolants within a reactor are described. They operate by measuring the coupling impedances between the sensor and the surrounding electrically conductive coolant. Since the system utilises electrical rather than thermal properties, the response to perturbations is rapid, typically displaying the changed conditions within a few milliseconds. The first form of the sensor was designed to operate whilst protected by a thick walled service tube positioned in the reactor coolant. Providing bends in the tube had a radius greater than 70 cm, the sensor could be removed for inspection and maintenance if necessary. The second sensor was fitted inside a streamlined NaK proof capsule. This was inserted directly into the coolant outlet stream of a fuel pin assembly in the Dounreay Fast Reactor. In this form the sensor successfully monitored flow, entrained gas and temperature excursions during the final operating cycle of D.F.R. (author)

  6. Rapid determination of human globin chains using reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Wan, Jun-Hui; Tian, Pei-Ling; Luo, Wei-Hao; Wu, Bing-Yi; Xiong, Fu; Zhou, Wan-Jun; Wei, Xiang-Cai; Xu, Xiang-Min

    2012-07-15

    Reversed-phase high-performance liquid chromatography (RP-HPLC) of human globin chains is an important tool for detecting thalassemias and hemoglobin variants. The challenges of this method that limit its clinical application are a long analytical time and complex sample preparation. The aim of this study was to establish a simple, rapid and high-resolution RP-HPLC method for the separation of globin chains in human blood. Red blood cells from newborns and adults were diluted in deionized water and injected directly onto a micro-jupiter C18 reversed-phase column (250 mm × 4.6 mm) with UV detection at 280 nm. Under the conditions of varying pH or the HPLC gradient, the globin chains (pre-β, β, δ, α, (G)γ and (A)γ) were denatured and separated from the heme groups in 12 min with a retention time coefficient of variation (CV) ranging from 0.11 to 1.29% and a peak area CV between 0.32% and 4.86%. Significant differences (P<0.05) among three groups (normal, Hb H and β thalassemia) were found in the area ratio of α/pre-β+β applying the rapid elution procedure, while P≥0.05 was obtained between the normal and α thalassemia silent/trait group. Based on the ANOVA results, receiver operating characteristic (ROC) curve analysis of the δ/β and α/pre-β+β area ratios showed a sensitivity of 100.0%, and a specificity of 100.0% for indicating β thalassemia carriers, and a sensitivity of 96.6% and a specificity of 89.6% for the prediction of hemoglobin H (Hb H) disease. The proposed cut-off was 0.026 of δ/β for β thalassemia carriers and 0.626 of α/pre-β+β for Hb H disease. In addition, abnormal hemoglobin hemoglobin E (Hb E) and Hb Westmead (Hb WS) were successfully identified using this RP-HPLC method. Our experience in developing this RP-HPLC method for the rapid separation of human globin chains could be of use for similar work. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Single-laboratory validation of a high-performance liquid chromatographic-diode array detector-fluorescence detector/mass spectrometric method for simultaneous determination of water-soluble vitamins in multivitamin dietary tablets.

    Science.gov (United States)

    Chen, Pei; Atkinson, Renata; Wolf, Wayne R

    2009-01-01

    The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors [diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS)] for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 microm, 250 x 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100% A (0.1% formic acid in water), a linear gradient to 50% A and 50% B (0.1% formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLDIMS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.

  8. Application of a rapid and sensitive liquid chromatography-tandem mass spectrometry method for determination of bumetanide in human plasma for a bioequivalence study.

    Science.gov (United States)

    Patel, Dinesh S; Sharma, Naveen; Patel, Mukesh C; Patel, Bhavin N; Shrivastav, Pranav S; Sanyal, Mallika

    2012-07-01

    A rapid, selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of bumetanide in human plasma using tamsulosin as internal standard (IS). The analyte and IS were extracted from 200 μL of human plasma via solid phase extraction and the chromatographic separation was achieved on Peerless Basic C18 (100 mm × 4.6 mm, 3 μm) column under isocratic conditions. Detection of bumetanide and IS was done by tandem mass spectrometry, operating in positive ionization and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for bumetanide and IS were m/z 365.2→240.2 and 409.2→228.2 respectively. The method was fully validated as per the US FDA guidelines. The limit of detection and lower limit of quantitation of the method were 0.03 and 0.30 ng/mL respectively with a linear dynamic range of 0.30-200.0 ng/mL for bumetanide. The intra-batch and inter-batch precision (% CV) was ≤6.9% while the mean extraction recovery was >90% across quality control levels. The method is selective in presence of four diuretic drugs and some commonly used medications by healthy volunteers. It was successfully applied to a bioequivalence study of 2mg bumetanide tablet formulation in 10 healthy Indian male subjects under fasting condition. The reproducibility in the measurement of study data was demonstrated by reanalysis of 42 incurred samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Rapid Quantification and Quantitation of Alkaloids in Xinjiang Fritillaria by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Aziz Mohammat

    2017-05-01

    Full Text Available The Fritillaria genus, including different kinds of medicinal and edible plants belonging to the Liliaceae family which have the function of treating and relieving a cough and eliminating phlegm, is widely planted in Xinjiang (China. There are few comprehensive studies reporting on the characterization of the chemical constituents of Fritillaria from Xinjiang, and to date, no work describing the quantitative differences between the components in Fritillaria from Xinjiang and related species. The purpose of this study was to develop qualitative and quantitative analytical methods by Ultra Performance Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry (UPLC-QTOF-MS for the rapid quantification and quantitation of alkaloids in wild and cultivated Xinjiang Fritillaria, which could be used in the quality control of medicine based on this natural herb. Using the UPLC-QTOF-MS method, the chemical constituents of Xinjiang Fritillaria were identified by fragmentation information and retention behavior, and were compared to reference standards. Furthermore, a quantitative comparision of four major alkaloids in wild and cultivated Xinjiang Fritillaria was conducted by determining the content of Sipeimine-3β-d-glucoside, Sipeimine, Peimisine, and Yibeinoside A, respectively. A total of 89 characteristic peaks, including more than 40 alkaloids, were identified in the chromatographic results of Fritillaria. Four main alkaloids were quantified by using a validated method based on UPLC-QTOF-MS. The relative contents of Sipeimine-3β-d-glucoside, Sipeimine, Peimisine, and Yibeinoside A varied from 0.0013%~0.1357%, 0.0066%~0.1218%, 0.0033%~0.0437%, and 0.0019%~0.1398%, respectively. A rough separation of wild and cultivated Fritillaria could be achieved by the cluster analysis method.

  10. Liquid chromatographic/electrospray ionization tandem mass spectrometric study of polyphenolic composition of four cultivars of Fragaria vesca L. berries and their comparative evaluation.

    Science.gov (United States)

    Del Bubba, Massimo; Checchini, Leonardo; Chiuminatto, Ugo; Doumett, Saer; Fibbi, Donatella; Giordani, Edgardo

    2012-09-01

    High-performance liquid chromatography coupled with ion spray mass spectrometry in the tandem mode with both negative and positive ionization was used for investigating a variety of polyphenolic compounds in four genotypes of Fragaria vesca berries. About 60 phenolic compounds belonging to the compound classes of phenolic acids, ellagitannins, ellagic acid derivatives, flavonols, monomeric and oligomeric flavanols, dihydrochalcones and anthocyanins were reported, providing for the first time a quite complete picture of polyphenolic composition of F. vesca berries. Some of the polyphenols herein investigated, such as a tris-galloyl-hexahydroxydiphenoyl-hexose, two castalagin/vescalagin-like isomers and peonidin-malonylglucoside, were described for the first time. Principal component analysis applied on original HPLC-MS/MS data, acquired in multiple reaction monitoring mode, successfully discriminated the four investigated cultivars on the basis of their polyphenolic composition, highlighting the fundamental role of mass spectrometry for food characterization. Copyright © 2012 John Wiley & Sons, Ltd.

  11. High-performance liquid chromatographic separations of stereoisomers of chiral basic agrochemicals with polysaccharide-based chiral columns and polar organic mobile phases.

    Science.gov (United States)

    Matarashvili, Iza; Shvangiradze, Iamze; Chankvetadze, Lali; Sidamonidze, Shota; Takaishvili, Nino; Farkas, Tivadar; Chankvetadze, Bezhan

    2015-12-01

    The separation of the stereoisomers of 23 chiral basic agrochemicals was studied on six different polysaccharide-based chiral columns in high-performance liquid chromatography with various polar organic mobile phases. Along with the successful separation of analyte stereoisomers, emphasis was placed on the effect of the chiral selector and mobile phase composition on the elution order of stereoisomers. The interesting phenomenon of reversal of enantiomer/stereoisomer elution order function of the polysaccharide backbone (cellulose or amylose), type of derivative (carbamate or benzoate), nature, and position of the substituent(s) in the phenylcarbamate moiety (methyl or chloro) and the nature of the mobile phase was observed. For several of the analytes containing two chiral centers all four stereoisomers were resolved with at least one chiral selector/mobile phase combination. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Analysis of 6-mercaptopurine in human plasma with a high-performance liquid chromatographic method including post-column derivatization and fluorimetric detection.

    Science.gov (United States)

    Jonkers, R E; Oosterhuis, B; ten Berge, R J; van Boxtel, C J

    1982-12-10

    A relatively simple assay with improved reliability and sensitivity for measuring levels of 6-mercaptopurine in human plasma is presented. After extraction of the compound and the added internal standard with phenyl mercury acetate, samples were separated by ion-pair reversed-phase high-performance liquid chromatography. On-line the analytes were oxidized to fluorescent products and detected in a flow-fluorimeter. The within-day coefficient of variation was 3.8% at a concentration of 25 ng/ml. The lower detection limit was 2 ng/ml when 1.0 ml of plasma was used. Mercaptopurine concentration versus time curves of two subjects after a single oral dose of azathioprine are shown.

  13. A Novel High Performance Liquid Chromatographic Method for Determination of Nystatin in Pharmaceutical Formulations by Box-Behnken Statistical Experiment Design.

    Science.gov (United States)

    Shokraneh, Farnaz; Asgharian, Ramin; Abdollahpour, Assem; Ramin, Mehdi; Montaseri, Ali; Mahboubi, Arash

    2015-01-01

    In this study a novel High Performance Liquid Chromatography for the assay of nystatin in oral and vaginal tablets were optimized and validated using Box-Behnken experimental design. The method was performed in the isocratic mode on a RP-18 column (30 °C) using a mobile phase consisting of ammonium acetate 0.05 M buffer/ Methanol mixture (30:70) and a flow-rate of 1.0 mL/min. The specificity, linearity, precision, accuracy, LOD and LOQ of the method were validated. The method was linear over the range of 5-500 µg/mL with an acceptable correlation coefficient (r(2) = 0.9996). The method's limit of detection (LOD) and quantification (LOQ) were 0.01 and 0.025 µg/mL respectively. The results indicate that this validated method can be used as an alternative method for assay of nystatin.

  14. Rapid and Low-cost Prototyping of Medical Devices Using 3D Printed Molds for Liquid Injection Molding

    Science.gov (United States)

    Chung, Philip; Heller, J. Alex; Etemadi, Mozziyar; Ottoson, Paige E.; Liu, Jonathan A.; Rand, Larry; Roy, Shuvo

    2014-01-01

    Biologically inert elastomers such as silicone are favorable materials for medical device fabrication, but forming and curing these elastomers using traditional liquid injection molding processes can be an expensive process due to tooling and equipment costs. As a result, it has traditionally been impractical to use liquid injection molding for low-cost, rapid prototyping applications. We have devised a method for rapid and low-cost production of liquid elastomer injection molded devices that utilizes fused deposition modeling 3D printers for mold design and a modified desiccator as an injection system. Low costs and rapid turnaround time in this technique lower the barrier to iteratively designing and prototyping complex elastomer devices. Furthermore, CAD models developed in this process can be later adapted for metal mold tooling design, enabling an easy transition to a traditional injection molding process. We have used this technique to manufacture intravaginal probes involving complex geometries, as well as overmolding over metal parts, using tools commonly available within an academic research laboratory. However, this technique can be easily adapted to create liquid injection molded devices for many other applications. PMID:24998993

  15. Liquid chromatographic/electrospray ionization quadrupole/time of flight tandem mass spectrometric study of polyphenolic composition of different Vaccinium berry species and their comparative evaluation.

    Science.gov (United States)

    Ancillotti, Claudia; Ciofi, Lorenzo; Rossini, Daniele; Chiuminatto, Ugo; Stahl-Zeng, Jianru; Orlandini, Serena; Furlanetto, Sandra; Del Bubba, Massimo

    2017-02-01

    Ultra-high-performance liquid chromatography coupled with high-resolution quadrupole-time of flight mass spectrometry with both negative and positive ionization was used for comprehensively investigating the phenolic and polyphenolic compounds in berries from three spontaneous or cultivated Vaccinium species (i.e., Vaccinium myrtillus, Vaccinium uliginosum subsp. gaultherioides, and Vaccinium corymbosum). More than 200 analytes, among phenolic and polyphenolic compounds belonging to the classes of anthocyanins, monomeric and oligomeric flavonols, flavanols, dihydrochalcones, phenolic acids, together with other polyphenolic compounds of mixed structural characteristics, were identified. Some of the polyphenols herein investigated, such as anthocyanidin glucuronides and malvidin-feruloyl-hexosides in V. myrtillus, or anthocyanindin aldopentosides and coumaroyl-hexosides in V. uliginosum subsp. gaultherioides and a large number of proanthocyanidins with high molecular weight in all species, were described for the first time in these berries. Principal component analysis applied on original LC-TOF data, acquired in survey scan mode, successfully discriminated the three Vaccinium berry species investigated, on the basis of their polyphenolic composition, underlying one more time the fundamental role of mass spectrometry for food characterization.

  16. A reverse phased high-pressure liquid chromatographic method for the estimation of a poisonous matter in Strychnos nux-vomica

    Directory of Open Access Journals (Sweden)

    Achu Hashim

    2015-01-01

    Full Text Available Seeds of Strychnos nux-vomica were subjected to preliminary phytochemical tests and its presence was confirmed by thin layer chromatography (TLC method. The TLC profile of the methanolic extract of seeds of S. nux-vomica was developed using the solvent system toluene:chloroform:methanol in the ratio 8:2:1. The plate was observed in visible light after spraying with Dragendorff′s reagent (specific method. High-performance liquid chromatography (HPLC profile of the methanolic extracts of S. nux-vomica was developed, and the amount of strychnine seems to be 0.36% (w/w in the seeds. The TLC and HPLC profiles developed are very valuable for the identification of the original drug from their adulterants. The TLC profile identifies the presence of strychnine in the plant material. The quantification method for the strychnine in the seeds can be used for the quality standardization of the raw drug because the strychnine is reported to have some toxicity.

  17. Molecularly imprinted polymer for selective extraction of malachite green from seawater and seafood coupled with high-performance liquid chromatographic determination

    International Nuclear Information System (INIS)

    Lian Ziru; Wang Jiangtao

    2012-01-01

    Highlights: ► The malachite green molecularly imprinted polymer (MG-MIP) was prepared. ► The characteristics and regeneration property of MIP were studied. ► An off-line method for MG was developed using MIP as solid-phase extraction. ► The MG concentrations from seawater and seafood samples were determined. - Abstract: In this paper, a highly selective sample cleanup procedure combining molecular imprinting technique (MIT) and solid-phase extraction (SPE) was developed for the isolation of malachite green in seawater and seafood samples. The molecularly imprinted polymer (MIP) was prepared using malachite green as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer. The imprinted polymer and non-imprinted polymer were characterized by scanning electron microscope and static adsorption experiments. The MIP showed a high adsorption capacity and was used as selective sorbent for the SPE of malachite green. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of malachite green in seawater and seafood samples was also established. Finally, five samples were determined. The results showed that malachite green concentration in one seawater sample was at 1.30 μg L −1 and the RSD (n = 3) was 4.15%.

  18. Molecularly imprinted polymer for selective extraction of malachite green from seawater and seafood coupled with high-performance liquid chromatographic determination.

    Science.gov (United States)

    Lian, Ziru; Wang, Jiangtao

    2012-12-01

    In this paper, a highly selective sample cleanup procedure combining molecular imprinting technique (MIT) and solid-phase extraction (SPE) was developed for the isolation of malachite green in seawater and seafood samples. The molecularly imprinted polymer (MIP) was prepared using malachite green as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer. The imprinted polymer and non-imprinted polymer were characterized by scanning electron microscope and static adsorption experiments. The MIP showed a high adsorption capacity and was used as selective sorbent for the SPE of malachite green. An off-line molecularly imprinted solid-phase extraction (MISPE) method followed by high-performance liquid chromatography with diodearray detection for the analysis of malachite green in seawater and seafood samples was also established. Finally, five samples were determined. The results showed that malachite green concentration in one seawater sample was at 1.30 μg L⁻¹ and the RSD (n=3) was 4.15%. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  19. Automated multi-plug filtration cleanup for liquid chromatographic-tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities.

    Science.gov (United States)

    Qin, Yuhong; Zhang, Jingru; Zhang, Yuan; Li, Fangbing; Han, Yongtao; Zou, Nan; Xu, Haowei; Qian, Meiyuan; Pan, Canping

    2016-09-02

    An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC-MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1-14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Liquid chromatographic determination of microcystins in water samples following pre-column excimer fluorescence derivatization with 4-(1-pyrene)butanoic acid hydrazide.

    Science.gov (United States)

    Hayama, Tadashi; Katoh, Kenji; Aoki, Takayoshi; Itoyama, Miki; Todoroki, Kenichiro; Yoshida, Hideyuki; Yamaguchi, Masatoshi; Nohta, Hitoshi

    2012-11-28

    A method to measure the concentrations of microcystins (MCs) in water samples has been developed by incorporating pre-column fluorescence derivatization and liquid chromatography (LC). A solid-phase extraction for pretreatment was used to extract the MCs in water samples. The MCs were derivatized with excimer-forming 4-(1-pyrene)butanoic acid hydrazide (PBH). The MCs could then be detected by fluorescence after separation with a pentafluorophenyl (PFP)-modified superficially porous (core shell) particle LC column. The derivatization reactions of MCs with PBH proceeded easily in the presence of 4,6-dimethoxy-1,3,5-triazin-2-yl-4-methylmorpholinium (DMT-MM) as a condensation reagent, and the resulting derivatives could be easily separated on the PFP column. The derivatives were selectively detected at excimer fluorescence wavelengths (440-540 nm). The instrument detection limit and the instrument quantification limit of the MCs standards were 0.4-1.2 μg L(-1) and 1.4-3.9 μg L(-1), respectively. The method was validated at 0.1 and 1.0 μg L(-1) levels in tap and pond water samples, and the recovery of MCs was between 67 and 101% with a relative standard deviation of 11%. The proposed method can be used to quantify trace amounts of MCs in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Total milk fat extraction and quantification of polar and neutral lipids of cow, goat, and ewe milk by using a pressurized liquid system and chromatographic techniques.

    Science.gov (United States)

    Castro-Gómez, M P; Rodriguez-Alcalá, L M; Calvo, M V; Romero, J; Mendiola, J A; Ibañez, E; Fontecha, J

    2014-11-01

    Although milk polar lipids such as phospholipids and sphingolipids located in the milk fat globule membrane constitute 0.1 to 1% of the total milk fat, those lipid fractions are gaining increasing interest because of their potential beneficial effects on human health and technological properties. In this context, the accurate quantification of the milk polar lipids is crucial for comparison of different milk species, products, or dairy treatments. Although the official International Organization for Standardization-International Dairy Federation method for milk lipid extraction gives satisfactory results for neutral lipids, it has important disadvantages in terms of polar lipid losses. Other methods using mixtures of solvents such as chloroform:methanol are highly efficient for extracting polar lipids but are also associated with low sample throughput, long time, and large solvent consumption. As an alternative, we have optimized the milk fat extraction yield by using a pressurized liquid extraction (PLE) method at different temperatures and times in comparison with those traditional lipid extraction procedures using 2:1 chloroform:methanol as a mixture of solvents. Comparison of classical extraction methods with the developed PLE procedure were carried out using raw whole milk from different species (cows, ewes, and goats) and considering fat yield, fatty acid methyl ester composition, triacylglyceride species, cholesterol content, and lipid class compositions, with special attention to polar lipids such as phospholipids and sphingolipids. The developed PLE procedure was validated for milk fat extraction and the results show that this method performs a complete or close to complete extraction of all lipid classes and in less time than the official and Folch methods. In conclusion, the PLE method optimized in this study could be an alternative to carry out milk fat extraction as a routine method. Copyright © 2014 American Dairy Science Association. Published by

  2. Reverse phase high performance liquid chromatographic method development based on ultravioletvisible detector for the analysis of 1-hydroxypyrene (PAH biomarker) in human urine.

    Science.gov (United States)

    Kamal, Atif; Gulfraz, Mohammad; Anwar, Mohammad Asad; Malik, Riffat Naseem

    2015-01-01

    1-hydroxypyrene is an important biomarker of exposure to polycyclic aromatic hydrocarbons (PAHs), which appears in the urine of exposed human subjects. In developing countries, where advanced instruments are not available, the importance of this biomarker demands convenient and sensitive methods for determination purposes. This study aimed at developing a methodology to quantify 1-hydroxypyrene (a biomarker of PAHs exposure) based on the UV-visible detector in the reverse phase high pressure liquid chromatography (HPLC). A 20 μl injection of sample was used for manual injection into the HPLC Shimadzu, equipped with the SPD-20 A UV-visible detector, the LC-20AT pump and the DGU-20A5 degasser. The C-18 column was used for the purpose of the analysis. The method showed a good linearity (the range: R2 = 0.979-0.989), and high detectability up to the nmol level. The average retention was 6.37, with the accuracy of 2%, and the percentage of recovery remained 108%. The overall performance of this method was comparable (in terms of detection sensitivity) and relatively better than previously reported studies using the HPLC system equipped with the UV-detector. This method is suitable and reliable for the detection/quantification of the 1-OHP in human urine samples, using the UV-detector, however, it is less sensitive as compared to the results of a florescence detector. This work is available in Open Access model and licensed under a CC BY-NC 3.0 PL license.

  3. Liquid chromatographic determination of the cyanobacterial toxin beta-n-methylamino-L-alanine in algae food supplements, freshwater fish, and bottled water.

    Science.gov (United States)

    Scott, Peter M; Niedzwiadek, Barbara; Rawn, Dorothea F K; Lau, Ben P-Y

    2009-08-01

    Beta-N-Methylamino-L-alanine (BMAA) is a neurotoxin originally found in cycad seeds and now known to be produced by many species of freshwater and marine cyanobacteria. We developed a method for its determination in blue-green algae (BGA) food supplements, freshwater fish, and bottled water by using a strong cation-exchange, solid-phase extraction column for cleanup after 0.3 M trichloroacetic acid extraction of BGA supplements and fish. Bottled water was applied directly onto the solid-phase extraction column. For analysis of carbonated water, sonication and pH adjustment to 1.5 were needed. To determine protein-bound BMAA, the protein pellet left after extraction of the BGA supplement and fish was hydrolyzed by boiling with 6 M hydrochloric acid; BMAA was cleaned up on a C18 column and a strong cation-exchange, solid-phase extraction column. Determination of BMAA was by liquid chromatography of the fluorescent derivative formed with 9-fluorenylmethyl chloroformate. The method was validated by recovery experiments using spiking levels of 1.0 to 10 microg/g for BGA supplements, 0.5 to 5.0 microg/g for fish, and 0.002 microg/g for bottled water; mean recoveries were in the range of 67 to 89% for BGA supplements and fish, and 59 to 92% for bottled water. Recoveries of BMAA from spiked extracts of hydrolyzed protein from BGA supplements and fish ranged from 66 to 83%. The cleanup developed provides a useful method for surveying foods and supplements for BMAA and protein-bound BMAA.

  4. Rapid Determination of Amino Acids in Beer, Red Wine, and Donkey-Hide Gelatin by Gradient Elution of HPLC: From Micellar Liquid Chromatography to High Submicellar Liquid Chromatography.

    Science.gov (United States)

    Xie, Yunfei; Luo, Tian; Yang, Jing; Dong, Yuming

    2018-01-01

    Amino acids (AAs) in beer, red wine, and donkey-hide gelatin were rapidly determined by gradient LC elution from micellar LC to high submicellar LC. Mobile phase A was a 0.075 M sodium dodecyl sulfate solution containing 20 mM ammonium acetate with a pH value adjusted to 3.5 with acetic acid solution, and mobile phase B was acetonitrile. Optimized chromatographic conditions were as follows: mobile phase B increased from 25 to 60% (v/v) in 30 min and the use of a Venusil XBP C18 column (5 µm, 250 × 4.6 mm) as the stationary phase, with a column temperature of 35°C, flow rate of 1.2 mL/min, and detection wavelength of 266 nm. The results indicated good linearity (r2 ≥ 0.9924). The intraday precision of the retention time was RSD ≤ 1.1%, whereas interday was RSD ≤ 3.2%; intraday precision of the peak area was RSD ≤ 3.3%, whereas interday was RSD ≤ 4.9%. The range of recovery was 94.6-102.4%. The RSDs of the retention time for the AAs for the different samples were 0.04-0.31%.

  5. A validated stability indicating high-performance liquid chromatographic method for simultaneous estimation of cefuroxime sodium and sulbactam sodium in injection dosage form

    Directory of Open Access Journals (Sweden)

    Falguni M Patel

    2012-01-01

    Full Text Available Background: A fixed dose combination of cefuroxime sodium (β lactam antibiotic and sulbactam sodium (β Lactamase inhibitor is used in ratio of 2:1 as powder for injection for the treatment of resistant lower respiratory tract and other infections. Aims: A simple, precise, and accurate ion-pair reverse-phase high-performance liquid chromatography (RP-HPLC method was developed and validated for determination of cefuroxime Na(CEF and sulbactam Na(SUL in injection. Materials and Methods: Isocratic RP-HPLC separation was achieved on an ACE C 18 column (150×4.6 mm id, 5 μm particle size using the mobile phase 0.002 M tetrabutylammonium hydroxide sulfate (TBAH in 10 mm potassium di-hydrogen phosphate buffer-acetonitrile (86:14 v/v, pH 3.7 at a flow rate of 1.0 ml/min. Results and Conclusion: The retention time of sulbactam Na and cefuroxime Na were 3.2 min and 10.2 min, respectively. The ion-pairing reagent improved the retention of highly polar sulbactam Na on reverse-phase column. The detection was performed at 210 nm. The method was validated for linearity, precision, accuracy, robustness, solution stability, and specificity. The method was validated for linearity, precision, accuracy, robustness, solution stability, and specificity. The method was linear in the concentration range of 10-100 μg/ml for cefuroxime Na and 5-50 μg/ml for sulbactam Na, with a correlation coefficient of 0.9999 and 0.9998 for the respective drugs. The intraday precision was 0.13-0.21% and 0.48-0.65%, and the interday precision was 0.32-0.81% and 0.60-0.83% for cefuroxime Na and sulbactam Na, respectively. The accuracy (recovery was found to be in the range of 98.76-100.61% and 98.99-100.30% for cefuroxime Na and sulbactam Na, respectively. The drugs were found to degrade under hydrolytic and oxidative conditions. The drugs could be effectively separated from different degradation products, and hence the method can be used for stability analysis.

  6. Chiral separations of cathinone and amphetamine-derivatives: Comparative study between capillary electrochromatography, supercritical fluid chromatography and three liquid chromatographic modes.

    Science.gov (United States)

    Albals, Dima; Heyden, Yvan Vander; Schmid, Martin G; Chankvetadze, Bezhan; Mangelings, Debby

    2016-03-20

    The screening part of an earlier defined chiral separation strategy in capillary electrochromatography (CEC) was used for the separation of ten cathinone- and amphetamine derivatives. They were analyzed using 4 polysaccharide-based chiral stationary phases (CSPs), containing cellulose tris(3,5-dimethylphenylcarbamate) (ODRH), amylose tris(3,5-dimethylphenylcarbamate) (ADH), amylose tris(5-chloro-2-methylphenylcarbamate) (LA2), and cellulose tris(4-chloro-3-methylphenylcarbamate) (LC4) as chiral selectors. After applying the screening to each compound, ADH and LC4 showed the highest success rate. In a second part of the study, a comparison between CEC and other analytical techniques used for chiral separations i.e., supercritical fluid chromatography (SFC), polar organic solvent chromatography (POSC), reversed-phase (RPLC) and normal-phase liquid chromatography (NPLC), was made. For this purpose, earlier defined screening approaches for each technique were applied to separate the 10 test substances. This allowed an overall comparison of the success rates of the screening steps of the 5 techniques for these compounds. The results showed that CEC had a similar enantioselectivity rate as NPLC and RPLC, producing the highest number of separations (9 out of 10 racemates). SFC resolved 7 compounds, while POSC gave only 2 separations. On the other hand, the baseline separation success rates for NPLC and RPLC was better than for CEC. For a second comparison, the same chiral stationary phases as in the CEC screening were also tested with all techniques at their specific screening conditions, which allowed a direct comparison of the performance of CEC versus the same CSPs in the other techniques. This comparison revealed that RPLC was able to separate all tested compounds, and also produced the highest number of baseline separations on the CSP that were used in the CEC screening step. CEC and NPLC showed the same success rate: nine out of ten substances were separated. When

  7. A microfluidic platform for the rapid determination of distribution coefficients by gravity assisted droplet-based liquid-liquid extraction

    DEFF Research Database (Denmark)

    Poulsen, Carl Esben; Wootton, Robert C. R.; Wolff, Anders

    2015-01-01

    The determination of pharmacokinetic properties of drugs, such as the distribution coefficient, D, is a crucial measurement in pharmaceutical research. Surprisingly, the conventional (gold standard) technique used for D measurements, the shake-flask method, is antiquated and unsuitable...... for the testing of valuable and scarce drug candidates. Herein we present a simple micro fluidic platform for the determination of distribution coefficients using droplet-based liquid-liquid extraction. For simplicity, this platform makes use of gravity to enable phase separation for analysis and is 48 times...... the apparent acid dissociation constant, pK', as a proxy for inter-system comparison. Our platform determines a pK' value of 7.24 ± 0.15, compared to 7.25 ± 0.58 for the shake-flask method in our hands and 7.21 for the shake-flask method in literature. Devices are fabricated using injection moulding, the batch...

  8. Rapid Determination of Imatinib in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jeong Soo; Cho, Eun Gi; Huh, Wooseong; Ko, Jaewook; Jung, Jin Ah; Lee, Sooyoun [Samsung Medical Center, Seoul (Korea, Republic of)

    2013-08-15

    A simple, fast and robust analytical method was developed to determine imatinib in human plasma using liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode. Imatinib and labeled internal standard were extracted from plasma with a simple protein precipitation. The chromatographic separation was performed using an isocratic elution of mobile phase involving 5.0 mM ammonium formate in water -5.0 mM ammonium formate in methanol (30:70, v/v) over 3.0 min on reversed-stationary phase. The detection was performed using a triple-quadrupole tandem mass spectrometer in multiple-reaction monitoring mode. The developed method was validated with lower limit of quantification of 10 ng/mL. The calibration curve was linear over 10-2000 ng/mL (R{sup 2} > 0.99). The method validation parameters met the acceptance criteria. The spiked samples and standard solutions were stable under conditions for storage and handling. The reliable method was successfully applied to real sample analyses and thus a pharmacokinetic study in 27 healthy Korean male volunteers.

  9. Rapid method for determination of glyphosate in groundwater using high performance liquid chromatography and solid-phase extraction after derivatization

    Directory of Open Access Journals (Sweden)

    Valdir Eduardo Olivo

    2015-04-01

    Full Text Available The intensive use of pesticides in agriculture has prompted researchers to develop new methods for identifying these pollutants in water. This study sought to validate a high performance liquid chromatography (HPLC method to determine the concentration of the pesticide glyphosate in groundwater samples by using solid-phase extraction (SPE filters after derivatization with chloroformate 9-fluorenylmethoxycarbonyl (FMOC-Cl. For the HPLC method, we evaluated the following main validation parameters: linearity, specificity, precision, accuracy, robustness, and limits of detection and quantification. After validation of the method, we determined the concentration of glyphosate in samples from thirteen deep, tubular wells distributed in urban and rural areas in Chapecó, SC, Brazil. The solvent used in the extraction of excess FMOC-Cl was dichloromethane and subsequently filtration was performed on C18 SPE, and injected into the chromatograph column in amino polymer with fluorescence detection. The analytical curve made in ultrapure water was linear, with a correlation coefficient of 0.99. The limits of detection and quantification were 0.24 and 0.07 µg L-1, respectively. Recovery tests in natural waters ranged from 90.37 to 101.70%. Glyphosate was detected in 5 of the thirteen wells evaluated. The highest concentration of glyphosate (6.80 µg L-1 was detected in a countryside well, near the municipal water supply. Despite the low levels of glyphosate detected in our study, any amount present in groundwater samples is worrisome, as these molecules have low ground mobility.

  10. Rapid determination of gross alpha and beta activity in seafood utilizing microwave digestion and liquid scintillation counting

    International Nuclear Information System (INIS)

    Daniel Sas; Jiri Janda; Alena Tokarova

    2015-01-01

    This paper describes a method for rapid determination of gross alpha and beta activity in seafood using liquid scintillation counting and microwave digestion for fast sample decomposition. The general group of seafood was divided into two groups based on its structure, whether it has shell or not. The selected group of radionuclides was chosen with respect to military significance, radiotoxicity, and possibility of potential misuse. 90 Sr and 239 Pu were selected as model radionuclides. (author)

  11. Simple setup for gas-phase H/D exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale.

    Science.gov (United States)

    Mistarz, Ulrik H; Brown, Jeffery M; Haselmann, Kim F; Rand, Kasper D

    2014-12-02

    Gas-phase hydrogen/deuterium exchange (HDX) is a fast and sensitive, yet unharnessed analytical approach for providing information on the structural properties of biomolecules, in a complementary manner to mass analysis. Here, we describe a simple setup for ND3-mediated millisecond gas-phase HDX inside a mass spectrometer immediately after ESI (gas-phase HDX-MS) and show utility for studying the primary and higher-order structure of peptides and proteins. HDX was achieved by passing N2-gas through a container filled with aqueous deuterated ammonia reagent (ND3/D2O) and admitting the saturated gas immediately upstream or downstream of the primary skimmer cone. The approach was implemented on three commercially available mass spectrometers and required no or minor fully reversible reconfiguration of gas-inlets of the ion source. Results from gas-phase HDX-MS of peptides using the aqueous ND3/D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium uptake of Leu-Enkephalin and Glu-Fibrinopeptide B, confirmed that this gas-phase HDX-MS approach allows for labeling of sites (heteroatom-bound non-amide hydrogens located on side-chains, N-terminus and C-terminus) not accessed by classical solution-phase HDX-MS. The simple setup is compatible with liquid chromatography and a chip-based automated nanoESI interface, allowing for online gas-phase HDX-MS analysis of peptides and proteins separated on a liquid chromatographic time scale at increased throughput. Furthermore, online gas-phase HDX-MS could be performed in tandem with ion mobility separation or electron transfer dissociation, thus enabling multiple orthogonal analyses of the structural properties of peptides and proteins in a single automated LC-MS workflow.

  12. Rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Yang, Xiao; Diao, Chun-Peng; Sun, Ai-Ling; Liu, Ren-Min

    2014-10-01

    A method for the rapid pretreatment and determination of bisphenol A in water samples based on vortex-assisted liquid-liquid microextraction followed by high-performance liquid chromatography with fluorescence detection was proposed in this paper. A simple apparatus consisting of a test tube and a cut-glass dropper was designed and applied to collect the floating extraction drop in liquid-liquid microextraction when low-density organic solvent was used as the extraction solvent. Solidification and melting steps that were tedious but necessary once the low-density organic solvent used as extraction solvent could be avoided by using this apparatus. Bisphenol A was selected as model pollutant and vortex-assisted liquid-liquid microextraction was employed to investigate the usefulness of the apparatus. High-performance liquid chromatography with fluorescence detection was selected as the analytical tool for the detection of bisphenol A. The linear dynamic range was from 0.10 to 100 μg/L for bisphenol A, with good squared regression coefficient (r(2) = 0.9990). The relative standard deviation (n = 7) was 4.7% and the limit of detection was 0.02 μg/L. The proposed method had been applied to the determination of bisphenol A in natural water samples and was shown to be economical, fast, and convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Interface for the rapid analysis of liquid samples by accelerator mass spectrometry

    Science.gov (United States)

    Turteltaub, Kenneth; Ognibene, Ted; Thomas, Avi; Daley, Paul F; Salazar Quintero, Gary A; Bench, Graham

    2014-02-04

    An interface for the analysis of liquid sample having carbon content by an accelerator mass spectrometer including a wire, defects on the wire, a system for moving the wire, a droplet maker for producing droplets of the liquid sample and placing the droplets of the liquid sample on the wire in the defects, a system that converts the carbon content of the droplets of the liquid sample to carbon dioxide gas in a helium stream, and a gas-accepting ion source connected to the accelerator mass spectrometer that receives the carbon dioxide gas of the sample in a helium stream and introduces the carbon dioxide gas of the sample into the accelerator mass spectrometer.

  14. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    Pharmacotherapy Group, Faculty of Pharmacy, University of Benin, Benin City, 300001 Nigeria. All rights reserved. ... Additionally, tablet splitting can minimize treatment costs for patients. [6]. ..... using the design space approach. Talanta. 2013 ...

  15. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    and weighed with the analytical balance. .... was analyzed occasionally to ensure the .... Retention time .... The authors declare that this work was done by .... Life Sci. 2002; 767: 341–351. 31. US Pharmacopeial Convention. United States.

  16. Liquid Chromatographic Analysis of Hydraulic Fluids.

    Science.gov (United States)

    1979-11-01

    chemical mixtures of a petroleum- or nonpetroleum-base stock component formulated with various additives which may be present in trace amounts or...absorb UV radiation near the monitoring wavelength may swamp the detector signal and therefore should be avoided in 1JV detection. The recorder trace of...Also, organic phosphites , thiophosphates, and sulfides are used to inhibit oxidative catalysis by metal ions. The oxidation inhibitor in 6083D-0 is BPC

  17. High Performance Liquid Chromatographic Determination of ...

    African Journals Online (AJOL)

    150 mm×4.6 mm, 5μm) by isocratic elution at 25oC The mobile phase consisted of phosphate buffered saline (pH = 4.5) and methanol (40/60, v/v). The flow rate was set at 0.8 ml/min and the effluent was monitored using a DAD set at 260 nm.

  18. Determination of solute descriptors by chromatographic methods

    International Nuclear Information System (INIS)

    Poole, Colin F.; Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K.

    2009-01-01

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  19. Determination of solute descriptors by chromatographic methods.

    Science.gov (United States)

    Poole, Colin F; Atapattu, Sanka N; Poole, Salwa K; Bell, Andrea K

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  20. Mixed-mode chromatographic matrices for the resolution of transfer ribonucleic acids

    NARCIS (Netherlands)

    Bischoff, Rainer; Mclaughlin, L.W.

    1984-01-01

    Modification of approximately 65% of the amine groups of an aminopropylsilyl bonded-phase silica high-performance liquid chromatographic anion exchanger (APS-Hypersil) with organic acids containing n-alkyl moieties of different chain lengths, results in mixed mode chromatographic matrices of varying

  1. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDfurfurals will contribute to characterise and quantify their presence in the human diet.

  2. Deformation and instabilities at a free surface of liquid subject to a local rapid evaporation

    International Nuclear Information System (INIS)

    Marechal, Anne

    1993-01-01

    This research thesis first addresses theoretical aspects related to the study of stationary system (the deformation of the liquid-vapour interface) and to the study of the linear stability of this interface, and more particularly the study of the liquid-vapour interface of a fluid heated by electron bombardment in a vacuum enclosure. The author reports the analysis of Landau and Palmer systems, reports the study of the marginal stability of a simplified SILVA (isotopic separation by laser on atomic vapour) system which allows the identification of destabilizing mechanisms, and the comparison between a liquid system heated from underneath with liquid system heated from above. Results are then validated by experimental results. In the next part, the author sets the equations of a SILVA system closer to reality by addressing vapour in a more realistic way. Results of conventional kinetic theory are studied again by analysing sonic evaporation of a liquid. The author reports a study of the linear stability of this system, and reports an attempt to analyse the obtained results [fr

  3. Electrokinetic migration across artificial liquid membranes. New concept for rapid sample preparation of biological fluids.

    Science.gov (United States)

    Pedersen-Bjergaard, Stig; Rasmussen, Knut Einar

    2006-03-24

    Basic drug substances were transported across a thin artificial organic liquid membrane by the application of 300 V d.c. From a 300 microl aqueous donor compartment (containing 10 mM HCl), the drugs migrated through a 200 microm artificial liquid membrane of 2-nitrophenyl octyl ether immobilized in the pores of a polypropylene hollow fiber, and into a 30 microl aqueous acceptor solution of 10 mM HCl inside the lumen of the hollow fiber. The transport was forced by an electrical potential difference sustained over the liquid membrane, resulting in electrokinetic migration of drug substances from the donor compartment to the acceptor solution. Within 5 min of operation at 300 V, pethidine, nortriptyline, methadone, haloperidol, and loperamide were extracted with recoveries in the range 70-79%, which corresponded to enrichments in the range 7.0-7.9. The chemical composition of the organic liquid membrane strongly affected the permeability, and may serve as an efficient tool for controlling the transport selectivity. Water samples, human plasma, and human urine were successfully processed, and in light of the present report, electrokinetic migration across thin artificial liquid membranes may be an interesting tool for future isolation within chemical analysis.

  4. [Rapid determination of theophylline, theobromine and caffeine in dietary supplements containing guarana by ultra-performance liquid chromatography].

    Science.gov (United States)

    Hasegawa, Takashi; Takahashi, Kazunaga; Saijo, Masaaki; Ishii, Toshiyasu; Nagata, Tomoko

    2009-12-01

    A rapid and simple method for determination of theophylline, theobromine and caffeine in dietary supplements containing guarana by ultra-performance liquid chromatography (UPLC) has been developed. Theophylline, theobromine and caffeine were extracted from finely powdered samples with water in a boiling water bath for 20 min, then the extracts were filtered and the filtrates were subjected to UPLC. Liquid samples were diluted with water and filteres, and the filtrates were subjected to UPLC. UPLC separation was performed on an AQUITY UPLC BEH C18 column (2.1 mm i.d.x50 mm, 1.7 microm, Waters) with 10 mmol/L ammonium acetate buffer (pH 4.0)-acetonitrile gradient and eluates were monitored at 275 nm. The recoveries of theophylline (spiked at 200 microg/g [tablet] and 50 microg/mL [liquid]), theobromine (spiked at 200 microg/g [tablet] and 50 microg/mL [liquid]) and caffeine (spiked at 1,000 microg/g [tablet] and 250 microg/mL [liquid]) were 97.6-98.7%, 97.3-99.7%, 97.1-105.4%, respectively. The quantitation limits of theophylline, theobromine and caffeine were 10 microg/g (seed, seed powder, tablet and capsule) and 2.0 microg/mL (liquid) each. When this analytical method was applied to commercial dietary supplements, theophylline, theobromine and caffeine were found at concentrations of 4.45 mg/tablet, 5.48 mg/tablet, 139 mg/tablet, respectively. Taking 4 tablets of this product according to the directions on the package could be dangerous to consumers because of possible overdosing of these ingredients.

  5. Rapid simultaneous determination of organophosphorus pesticides in human serum and urine by liquid chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Zlatković Milica

    2010-01-01

    Full Text Available Background/Aim. Analysis of organophosphosphorus compounds and their metabolites in a biological material includes the use of numerous methods, covering both preparation of samples for analysis and their identification that is considered to be very complex. Low concentrations monitoring requires implementation of highly sensitive analytical techniques. The aim of this study was to develop and validate an original and sensitive method for the detection and quantitation of organophosphorus pesticides (dimethoate, diazinon, malathion and malaoxon in human biological matrices (serum, urine. Methods. This method was based on a solid-phase extraction procedure, a chromatographic separation using an ACQUITY UPLC ® HSST3 column and mass spectrometric detection in the positve ion mode. Mobile phase: was consited of Solvent A (5 mM ammonium formate pH 3.0 and Solvent B (0.1% acetic formate in methanol, in a linear gradient (constant flow-rate 0.3 mL/min. Results. The standard curve was linear in the range of 0.05-5.00 mg/L for malathion and malaoxon, 0.10-5.00 mg/L for dimethoate and 0.05-2.50 mg/L for diazinon. The correlation coefficient was r ≥ 0.99. Extraction recoveries were satisfactory and ranged between 90-99%. The limits of detection (LOD was between 0.007- 0.07 mg/L and the limits of quantitation (LOQ ranged between 0.022-0.085 mg/L. Intra- and interassay precision and accuracy were satisfactory for all of the pesticides analyzed. Conclusion. The method of liquid chromatography - mass spectrometry is simple, accurate, and useful for the determination of organophosphorus pesticides in both clinical and forensic toxicology.

  6. Development, validation and application of an ultra high performance liquid chromatographic-tandem mass spectrometric method for the simultaneous detection and quantification of five different classes of veterinary antibiotics in swine manure.

    Science.gov (United States)

    Van den Meersche, Tina; Van Pamel, Els; Van Poucke, Christof; Herman, Lieve; Heyndrickx, Marc; Rasschaert, Geertrui; Daeseleire, Els

    2016-01-15

    In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 μg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure

  7. Dual quantification of dapivirine and maraviroc in cervicovaginal secretions from ophthalmic tear strips and polyester-based swabs via liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis.

    Science.gov (United States)

    Parsons, Teresa L; Emory, Joshua F; Seserko, Lauren A; Aung, Wutyi S; Marzinke, Mark A

    2014-09-01

    Topical microbicidal agents are being actively pursued as a modality to prevent HIV viral transmission during sexual intercourse. Quantification of antiretroviral agents in specimen sources where antiviral activity is elicited is critical, and drug measurements in cervicovaginal fluid can provide key information on local drug concentrations. Two antiretroviral drugs, dapivirine and maraviroc, have gained interest as vaginal microbicidal agents, and rugged methods are required for their quantification in cervicovaginal secretions. Cervicovaginal fluid spiked with dapivirine and maraviroc were applied to ophthalmic tear strips or polyester-based swabs to mimic collection procedures used in clinical studies. Following sample extraction and the addition of isotopically labeled internal standards, samples were subjected to liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis using a Waters BEH C8, 50mm×2.1mm, 1.7μm particle size column, on an API 4000 mass analyzer operated in selective reaction monitoring mode. The method was validated according to FDA Bioanalytical Method Validation guidelines. Due to the disparate saturation capacity of the tested collection devices, the analytical measuring ranges for dapivirine and maravirocin cervicovaginal fluid on the ophthalmic tear strip were 0.05-25ng/tear strip, and 0.025-25ng/tear strip, respectively. As for the polyester-based swab, the analytical measuring ranges were 0.25-125ng/swab for dapivirine and 0.125-125ng/swab for maraviroc. Dilutional studies were performed for both analytes to extended ranges of 25,000ng/tear strip and 11,250ng/swab. Standard curves were generated via weighted (1/x(2)) linear or quadratic regression of calibrators. Precision, accuracy, stability and matrix effects studies were all performed and deemed acceptable according to the recommendations of the FDA Bioanalytical Method Validation guidelines. A rugged LC-MS/MS method for the dual quantification of dapivirine and

  8. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    Science.gov (United States)

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Room-temperature saturated ferroelectric polarization in BiFeO3 ceramics synthesized by rapid liquid phase sintering

    International Nuclear Information System (INIS)

    Wang, Y.P.; Zhou, L.; Zhang, M.F.; Chen, X.Y.; Liu, J.-M.; Liu, Z.G.

    2004-01-01

    Single-phased ferroelectromagnet BiFeO 3 ceramics with high resistivity were synthesized by a rapid liquid phase sintering technique. Saturated ferroelectric hysteresis loops were observed at room temperature in the ceramics sintered at 880 deg. C for 450 s. The spontaneous polarization, remnant polarization, and the coercive field are 8.9 μC/cm 2 , 4.0 μC/cm 2 , and 39 kV/cm, respectively, under an applied field of 100 kV/cm. It is proposed that the formation of Fe 2+ and an oxygen deficiency leading to the higher leakage can be greatly suppressed by the very high heating rate, short sintering period, and liquid phase sintering technique. The latter was also found effective in increasing the density of the ceramics. The sintering technique developed in this work is expected to be useful in synthesizing other ceramics from multivalent or volatile starting materials

  10. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  11. An on-line push/pull perfusion-based hollow-fiber liquid-phase microextraction system for high-performance liquid chromatographic determination of alkylphenols in water samples.

    Science.gov (United States)

    Chao, Yu-Ying; Jian, Zhi-Xuan; Tu, Yi-Ming; Wang, Hsaio-Wen; Huang, Yeou-Lih

    2013-06-07

    In this study, we employed a novel on-line method, push/pull perfusion hollow-fiber liquid-phase microextraction (PPP-HF-LPME), to extract 4-tert-butylphenol, 2,4-di-tert-butylphenol, 4-n-nonylphenol, and 4-n-octylphenol from river and tap water samples; we then separated and quantified the extracted analytes through high-performance liquid chromatography (HPLC). Using this approach, we overcame the problem of fluid loss across the porous HF membrane to the donor phase, permitting on-line coupling of HF-LPME to HPLC. In our PPP-HF-LPME system, we used a push/pull syringe pump as the driving source to perfuse the acceptor phase, while employing a heating mantle and an ultrasonic probe to accelerate mass transfer. We optimized the experimental conditions such as the nature of the HF supported intermediary phase and the acceptor phase, the composition of the donor and acceptor phases, the sample temperature, and the sonication conditions. Our proposed method provided relative standard deviations of 3.1-6.2%, coefficients of determination (r(2)) of 0.9989-0.9998, and limits of detection of 0.03-0.2 ng mL(-1) for the analytes under the optimized conditions. When we applied this method to analyses of river and tap water samples, our results confirmed that this microextraction technique allows reliable monitoring of alkylphenols in water samples.

  12. A novel analytical method of 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine in fluids of drug addicts using liquid-liquid extraction-gas chromatographic/nitrogen-phosphorous detection

    Directory of Open Access Journals (Sweden)

    Jing Chang

    2017-01-01

    Full Text Available In accordance with the research specifications and guidelines in China, we developed a novel experimental method to detect new piperazine-type drugs, such as 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine. In this study, a new pretreatment method and gas chromatography (GC/nitrogen-phosphorus detector detection technique were used to characterize these two kinds of drugs in urine and blood samples. For the purpose of isolation of these trace drugs from the samples, liquid-liquid extraction/solid-phase extraction was modified and validated for this specific study. The pretreatment method presented in this paper has many advantages, such as high recovery rate, high extraction efficiency, high detection sensitivity, low limit of detection, and simple operation. The GC/NPD instrument is popular in most laboratories because it can meet the routine requirements of forensic science. All these aspects make this combination of sample pretreatment and GC/NPD technique the most suitable choice for drug detection in biological samples.

  13. Gas chromatographic column for the Viking 1975 molecular analysis experiment

    Science.gov (United States)

    Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

    1975-01-01

    A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

  14. Radioimmunoassay of methaqualone in human urine compared with chromatographic methods

    International Nuclear Information System (INIS)

    Mule, S.J.; Kogan, M.; Jukofsky, D.

    1978-01-01

    The 125 I-radioimmunoassay for methaqualone in human urine was evaluated by a comparison with newly modified gas-liquid chromatographic and thin-layer chromatographic methods. The statistically significant sensitivity value for the radioimmunoassay was at 2 μg of methaqualone per liter of urine. The coefficient of variation was 2.88 -+ 0.16% intraassay. There was cross-reactivity only with metabolites of methaqualone, 4'-hydroxymethaqualone being twice as sensitively measured as methaqualone. There was complete agreement between results by radioimmunoassay and by gas-liquid chromatography in 96.7% of the samples analyzed. Only 1.2% of the radioimmunoassay values were false positives, and 2.1% false negatives (phi = 0.8917, P < 0.001). Comparisons between the thin-layer chromatographic data and the gas--liquid chromatographic or radioimmunoassay data showed less agreement because of the 50- to 200-fold higher sensitivity of the latter techniques. Gas--liquid chromatography therefore appears to represent the best reference method for the evaluation of the radioimmunoassay, which appears to be a very sensitive and reliable technique for detecting methaqualone and its metabolites in human urine

  15. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Method for chromatographically recovering scandium and yttrium

    International Nuclear Information System (INIS)

    Snyder, T.S.; Stoltz, R.A.

    1991-01-01

    This paper describes a method for chromatographically recovering scandium and yttrium from the residue of a sand chlorinator. It comprises: providing a residue from a sand chlorinator, the residue containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; digesting the residue with an acid to produce an aqueous liquid containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; feeding the metal containing liquid through a cation exchanger; eluding the cation exchanger with an acid eluant to to produce: a first eluate containing at least half of the total weight of the calcium and sodium in the feed liquid; a second eluate containing at least half of the total weight of the one or more radioactive metals in the feed liquid; a third eluate containing at least half of the yttrium in the feed liquid, and a fourth eluate containing at least half of the weight of the scandium in the feed liquid

  17. Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Lei Zhang

    2014-01-01

    Full Text Available Rapid Resolution Liquid Chromatography coupled with Electrospray Ionization Tandem Mass Spectrometry (RRLC-ESI-MSn was used to separate and identify related substances in ampicillin capsule. The fragmentation behaviors of related substances were used to identify their chemical structures. Finally, a total of 13 related substances in ampicillin capsule were identified, including four identified components for the first time and three groups of isomers on the basis of the exact mass, fragmentation behaviors, retention time, and chemical structures in the literature. This study avoided time-consuming and complex chemosynthesis of related substances of ampicillin and the results could be useful for the quality control of ampicillin capsule to guarantee its safety in clinic. In the meantime, it provided a good example for the rapid identification of chemical structures of related substances of drugs.

  18. Simultaneous determination of dapsone, monoacetyldapsone and pyrimethamine in whole blood and plasma by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Lemnge, M M; Rønn, A; Flachs, H

    1993-01-01

    A sensitive, selective and rapid reversed-phase high-performance liquid chromatographic method was developed for the simultaneous analysis of dapsone, monoacetyldapsone and pyrimethamine in human whole blood and plasma. The procedure involved extraction of the compounds and the internal standard...

  19. Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

    Science.gov (United States)

    Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

    2017-12-01

    Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.

  20. Impurity analysis in EC-99mTC radiotracer using chromatographic techniques

    International Nuclear Information System (INIS)

    Almeida, E.V.; Fukumori, N.T.O.; Mengatti, J.; Silva, C.P.G.; Matsuda, M.M.N.

    2008-01-01

    The objective of this study was to develop two chromatographic methods of impurity analysis in radiotracer 99m Tc-EC: the Thin Layer Chromatography (TLC) and the High Performance Liquid Chromatography Reversed Phase (HPLC-RP)

  1. Rapid conversion of sorbitol to isosorbide in hydrophobic ionic liquids under microwave irradiation.

    Science.gov (United States)

    Kamimura, Akio; Murata, Kengo; Tanaka, Yoshiki; Okagawa, Tomoki; Matsumoto, Hiroshi; Kaiso, Kouji; Yoshimoto, Makoto

    2014-12-01

    Sorbitol was effectively converted to isosorbide by treatment with [TMPA][NTf2 ] in the presence of catalytic amounts of TsOH under microwave heating at 180 °C. The reaction completed within 10 min and isosorbide was isolated to about 60%. Ionic liquids were readily recovered by an extraction treatment and reused several times. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Centrifuge-less dispersive liquid-liquid microextraction base on the solidification of switchable solvent for rapid on-site extraction of four pyrethroid insecticides in water samples.

    Science.gov (United States)

    Hu, Lu; Wang, Huazi; Qian, Heng; Liu, Chaoran; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Xu, Donghui

    2016-11-11

    An on-site dispersive liquid liquid microextraction base on the solidification of switchable solvent has been developed as a simple, rapid and eco-friendly sample extraction method for the fast determination of pyrethroid insecticides in aqueous samples using high-performance liquid chromatography with ultraviolet detection. In this extraction method, medium-chain saturated fatty acids (n≥10), which can rapidly solidify at low temperatures (centrifugation. The microextraction process was performed in a 10mL syringe and the pretreatment process could thus be finished in 5min. No external energy resources were required in this method, which makes it a potential method for on-site extraction. The optimal experimental parameters were as follows: 350μL of decanoic acid (1mol/L) was used as the extraction solvent, 150μL of sulfuric acid (2mol/L) was used to decrease the pH of the samples, no salt was added, and the temperature of the samples was in the range of 20-40°C. Finally, the sample was cooled in an ice bath for three minutes. Under these optimal conditions, good responses for four pyrethroid insecticides were obtained in the concentration ranges of 1-500μg/L, with coefficients of determination greater than 0.9993. The recoveries of the four pyrethroid insecticides ranged from 84.7 to 95.3%, with relative standard deviations ranging from 1.6 to 4.6%. The limits of detection based on a signal-to-noise ratio of 3 were in the range of 0.24-0.68μg/L, and the enrichment factors were in the range of 121-136. The results demonstrate that this method was successfully applied to determine pyrethroid insecticides in real water samples. No centrifugation or any special apparatus are required, make this a promising method for rapid field-sampling procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Microwave-assisted ionic liquid-mediated rapid catalytic conversion of non-edible lignocellulosic Sunn hemp fibres to biofuels.

    Science.gov (United States)

    Paul, Souvik Kumar; Chakraborty, Saikat

    2018-04-01

    Sunn hemp fibre - a cellulose-rich crystalline non-food energy crop, containing 75.6% cellulose, 10.05% hemicellulose, 10.32% lignin, with high crystallinity (80.17%) and degree of polymerization (650) - is identified as a new non-food substrate for lignocellulosic biofuel production. Microwave irradiation is employed to rapidly rupture the cellulose's glycosidic bonds and enhance glucose yield to 78.7% at 160 °C in only 46 min. The reactants - long-chain cellulose, ionic liquid, transition metal catalyst, and water - form a polar supramolecular complex that rotates under the microwave's alternating polarity and rapidly dissipates the electromagnetic energy through molecular collisions, thus accelerating glycosidic bond breakage. In 46 min, 1 kg of Sunn hemp fibres containing 756 g of cellulose produces 595 g of glucose at 160 °C, and 203 g of hydroxymethyl furfural (furanic biofuel precursor) at 180 °C. Yeast mediated glucose fermentation produces 75.6% bioethanol yield at 30 °C, and the ionic liquid is recycled for cost-effectiveness. Copyright © 2018 Elsevier Ltd. All rights reserved.

  4. Rapid and sensitive analysis of phthalate metabolites, bisphenol A, and endogenous steroid hormones in human urine by mixed-mode solid-phase extraction, dansylation, and ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Wang, He-xing; Wang, Bin; Zhou, Ying; Jiang, Qing-wu

    2013-05-01

    Steroid hormone levels in human urine are convenient and sensitive indicators for the impact of phthalates and/or bisphenol A (BPA) exposure on the human steroid hormone endocrine system. In this study, a rapid and sensitive method for determination of 14 phthalate metabolites, BPA, and ten endogenous steroid hormones in urine was developed and validated on the basis of ultra-performance liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry. The optimized mixed-mode solid phase-extraction separated the weakly acidic or neutral BPA and steroid hormones from acidic phthalate metabolites in urine: the former were determined in positive ion mode with a methanol/water mobile phase containing 10 mM ammonium formate; the latter were determined in negative ion mode with a acetonitrile/water mobile phase containing 0.1 % acetic acid, which significantly alleviated matrix effects for the analysis of BPA and steroid hormones. Dansylation of estrogens and BPA realized simultaneous and sensitive analysis of the endogenous steroid hormones and BPA in a single chromatographic run. The limits of detection were less than 0.84 ng/mL for phthalate metabolites and less than 0.22 ng/mL for endogenous steroid hormones and BPA. This proposed method had satisfactory precision and accuracy, and was successfully applied to the analyses of human urine samples. This method could be valuable when investigating the associations among endocrine-disrupting chemicals, endogenous steroid hormones, and relevant adverse outcomes in epidemiological studies.

  5. Lithium adduct as precursor ion for sensitive and rapid quantification of 20 (S)-protopanaxadiol in rat plasma by liquid chromatography/quadrupole linear ion trap mass spectrometry and application to rat pharmacokinetic study.

    Science.gov (United States)

    Bao, Yuanwu; Wang, Quanying; Tang, Pingming

    2013-03-01

    A novel, rapid and sensitive liquid chromatography/quadrupole linear ion trap mass spectrometry [LC-ESI-(QqLIT)MS/MS] method was developed and validated for the quantification of protopanaxadiol (PPD) in rat plasma. Oleanolic acid (OA) was used as internal standard (IS). A simple protein precipitation based on acetonitrile (ACN) was employed. Chromatographic separation was performed on a Sepax GP-C18 column (50 × 2.1 mm, 5 μM) with a mobile phase consisting of ACN-water and 1.5 μM formic acid and 25 mM lithium acetate (90 : 10, v/v) at a flow rate of 0.4 ml/min for 3.0 min. Multiple-reaction-monitoring mode was performed using lithium adduct ion as precursor ion of m/z 467.5/449.4 and 455.6/407.4 for the drug and IS, respectively. Calibration curve was recovered over a concentration range of 0.5-100 ng/ml with a correlation coefficient >0.99. The limit of detection was 0.2 ng/ml in rat plasma for PPD. The results of the intraday and interday precision and accuracy studies were well within the acceptable limits. The validated method was successfully applied to investigate the pharmacokinetic study of PPD after intravenous and gavage administration to rat. Copyright © 2013 John Wiley & Sons, Ltd.

  6. Rapid Identification of unstable acyl glucoside flavonoids of Oxytropis racemosa Turcz by high-performance liquid chromatography-diode array detection-electrospray ionisation/multi-stage mass spectrometry.

    Science.gov (United States)

    Song, Shuang; Zheng, Xiu-Ping; Liu, Wei-Dong; Du, Rui-Fang; Feng, Zi-Ming; Zhang, Pei-Cheng; Bi, Li-Fu

    2013-02-01

    Oxytropis racemosa Turcz is an important minority medicine that is used mainly to improve children's indigestion, especially in inner Mongolia and Tibet. Previous studies indicated that the characteristic constituents of this plant are acylated flavonoids. Rapidly identify the characteristic chemical constituents of O. racemosa by high-performance liquid chromatography-diode array detection-electrospray ionisation/multi-stage mass spectrometry (HPLC-DAD-ESI/MS(n) ) and suggest a useful method to control the quality of this medicinal plant. In the HPLC fingerprint, 32 flavonoids were tentatively identified by a detailed analysis of their mass spectra, UV spectra and retention times. Furthermore, 13 flavonoids were confirmed by comparison with previously isolated compounds obtained from O. racemosa. In total, 32 flavonoids, including 13 flavonoids with 3-hydroxy-3-methylglutaric acid (HMG) moieties and four flavonoids with 3-malonyl moieties, were identified in the extract of O. racemosa. Among the compounds identified, 10 were characterised as new compounds for their particular acylated sugar moieties. The method described is effective for obtaining a comprehensive phytochemical profile of plants containing unstable acylated flavonoids. The method is also useful for constructing the chromatographic fingerprint of the minority medicine -O. racemosa Turcz for quality control. Copyright © 2012 John Wiley & Sons, Ltd.

  7. Molecular dynamics study of dynamic and structural properties of supercooled liquid and glassy iron in the rapid-cooling processes

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Qi-Long; Huang, Duo-Hui; Yang, Jun-Sheng; Wan, Min-Jie; Wang, Fan-Hou, E-mail: eatonch@gmail.com

    2014-10-01

    Molecular dynamics simulations were applied to study the dynamic and structural properties of supercooled liquid and glassy iron in the rapid-cooling processes. The mean-square displacement and the non-Gaussian parameter were used to describe the dynamic properties. The evolution of structural properties was investigated using the pair distribution functions and bond-angle distribution functions. Results for dynamic and structural relaxations indicate that the dynamic features are consistently correlated with the structure evolution, and there are three temperature regions as the temperature decreases: (1) at higher temperatures (1500 K, 1300 K, and 1100 K), the system remains in the liquid characteristics during the overall relaxation process. (2) At medial temperatures (1050 K, 900 K, and 700 K), a fast β-relaxation is followed by a much slower α-relaxation. There is a little change in the structural properties in the β-relaxation region, while major configuration rearrangements occurred in the α-relaxation range and the crystallization process was completed at the end of α-relaxation region. (3) At lower temperature (500 K), the system shows glassy characteristics during the overall relaxation process. In addition, the melting temperature, glass transition temperature and diffusion coefficients of supercooled liquid iron are also computed.

  8. Direct coupling of a dense (supercritical) gas chromatograph to a mass spectrometer using a supersonic molecular beam interface

    International Nuclear Information System (INIS)

    Randall, L.G.; Wahrhaftig, A.L.

    1981-01-01

    A detecting mass spectrometer has been successfully coupled to a dense gas (supercritical fluid) chromatograph to produce an instrument (DGC/MS) that may be an alternative to high performance liquid chromatograph/mass spectrometer instruments (HPLC/MS) and gas chromatograph/mass spectrometer instruments (GC/MS) for analysis of involatile and/or thermally labile compounds. The mobile phase in DGC is a gas held at temperatures above the critical temperature and at pressures sufficient to obtain nearly liquid-like densities. DGC combines advantages of GC and HPLC: rapid separations, moderate operating temperatures, and analysis of involatile compounds. An advantage unique to DGC is the solvent power dependence upon pressure. While several groups have studied DGC, its development has been limited by the lack of a sensitive and selective detector. Hence, work has been directed towards the design and construction of a DGC/MS resulting in a trial instrument capable of chromatographic pressures of at least 300 atm and temperatures from 10 0 to 60 0 C. The DGC/MS coupling has been accomplished by the use of a supersonic molecular beam interface. This application of molecular beam formation appears to be unique in its requirements of a large pressure ratio (approx.10 8 ), low flow rates, and low final pressures. The authors outline characteristics of supersonic jets and molecular beams pertinent to the design of such an instrument. The interface which uses pumping speeds of 2400 and 1200 l/s in the beam forming chambers is described in detail, while the other components: the detecting mass spectrometer, the dense gas supply, and the DGC: are briefly described. Preliminary work with this instrument has established the feasibility of DGC/MS as an analytical technique and further development is recommended

  9. [Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Liu, Hualiang; Wang, Yuan; Zhu, Baoli

    2015-11-01

    To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides. After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode. The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%. This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

  10. Rapid characterisation of Klebsiella oxytoca isolates from contaminated liquid hand soap using mass spectrometry, FTIR and Raman spectroscopy.

    Science.gov (United States)

    Dieckmann, Ralf; Hammerl, Jens Andre; Hahmann, Hartmut; Wicke, Amal; Kleta, Sylvia; Dabrowski, Piotr Wojciech; Nitsche, Andreas; Stämmler, Maren; Al Dahouk, Sascha; Lasch, Peter

    2016-06-23

    Microbiological monitoring of consumer products and the efficiency of early warning systems and outbreak investigations depend on the rapid identification and strain characterisation of pathogens posing risks to the health and safety of consumers. This study evaluates the potential of three rapid analytical techniques for identification and subtyping of bacterial isolates obtained from a liquid hand soap product, which has been recalled and reported through the EU RAPEX system due to its severe bacterial contamination. Ten isolates recovered from two bottles of the product were identified as Klebsiella oxytoca and subtyped using matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI TOF MS), near-infrared Fourier transform (NIR FT) Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. Comparison of the classification results obtained by these phenotype-based techniques with outcomes of the DNA-based methods pulsed-field gel electrophoresis (PFGE), multi-locus sequence typing (MLST) and single nucleotide polymorphism (SNP) analysis of whole-genome sequencing (WGS) data revealed a high level of concordance. In conclusion, a set of analytical techniques might be useful for rapid, reliable and cost-effective microbial typing to ensure safe consumer products and allow source tracking.

  11. A new immersion sensor for rapid electrochemical determination of dissolved oxygen in liquid metals

    International Nuclear Information System (INIS)

    Janke, D.; Schwerdtfeger, K.

    1978-01-01

    Development of a new solid electrolyte 'needle sensor' with ZrO 2 or ThO 2 electrolyte and metal-metal oxide reference mixture for the rapid determination of oxygen in steel melts. Details of the manufacture of the layer-structured, miniaturized probe. Test results of simultaneous measurements performed with the newly developed ZrO 2 needle sensor and the hitherto usual tubular sensor in iron melts at oxygen activities between 0.00005 and 0.030. (orig.) [de

  12. Disorder trapping by rapidly moving phase interface in an undercooled liquid

    Science.gov (United States)

    Galenko, Peter; Danilov, Denis; Nizovtseva, Irina; Reuther, Klemens; Rettenmayr, Markus

    2017-08-01

    Non-equilibrium phenomena such as the disappearance of solute drag, the origin of solute trapping and evolution of disorder trapping occur during fast transformations with originating metastable phases [D.M. Herlach, P.K. Galenko, D. Holland-Moritz, Metastable solids from undrercooled melts (Elsevier, Amsterdam, 2007)]. In the present work, a theoretical investigation of disorder trapping by a rapidly moving phase interface is presented. Using a model of fast phase transformations, a system of governing equations for the diffusion of atoms, and the evolution of both long-range order parameter and phase field variable is formulated. First numerical solutions are carried out for a congruently melting binary alloy system.

  13. Three rapid methods for determination 90Sr in milk samples using liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Abbasisiara, F.; Attarilar, N.; Afshar, N.

    2006-01-01

    Strontium radionuclide 90 Sr is one of the main long-lived components of the radioactive fallout which occurred as a result of previous atmospheric nuclear tests and also nuclear accidents such as Chernobyl accident. Due to chemical and biochemical similarities between strontium and calcium, more than 99% of strontium is efficiently incorporated into bone tissue and teeth and Characterized by along physical and biological half-life, it may cause damage to bone marrow. Since determination of this radionuclide often is a time consuming process, rapid determination methods specially in emergency situations is always desirable. In this work, three rapid methods for determination of this radionuclide in milk samples will be evaluated. All of the methods include two major steps: 1- strontium separation from fats and proteins which can be performed by drying (in case of the fresh milk samples), ashing and leaching by nitric acids or by using exchange or chelating resins which have strong affinity for alkaline earth cations such as Dowex 50W-X8. And 2- Separation of Sr-90 or its daughter product, Y-90. In two methods separation of 90 Sr is performed by extraction of the daughter nuclide, 90 Y, by aid of organic extracting agent, Tributylphosphate or T.B.P., and then Cherenkov counting of the Y-90 extracted. The third method is based on separation of this radionuclide using Crown Ether or Sr -Spec resin. The detailed radiochemical procedures and evaluation of each method advantages or disadvantages will explained in full text paper. (authors)

  14. Rapid radiometric detection of microbial contamination using 14C-glucose and standard liquid scintillation counting system

    International Nuclear Information System (INIS)

    Joshi, S.H.; Kamble, S.B.; Pilkhwal, N.S.; Ramamoorthy, N.

    1998-01-01

    A simple and rapid method for detection of microbial contamination based on quantitation of 14 CO 2 released during metabolism of 14 C-Glucose by microorganisms is reported. Liquid scintillation counting system (LSCS) with a modified sample preparation method was utilised. The scintillator was impregnated on Whatman-1 paper on which 14 CO 2 evolved during metabolism could be absorbed. The important parameters of counting such as efficiency, position sensitivity and geometry as well as effect of NaOH quantity and of microbial load on detection period were studied. The efficiency of radioactivity assay was 18±2.8 %. Contamination of the order of 5-10 organism/ml of product could be detected in about 24 hours. (author)

  15. Rapid determination of vitamin D₃ in milk-based infant formulas by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kwak, Byung-Man; Jeong, In-Seek; Lee, Moon-Seok; Ahn, Jang-Hyuk; Park, Jong-Su

    2014-12-15

    A rapid and simple sample preparation method for vitamin D3 (cholecalciferol) was developed for emulsified dairy products such as milk-based infant formulas. A sample was mixed in a 50 mL centrifuge tube with the same amount of water and isopropyl alcohol to achieve chemical extraction. Ammonium sulfate was used to induce phase separation. No-heating saponification was performed in the sample tube by adding KOH, NaCl, and NH3. Vitamin D3 was then separated and quantified using liquid chromatography-tandem mass spectrometry. The results for added recovery tests were in the range 93.11-110.65%, with relative standard deviations between 2.66% and 2.93%. The results, compared to those obtained using a certified reference material (SRM 1849a), were within the range of the certificated values. This method could be implemented in many laboratories that require time and labour saving. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. Rapid liquid phase sintered Mn doped BiFeO3 ceramics with enhanced polarization and weak magnetization

    Science.gov (United States)

    Kumar, Manoj; Yadav, K. L.

    2007-12-01

    Single-phase BiFe1-xMnxO3 multiferroic ceramics have been synthesized by rapid liquid phase sintering method to study the influence of Mn substitution on their crystal structure, dielectric, magnetic, and ferroelectric behaviors. From XRD analysis it is seen that Mn substitution does not affect the crystal structure of the BiFe1-xMnxO3 system. An enhancement in magnetization was observed for BiFe1-xMnxO3 ceramics. However, the ferooelectric hysteresis loops were not really saturated, we observed a spontaneous polarization of 10.23μC /cm2 under the applied field of 42kV/cm and remanent polarization of 3.99μC/cm2 for x =0.3 ceramic.

  17. Rapid screening for drugs of abuse in biological fluids by ultra high performance liquid chromatography/Orbitrap mass spectrometry.

    Science.gov (United States)

    Jagerdeo, Eshwar; Schaff, Jason E

    2016-08-01

    We present a UPLC(®)-High Resolution Mass Spectrometric method to simultaneously screen for nineteen benzodiazepines, twelve opiates, cocaine and three metabolites, and three "Z-drug" hypnotic sedatives in both blood and urine specimens. Sample processing consists of a high-speed, high-temperature enzymatic hydrolysis for urine samples followed by a rapid supported liquid extraction (SLE). The combination of ultra-high resolution chromatography with high resolution mass spectrometry allows all 38 analytes to be uniquely detected with a ten minute analytical run. Limits of detection for all target analytes are 3ng/mL or better, with only 0.3mL of specimen used for analysis. The combination of low sample volume with fast processing and analysis makes this method a suitable replacement for immunoassay screening of the targeted drug classes, while providing far superior specificity and better limits of detection than can routinely be obtained by immunoassay. Published by Elsevier B.V.

  18. Three rapid methods for determination {sup 90}Sr in milk samples using liquid scintillation spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Abbasisiara, F.; Attarilar, N. [Iranian Nuclear Regulatory Authority (INRA), Atomic Energy Organization of Iran (AEOI), Environmental Radiation Protection Div., National Radiation Protection Dept. (Iran, Islamic Republic of); Afshar, N. [Tarbiat Modarres Univ. (Iran, Islamic Republic of)

    2006-07-01

    Strontium radionuclide {sup 90}Sr is one of the main long-lived components of the radioactive fallout which occurred as a result of previous atmospheric nuclear tests and also nuclear accidents such as Chernobyl accident. Due to chemical and biochemical similarities between strontium and calcium, more than 99% of strontium is efficiently incorporated into bone tissue and teeth and Characterized by along physical and biological half-life, it may cause damage to bone marrow. Since determination of this radionuclide often is a time consuming process, rapid determination methods specially in emergency situations is always desirable. In this work, three rapid methods for determination of this radionuclide in milk samples will be evaluated. All of the methods include two major steps: 1- strontium separation from fats and proteins which can be performed by drying (in case of the fresh milk samples), ashing and leaching by nitric acids or by using exchange or chelating resins which have strong affinity for alkaline earth cations such as Dowex 50W-X8. And 2- Separation of Sr-90 or its daughter product, Y-90. In two methods separation of {sup 90}Sr is performed by extraction of the daughter nuclide, {sup 90}Y, by aid of organic extracting agent, Tributylphosphate or T.B.P., and then Cherenkov counting of the Y-90 extracted. The third method is based on separation of this radionuclide using Crown Ether or Sr -Spec resin. The detailed radiochemical procedures and evaluation of each method advantages or disadvantages will explained in full text paper. (authors)

  19. Rapid determination of fumonisins in corn-based products by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Li, Wei; Herrman, Timothy J; Dai, Susie Y

    2010-01-01

    A simple, fast, and robust method was developed for the determination of fumonisin B1 (FB1), fumonisin B2 (FB2), and fumonisin B3 (FB3) in corn-based human food and animal feed (cornmeal). The method involves a single extraction step followed by centrifugation and filtration before analysis by ultra-performance liquid chromatographylelectrospray ionization (UPLC/ESI)-MS/MS. The LC/MS/MS method developed here represents the fastest and simplest procedure (<30 min) among both conventional HPLC methods and other LC/MS methods using SPE cleanup. The potential for high throughput analysis makes the method particularly beneficial for regulatory agencies and analytical laboratories with a high sample volume. A single-laboratory validation was conducted by testing three different spiking levels (200, 500, and 1000 ng/g for FB1 and FB2; 100, 250, and 500 ng/g for FB3) for accuracy and precision. Recoveries of FB1 ranged from 93 to 98% with RSD values of 3-8%. Recoveries of FB2 ranged from 104 to 108%, with RSD values of 2-6%. Recoveries of FB3 ranged from 94 to 108%, with RSD values of 2-5%.

  20. Rapid production of Candida albicans chlamydospores in liquid media under various incubation conditions.

    Science.gov (United States)

    Alicia, Zavalza-Stiker; Blanca, Ortiz-Saldivar; Mariana, García-Hernández; Magdalena, Castillo-Casanova; Alexandro, Bonifaz

    2006-01-01

    The production of chlamydospores is a diagnostic tool used to identify Candida albicans; these structures also represent a model for morphogenetic research. The time required to produce them with standard methods is 48-72 hours in rice meal agar and tensoactive agents. This time can be shorted using liquid media such as cornmeal broth (CMB) and dairy supplements. Five media were tested: CMB plus 1% Tween-80, CMB plus 5% milk, CMB plus 5% milk serum, milk serum, and milk serum plus 1% Tween-80, under different incubation conditions: at 28 degrees C and 37 degrees C in a metabolic bath stirring at 150 rpm, and at 28 degrees C in a culture stove. The reading time points were established at 8 and 16 hours. The best results were obtained at 16 hours with CMB plus 5% milk under incubation at 28 degrees C and stirring at 150 rpm. The next most efficient methods were CMB plus 5% milk serum and CMB plus 1% Tween-80, under the same incubation conditions. The other media were ineffective in producing chlamydospores. The absence of stirring at 28 degrees C prevented the formation of chlamydospores within the set time points, and incubation at 37 degrees C decreased their production. This paper reports that the time to form C. albicans chlamydospores can be reduced.

  1. Rapid and sensitive liquid chromatography-tandem mass spectrometric method for the quantitative determination of potentially harmful substance 5,5'-oxydimethylenebis (2-furfural) in traditional Chinese medicine injections.

    Science.gov (United States)

    Zang, Qingce; Gao, Yang; Huang, Luojiao; He, Jiuming; Lin, Sheng; Jin, Hongtao; Zhang, Ruiping; Abliz, Zeper

    2018-03-01

    With the rapid development and wide application of traditional Chinese medicine injection (TCMI), a number of adverse events of some TCMIs have incessantly been reported and have drawn broad attention in recent years. Establishing effective and practical analytical methods for safety evaluation and quality control of TCMI can help to improve the safety of TCMIs in clinical applications. In this study, a sensitive and rapid high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method has been developed and validated for the quantitative determination of potentially harmful substance 5,5'-oxydimethylenebis (2-furfural, OMBF) in TCMI samples. Chromatographic separation was performed on a C18 reversed-phase column (150 mm × 2.1 mm, 5 µm) by gradient elution, using methanol-water containing 0.1% formic acid as mobile phase at the flow rate of 0.3 mL/min. MS/MS detection was performed on a triple quadrupole mass spectrometer with positive electrospray ionization in the multiple reaction-monitoring mode. The method was sensitive with a limit of quantification of 0.3 ng/mL and linear over the range of 0.3-30 ng/mL ( r =0.9998). Intra- and inter-day precision for analyte was <9.52% RSD with recoveries in the range 88.0-109.67% at three concentration levels. The validated method was successfully applied to quantitatively determine the compound OMBF in TCMIs and glucose injections. Our study indicates that this method is simple, sensitive, practicable and reliable, and could be applied for safety evaluation and quality control of TCMIs and glucose injections.

  2. Rapid and sensitive liquid chromatography–tandem mass spectrometric method for the quantitative determination of potentially harmful substance 5,5′-oxydimethylenebis (2-furfural in traditional Chinese medicine injections

    Directory of Open Access Journals (Sweden)

    Qingce Zang

    2018-03-01

    Full Text Available With the rapid development and wide application of traditional Chinese medicine injection (TCMI, a number of adverse events of some TCMIs have incessantly been reported and have drawn broad attention in recent years. Establishing effective and practical analytical methods for safety evaluation and quality control of TCMI can help to improve the safety of TCMIs in clinical applications. In this study, a sensitive and rapid high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS method has been developed and validated for the quantitative determination of potentially harmful substance 5,5′-oxydimethylenebis (2-furfural, OMBF in TCMI samples. Chromatographic separation was performed on a C18 reversed-phase column (150 mm × 2.1 mm, 5 µm by gradient elution, using methanol–water containing 0.1% formic acid as mobile phase at the flow rate of 0.3 mL/min. MS/MS detection was performed on a triple quadrupole mass spectrometer with positive electrospray ionization in the multiple reaction-monitoring mode. The method was sensitive with a limit of quantification of 0.3 ng/mL and linear over the range of 0.3–30 ng/mL (r=0.9998. Intra- and inter-day precision for analyte was <9.52% RSD with recoveries in the range 88.0–109.67% at three concentration levels. The validated method was successfully applied to quantitatively determine the compound OMBF in TCMIs and glucose injections. Our study indicates that this method is simple, sensitive, practicable and reliable, and could be applied for safety evaluation and quality control of TCMIs and glucose injections. KEY WORDS: 5,5′-Oxydimethylenebis (2-furfural, LC–MS/MS, Quantitative analytical method, Traditional Chinese medicine injection, Quality control

  3. Chromatographic analysis and purification of multiply tritium-labelled eicosanoids

    International Nuclear Information System (INIS)

    Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

    1988-01-01

    A comparative study of different chromatographic techniques (gas-liquid (GLC), thin-layer (TLC), liquid (LC), high-pressure liquid (HPLC) chromatography) is presented. They were applied to the analysis and preparative purification of tritium-labelled eicosanoids with a molar radioactivity of 1.8-8.8 TBq/mmol, obtained by selective hydrogenation and by chemical or enzymic methods. The possibility of analyzing reaction mixtures and isolating individual multiply labelled eicosanoids with a chemical and radiochemical purity of 95-98% was demonstrated. Special features of HPLC for high molar radioactivity eicosanoids are considered. (author) 9 refs.; 6 tabs

  4. Rapid determination of triclosan in personal care products using new in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction coupled with high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Chen, Ming-Jen; Liu, Ya-Ting; Lin, Chiao-Wen; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

    2013-03-12

    This paper describes the development of a novel, simple and efficient in-tube based ultrasound-assisted salt-induced liquid-liquid microextraction (IT-USA-SI-LLME) technique for the rapid determination of triclosan (TCS) in personal care products by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. IT-USA-SI-LLME method is based on the rapid phase separation of water-miscible organic solvent from the aqueous phase in the presence of high concentration of salt (salting-out phenomena) under ultrasonication. In the present work, an indigenously fabricated home-made glass extraction device (8-mL glass tube inbuilt with a self-scaled capillary tip) was utilized as the phase separation device for USA-SI-LLME. After the extraction, the upper extractant layer was narrowed into the self-scaled capillary tip by pushing the plunger plug; thus, the collection and measurement of the upper organic solvent layer was simple and convenient. The effects of various parameters on the extraction efficiency were thoroughly evaluated and optimized. Under optimal conditions, detection was linear in the concentration range of 0.4-100ngmL(-1) with correlation coefficient of 0.9968. The limit of detection was 0.09ngmL(-1) and the relative standard deviations ranged between 0.8 and 5.3% (n=5). The applicability of the developed method was demonstrated for the analysis of TCS in different commercial personal care products and the relative recoveries ranged from 90.4 to 98.5%. The present method was proven to be a simple, sensitive, less organic solvent consuming, inexpensive and rapid procedure for analysis of TCS in a variety of commercially available personal care products or cosmetic preparations. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Rapid determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction and ultraperformance convergence chromatography tandem mass spectrometry.

    Science.gov (United States)

    Deng, Huimin; Yang, Fei; Li, Zhonghao; Bian, Zhaoyang; Fan, Ziyan; Wang, Ying; Liu, Shanshan; Tang, Gangling

    2017-07-21

    Aromatic amines in mainstream cigarette smoke have long been monitored due to their carcinogenic toxicity. In this work, a reliable and rapid method was developed for the simultaneous determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction (DLLME) and ultraperformance convergence chromatography tandem mass spectrometry (UPC 2 -MS/MS). Briefly, the particulate phase of the cigarette smoke was captured by a Cambridge filter pad, and diluted hydrogen chloride aqueous solution is employed to extract the aromatic amines under mechanical shaking. After alkalization with sodium hydroxide solution, small amount of toluene was introduced to further extract and enrich aromatic amines by modified DLLME under vortexing. After centrifugation, toluene phase was purified by a universal QuEChERS cleanup kit and was finally analyzed by UPC 2 -MS/MS. Attributing to the superior performance of UPC 2 -MS/MS, this novel approach allowed the separation and determination of 9 aromatic amines within 5.0min with satisfactory resolution and sensitivity. The proposed method was finally validated using Kentucky reference cigarette 3R4F, and emission levels of targeted aromatic amines determined were comparable to previously reported methods At three different spiked levels, the recoveries of most analytes were ranged from 74.01% to 120.50% with relative standard deviation (RSD) less than 12%, except that the recovery of p-toluidine at low spiked level and 3-aminobiphenyl at medium spiked level was 62.77% and 69.37% respectively. Thus, this work provides a novel alternative method for the simultaneous analysis of 9 aromatic amines in mainstream cigarette smoke. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    Energy Technology Data Exchange (ETDEWEB)

    Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

    2005-02-15

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

  7. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Lim, Chang Hyun

    2005-01-01

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

  8. Rapid Solid-Liquid Dynamic Extraction (RSLDE): a New Rapid and Greener Method for Extracting Two Steviol Glycosides (Stevioside and Rebaudioside A) from Stevia Leaves.

    Science.gov (United States)

    Gallo, Monica; Vitulano, Manuela; Andolfi, Anna; DellaGreca, Marina; Conte, Esterina; Ciaravolo, Martina; Naviglio, Daniele

    2017-06-01

    Stevioside and rebaudioside A are the main diterpene glycosides present in the leaves of the Stevia rebaudiana plant, which is used in the production of foods and low-calorie beverages. The difficulties associated with their extraction and purification are currently a problem for the food processing industries. The objective of this study was to develop an effective and economically viable method to obtain a high-quality product while trying to overcome the disadvantages derived from the conventional transformation processes. For this reason, extractions were carried out using a conventional maceration (CM) and a cyclically pressurized extraction known as rapid solid-liquid dynamic extraction (RSLDE) by the Naviglio extractor (NE). After only 20 min of extraction using the NE, a quantity of rebaudioside A and stevioside equal to 1197.8 and 413.6 mg/L was obtained, respectively, while for the CM, the optimum time was 90 min. From the results, it can be stated that the extraction process by NE and its subsequent purification developed in this study is a simple, economical, environmentally friendly method for producing steviol glycosides. Therefore, this method constitutes a valid alternative to conventional extraction by reducing the extraction time and the consumption of toxic solvents and favouring the use of the extracted metabolites as food additives and/or nutraceuticals. As an added value and of local interest, the experiment was carried out on stevia leaves from the Benevento area (Italy), where a high content of rebaudioside A was observed, which exhibits a sweet taste compared to stevioside, which has a significant bitter aftertaste.

  9. Performance of chromatographic systems to model soil-water sorption.

    Science.gov (United States)

    Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

    2012-08-24

    A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Miniaturized chromatographic radiochemical procedure for 131I - MIBG

    International Nuclear Information System (INIS)

    Barboza, M.F. de; Pereira, N.S. de; Colturato, M.T.; Silva, C.P.G. da.

    1989-12-01

    Different solvents were used in paper chromatographic methods to obtain the best system in routine radiochemical control for 131 I-MIBG produced at IPEN-CNEN/SP. The dates were compared with those obtained with eletrophoresis method in buffer acetate, pH=4.5, 350V, during 40 minutes. The stability of the labeled compound store under 4 0 C was studied during 15 days. Miniaturized chromatographic procedures were established using Whatman 3MM (8x1cm) and n-butanol-:acetic acid: water (S:2:1) as a solvent. the Rf values were: 0.3 (I - ) and 1.0 (MIBG). The radiochemical purity was 99.3 and 99.2% (first day) obtained with eletrophoresis and miniaturized chromatographic procedures, respectively and, 84.7% after 15 days of its preparation. It is a rapid, practical and reproductive method. (author) [pt

  11. Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

    2015-02-27

    A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (∼20μL). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7μm) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/μL, while method quantification limits were between 0.05 and 2.3pg/μL. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20μL plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/μL (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as

  12. Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

    Science.gov (United States)

    Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

    2014-01-01

    This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Chromatographic and electrophoretic approaches in ink analysis.

    Science.gov (United States)

    Zlotnick, J A; Smith, F P

    1999-10-15

    Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

  14. Artificial neural network model for photosynthetic pigments identification using multi wavelength chromatographic data

    Science.gov (United States)

    Prilianti, K. R.; Hariyanto, S.; Natali, F. D. D.; Indriatmoko, Adhiwibawa, M. A. S.; Limantara, L.; Brotosudarmo, T. H. P.

    2016-04-01

    The development of rapid and automatic pigment characterization method become an important issue due to the fact that there are only less than 1% of plant pigments in the earth have been explored. In this research, a mathematical model based on artificial intelligence approach was developed to simplify and accelerate pigment characterization process from HPLC (high-performance liquid chromatography) procedure. HPLC is a widely used technique to separate and identify pigments in a mixture. Input of the model is chromatographic data from HPLC device and output of the model is a list of pigments which is the spectrum pattern is discovered in it. This model provides two dimensional (retention time and wavelength) fingerprints for pigment characterization which is proven to be more accurate than one dimensional fingerprint (fixed wavelength). Moreover, by mimicking interconnection of the neuron in the nervous systems of the human brain, the model have learning ability that could be replacing expert judgement on evaluating spectrum pattern. In the preprocessing step, principal component analysis (PCA) was used to reduce the huge dimension of the chromatographic data. The aim of this step is to simplify the model and accelerate the identification process. Six photosynthetic pigments i.e. zeaxantin, pheophytin a, α-carotene, β-carotene, lycopene and lutein could be well identified by the model with accuracy up to 85.33% and processing time less than 1 second.

  15. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Rapid methods to determine procyanidins, anthocyanins, theobromine and caffeine in rat tissues by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Serra, Aida; Macià, Alba; Romero, Maria-Paz; Piñol, Carme; Motilva, Maria-José

    2011-06-01

    Rapid, selective and sensitive methods were developed and validated to determine procyanidins, anthocyanins and alkaloids in different biological tissues, such as liver, brain, the aorta vein and adipose tissue. For this purpose, standards of procyanidins (catechin, epicatechin, and dimer B(2)), anthocyanins (cyanidin-3-glucoside and malvidin-3-glucoside) and alkaloids (theobromine, caffeine and theophylline) were used. The methods included the extraction of homogenized tissues by off-line liquid-solid extraction, and then solid-phase extraction to analyze alkaloids, or microelution solid-phase extraction plate for the analysis of procyanidins and anthocyanins. The eluted extracts were then analyzed by ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry, using a triple quadrupole as the analyzer. The optimum extraction solution was water/methanol/phosphoric acid 4% (94/4.5/1.5, v/v/v). The extraction recoveries were higher than 81% for all the studied compounds in all the tissues, except the anthocyanins, which were between 50 and 65% in the liver and brain. In order to show the applicability of the developed methods, different rat tissues were analyzed to determine the procyanidins, anthocyanins and alkaloids and their generated metabolites. The rats had previously consumed 1g of a grape pomace extract (to analyze procyanidins and anthocyanins) or a cocoa extract (to analyze alkaloids) per kilogram of body weight. Different tissues were extracted 4h after administration of the respective extracts. The analysis of the metabolites revealed a hepatic metabolism of procyanidins. The liver was the tissue which produced a greater accumulation of these metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Non-invasive transdermal two-dimensional mapping of cutaneous oxygenation with a rapid-drying liquid bandage.

    Science.gov (United States)

    Li, Zongxi; Roussakis, Emmanuel; Koolen, Pieter G L; Ibrahim, Ahmed M S; Kim, Kuylhee; Rose, Lloyd F; Wu, Jesse; Nichols, Alexander J; Baek, Yunjung; Birngruber, Reginald; Apiou-Sbirlea, Gabriela; Matyal, Robina; Huang, Thomas; Chan, Rodney; Lin, Samuel J; Evans, Conor L

    2014-11-01

    Oxygen plays an important role in wound healing, as it is essential to biological functions such as cell proliferation, immune responses and collagen synthesis. Poor oxygenation is directly associated with the development of chronic ischemic wounds, which affect more than 6 million people each year in the United States alone at an estimated cost of $25 billion. Knowledge of oxygenation status is also important in the management of burns and skin grafts, as well as in a wide range of skin conditions. Despite the importance of the clinical determination of tissue oxygenation, there is a lack of rapid, user-friendly and quantitative diagnostic tools that allow for non-disruptive, continuous monitoring of oxygen content across large areas of skin and wounds to guide care and therapeutic decisions. In this work, we describe a sensitive, colorimetric, oxygen-sensing paint-on bandage for two-dimensional mapping of tissue oxygenation in skin, burns, and skin grafts. By embedding both an oxygen-sensing porphyrin-dendrimer phosphor and a reference dye in a liquid bandage matrix, we have created a liquid bandage that can be painted onto the skin surface and dries into a thin film that adheres tightly to the skin or wound topology. When captured by a camera-based imaging device, the oxygen-dependent phosphorescence emission of the bandage can be used to quantify and map both the pO2 and oxygen consumption of the underlying tissue. In this proof-of-principle study, we first demonstrate our system on a rat ischemic limb model to show its capabilities in sensing tissue ischemia. It is then tested on both ex vivo and in vivo porcine burn models to monitor the progression of burn injuries. Lastly, the bandage is applied to an in vivo porcine graft model for monitoring the integration of full- and partial-thickness skin grafts.

  18. Isocratic Solid Phase Extraction-Liquid Chromatography (SPE-LC) Interfaced to High-Performance Tandem Mass Spectrometry for Rapid Protein Identification

    DEFF Research Database (Denmark)

    Hørning, Ole B; Kjeldsen, Frank; Theodorsen, Søren

    2008-01-01

    the isocratic solid phase extraction-liquid chromatography (SPE-LC) technology for rapid separation ( approximately 8 min) of simple peptide samples. We now extend these studies to demonstrate the potential of SPE-LC separation in combination with a hybrid linear ion trap-Orbitrap tandem mass spectrometer...

  19. Development of an automated on-line pepsin digestion-liquid chromatography-tandem mass spectrometry configuration for the rapid analysis of protein adducts of chemical warfare agents

    NARCIS (Netherlands)

    Carol-Visser, J.; van der Schans, M.; Fidder, A.; Huist, A.G.; van Baar, B.L.M.; Irth, H.; Noort, D.

    2008-01-01

    Rapid monitoring and retrospective verification are key issues in protection against and non-proliferation of chemical warfare agents (CWA). Such monitoring and verification are adequately accomplished by the analysis of persistent protein adducts of these agents. Liquid chromatography-mass

  20. Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

    Science.gov (United States)

    Xu, Jiao-Jiao; Zhou, Jian; Huang, Bai-Fen; Cai, Zeng-Xuan; Xu, Xiao-Min; Ren, Yi-Ping

    2016-06-01

    A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Rapid quantification of underivatized amino acids in plasma by hydrophilic interaction liquid chromatography (HILIC) coupled with tandem mass-spectrometry.

    Science.gov (United States)

    Prinsen, Hubertus C M T; Schiebergen-Bronkhorst, B G M; Roeleveld, M W; Jans, J J M; de Sain-van der Velden, M G M; Visser, G; van Hasselt, P M; Verhoeven-Duif, N M

    2016-09-01

    Amino acidopathies are a class of inborn errors of metabolism (IEM) that can be diagnosed by analysis of amino acids (AA) in plasma. Current strategies for AA analysis include cation exchange HPLC with post-column ninhydrin derivatization, GC-MS, and LC-MS/MS-related methods. Major drawbacks of the current methods are time-consuming procedures, derivative problems, problems with retention, and MS-sensitivity. The use of hydrophilic interaction liquid chromatography (HILIC) columns is an ideal separation mode for hydrophilic compounds like AA. Here we report a HILIC-method for analysis of 36 underivatized AA in plasma to detect defects in AA metabolism that overcomes the major drawbacks of other methods. A rapid, sensitive, and specific method was developed for the analysis of AA in plasma without derivatization using HILIC coupled with tandem mass-spectrometry (Xevo TQ, Waters). Excellent separation of 36 AA (24 quantitative/12 qualitative) in plasma was achieved on an Acquity BEH Amide column (2.1×100 mm, 1.7 μm) in a single MS run of 18 min. Plasma of patients with a known IEM in AA metabolism was analyzed and all patients were correctly identified. The reported method analyzes 36 AA in plasma within 18 min and provides baseline separation of isomeric AA such as leucine and isoleucine. No separation was obtained for isoleucine and allo-isoleucine. The method is applicable to study defects in AA metabolism in plasma.

  2. Qualitative and Quantitative Analysis of Andrographis paniculata by Rapid Resolution Liquid Chromatography/Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jian-Fei Qin

    2013-09-01

    Full Text Available A rapid resolution liquid chromatography/time-of-flight tandem mass spectrometry (RRLC-TOF/MS method was developed for qualitative and quantitative analysis of the major chemical constituents in Andrographis paniculata. Fifteen compounds, including flavonoids and diterpenoid lactones, were unambiguously or tentatively identified in 10 min by comparing their retention times and accurate masses with standards or literature data. The characteristic fragmentation patterns of flavonoids and diterpenoid lactones were summarized, and the structures of the unknown compounds were predicted. Andrographolide, dehydroandrographolide and neoandrographolide were further quantified as marker substances. It was found that the calibration curves for all analytes showed good linearity (R2 > 0.9995 within the test ranges. The overall limits of detection (LODs and limits of quantification (LOQs were 0.02 μg/mL to 0.06 μg/mL and 0.06 μg/mL to 0.2 μg/mL, respectively. The relative standard deviations (RSDs for intra- and inter-day precisions were below 3.3% and 4.2%, respectively. The mean recovery rates ranged from 96.7% to 104.5% with the relative standard deviations (RSDs less than 2.72%. It is concluded that RRLC-TOF/MS is powerful and practical in qualitative and quantitative analysis of complex plant samples due to time savings, sensitivity, precision, accuracy and lowering solvent consumption.

  3. Simple and Rapid Dual-Dispersive Liquid-Liquid Microextraction as an Innovative Extraction Method for Uranium in Real Water Samples Prior to the Determination of Uranium by a Spectrophotometric Technique.

    Science.gov (United States)

    Khan, Naeemullah; Tuzen, Mustafa; Kazi, Tasneem Gul

    2017-11-01

    An innovative, rapid, and simple dual-dispersive liquid-liquid microextraction (DDLL-ME) approach was used to extract uranium from real samples for the first time. The main objective of this study was to disperse extraction solvent by using an air-agitated syringe system to overcome matrix effects and avoid dispersion of hazardous dispersive organic solvents by using heat. The DDLL-ME method consisted of two dispersive liquid-liquid extraction steps with chloroform as the extracting solvent. Uranium formed complexes with 4-(2-thiazolylazo) resorcinol in the aqueous phase and was extracted in extracting solvent (chloroform) after the first dispersive liquid-liquid process. Uranium was then back-extracted in the acidic aqueous phase in a second dispersive liquid-liquid process. Finally, uranium was determined by a spectrophotometric detection technique. The variables that played a key role in the proposed method were studied and optimized. The LOD and sensitivity enhancement factor for uranium were found to be 0.60 µg/L and 45, respectively, under optimized conditions. Calibration graphs were found to be linear in the range of 5.0-600 µg/L. The RSD was 2.5%. Reliability of the proposed method was verified by analyzing certified reference material TM-28.3.

  4. A Procedure for the Rapid Determination of 226Ra and 228Ra in Drinking Water by Liquid Scintillation Counting

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, the environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Reliable, comparable and ‘fit for purpose’ results are essential requirements for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of such data. For maximum utility, such procedures should be comprehensive, clearly formulated and readily available to both the analyst and the customer. This publication describes a procedure for the rapid determination of 226 Ra and 228 Ra in drinking water. The determination of radium in drinking water is important for protecting human health, since the consumption of drinking water containing radium may lead to an accumulation in the body, contributing to the radiological dose. The method is based on the separation of 226 Ra and 228 Ra from interfering elements using PbSO 4 and Ba(Ra)SO 4 coprecipitation steps. The isotopes 226 Ra and 228 Ra are then determined by liquid scintillation counting. The procedure is expected to be of general use to a wide range of laboratories, including the laboratories of the Analytical Laboratories for the Measurement of Environmental Radioactivity (ALMERA) network, both in emergency situations and for routine environmental monitoring purposes. The method was established after an extensive review of papers from the scientific literature, and was tested and validated in terms of repeatability and trueness (relative bias) in accordance with International Organization for Standardization guidelines. Reproducibility tests were performed at expert laboratories. The calculation of massic activities, uncertainty budget, decision threshold and detection limit are also described

  5. Correlations between chromatographic parameters and bioactivity predictors of potential herbicides.

    Science.gov (United States)

    Janicka, Małgorzata

    2014-08-01

    Different liquid chromatography techniques, including reversed-phase liquid chromatography on Purosphere RP-18e, IAM.PC.DD2 and Cosmosil Cholester columns and micellar liqud chromatography with a Purosphere RP-8e column and using buffered sodium dodecyl sulfate-acetonitrile as the mobile phase, were applied to study the lipophilic properties of 15 newly synthesized phenoxyacetic and carbamic acid derivatives, which are potential herbicides. Chromatographic lipophilicity descriptors were used to extrapolate log k parameters (log kw and log km) and log k values. Partitioning lipophilicity descriptors, i.e., log P coefficients in an n-octanol-water system, were computed from the molecular structures of the tested compounds. Bioactivity descriptors, including partition coefficients in a water-plant cuticle system and water-human serum albumin and coefficients for human skin partition and permeation were calculated in silico by ACD/ADME software using the linear solvation energy relationship of Abraham. Principal component analysis was applied to describe similarities between various chromatographic and partitioning lipophilicities. Highly significant, predictive linear relationships were found between chromatographic parameters and bioactivity descriptors. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Chromatographic determination of Terbinafine in presence of its Photodegradation products

    International Nuclear Information System (INIS)

    Abdel-Moety, E.M.; Kelani, K.O.; Abou Al-Alamein, A.M.

    2003-01-01

    Two different chromatographic techniques have been developed for the determination of terbinafine hydrochloride in presence of its photodegradation products. The first method depends on coupling the TLC- fractionation, on silicia gel 60F254 utilizing chloroform+methanol+25% aq. ammonia ( 12: 0.1:0.1,by volumes), with the direct scanning at 284nm. The second method describes a liquid chromatographic separation of terbinafine and its photolytic degradates on a reversed-phase column[u-Bondapak-TMC 18 (10um,25cmx4.6mm,i.d.)] using a mobile phase containing methanol+water= 80:20 (v/v) with UV-detection at 284 nm. The proposed methods showed significant stability-indication with good linearity, precision and reproducibility. (author)

  7. An evaluation of liquid chromatography/mass spectrometry with atmospheric pressure chemical ionization for the rapid and simultaneous measurement of carbamate pesticides and organophorus pesticides

    International Nuclear Information System (INIS)

    Kim, Byung Joo; So, Hun Young

    2000-01-01

    Liquid chromatography/mass spectrometry with an atmospheric pressure chemical ionization interface (LC/APCI/MS) is evaluated for the simultaneous determination of carbamate pesticides and organophosphorus pesticides in a single chromatographic analysis. APCI mass spectra of those compounds were obtained to study their ionization characteristics. APCI provided abundant ions such as protonated molecules and characteristic fragment ions for carbamate pesticides and organophosphorus pesticides. To evaluate the feasibility of the LC/APCI/MS for a routine quantitative analysis, the linearity and repeatability of LC/APCI/MS were examined by measuring standard solution mixtures of five carbamate pesticides and four organophosphorus pesticides over the range of 1 to 100 μg/mL. The peak areas in chromatograms of characteristic ions for those compounds showed less than 3% of variation from run to tun. The standard calibration curves for the nine pesticides show good linearity in the concentration range. The detection limits of the LC/APCI/MS system for those compounds range from 0.006 to 0.2 ng

  8. A rapid and sensitive evaluation of nitrite content in Saudi Arabian processed meat and poultry using a novel ultra performance liquid chromatography-mass spectrometry method.

    Science.gov (United States)

    Siddiqui, Masoom Raza; Wabaidur, Saikh Mohammad; Khan, Moonis Ali; ALOthman, Zeid A; Rafiquee, M Z A; Alqadami, Ayoub Abdullah

    2018-01-01

    Quantitative assessment of nitrite (NO 2 - ) anion was performed using a newly developed high throughput ultra performance liquid chromatography-mass spectrometric (UPLC-MS) method. The nitrite determination with the proposed method using micellar mobile phase was unknown. Selected ion reaction mode using negative electrospray ionization was adopted for the identification and quantitative analysis of nitrite. The chromatographic separation was performed using BEH C-18 column and a micellar mobile phase consisted of sodium dodecyl sulphate and acetonitrile in ratio 30:70 was used. The elution of nitrite anion was accomplished in less than 1 min. Under the optimal analysis conditions, the linearity of the developed method was checked in the concentration range of 0.5-20 mg kg -1 NO 2 - with an excellent correlation coefficient of 0.996. The precisions of the method with relative standard deviation <2% was observed when standard at concentration of 1 mg kg -1 was used. The limit of detection and limit of quantitation of the developed mass spectrometric method was found to be 0.114 and 0.346 mg kg -1 , respectively. The developed UPLC/MS method was applied to quantify this anion in processed meats and poultries from various super market of Saudi Arabia (Riyadh region). The recoveries of the nitrite in the various samples were found in the range of 100.03-103.5%.

  9. An evaluation of liquid chromatography/mass spectrometry with atmospheric pressure chemical ionization for the rapid and simultaneous measurement of carbamate pesticides and organophorus pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Byung Joo; So, Hun Young [Korea Research Institute of Standards and Sceince, Taejon (Korea, Republic of)

    2000-05-01

    Liquid chromatography/mass spectrometry with an atmospheric pressure chemical ionization interface (LC/APCI/MS) is evaluated for the simultaneous determination of carbamate pesticides and organophosphorus pesticides in a single chromatographic analysis. APCI mass spectra of those compounds were obtained to study their ionization characteristics. APCI provided abundant ions such as protonated molecules and characteristic fragment ions for carbamate pesticides and organophosphorus pesticides. To evaluate the feasibility of the LC/APCI/MS for a routine quantitative analysis, the linearity and repeatability of LC/APCI/MS were examined by measuring standard solution mixtures of five carbamate pesticides and four organophosphorus pesticides over the range of 1 to 100 {mu}g/mL. The peak areas in chromatograms of characteristic ions for those compounds showed less than 3% of variation from run to tun. The standard calibration curves for the nine pesticides show good linearity in the concentration range. The detection limits of the LC/APCI/MS system for those compounds range from 0.006 to 0.2 ng.

  10. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  11. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  12. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    International Nuclear Information System (INIS)

    Ying Liu

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  13. Validation and global uncertainty of a liquid chromatographic with diode array detection method for the screening of azoxystrobin, kresoxim-methyl, trifloxystrobin, famoxadone, pyraclostrobin and fenamidone in grapes and wine.

    Science.gov (United States)

    de Melo Abreu, Susana; Caboni, Pierluigi; Cabras, Paolo; Garau, Vincenzo Luigi; Alves, Arminda

    2006-07-28

    Azoxystrobin, kresoxim-methyl, trifloxystrobin, pyraclostrobin, famoxadone and fenamidone are permitted Q(o) Inhibitor (Q(o)I) fungicides applied to vine in some European countries for the treatment of downy and powdery mildews. In this work, a method is validated for the analysis of these fungicides in grapes and wine. This screening method consists in a simple one step liquid-liquid extraction followed by liquid chromatography (LC) fitted with a diode array detector (DAD). Limits of detection for grapes and wine were below 0.2 mg kg(-1) or mg l(-1), precision was not above 13%, and recoveries were, on average, 95+/-5% for grapes and 104+/-6% for wine. Global uncertainties evaluated in the concentration range from 0.25 to 2.50 mg l(-1) were below 20%. A confirmatory method by gas chromatography (GC) with mass spectrometry (MS) detection was used.

  14. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  15. A rapid method for measuring maximum density temperatures in water and aqueous solutions for the study of quantum zero point energy effects in these liquids

    International Nuclear Information System (INIS)

    Deeney, F A; O'Leary, J P

    2008-01-01

    The connection between quantum zero point fluctuations and a density maximum in water and in liquid He 4 has recently been established. Here we present a description of a simple and rapid method of determining the temperatures at which maximum densities in water and aqueous solutions occur. The technique is such as to allow experiments to be carried out in one session of an undergraduate laboratory thereby introducing students to the concept of quantum zero point energy

  16. Quantification of rifampicin in human plasma and cerebrospinal fluid by a highly sensitive and rapid liquid chromatographic–tandem mass spectrometric method

    OpenAIRE

    Srivastava, Abhishek; Waterhouse, David; Ardrey, Alison; Ward, Stephen A.

    2012-01-01

    A highly sensitive and rapid liquid chromatography tandem mass spectrometry (LC–MS/MS) method has been developed to measure the levels of the antitubercular drug rifampicin (RIF) in human plasma and cerebrospinal fluid (CSF). The analyte and internal standard (IS) were isolated from plasma and CSF by a simple organic solvent based precipitation of proteins followed by centrifugation. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monit...

  17. Rapid method for the analysis of itraconazole and hydroxyitraconazole in serum by high-performance liquid chromatography

    NARCIS (Netherlands)

    Compas, D; Touw, D J; de Goede, P N

    1996-01-01

    An assay for the determination of itraconazole and its active metabolite hydroxyitraconazole in serum has been developed, using ketoconazole as internal standard. The procedure involved a one-step liquid-liquid extraction of the drug, its metabolite and the internal standard, followed by their

  18. Rapid determination of benzodiazepines, zolpidem and their metabolites in urine using direct injection liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jeong, Yu-Dong; Kim, Min Kyung; Suh, Sung Ill; In, Moon Kyo; Kim, Jin Young; Paeng, Ki-Jung

    2015-12-01

    Benzodiazepines and zolpidem are generally prescribed as sedative, hypnotics, anxiolytics or anticonvulsants. These drugs, however, are frequently misused in drug-facilitated crime. Therefore, a rapid and simple liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of benzodiazepines, zolpidem and their metabolites in urine using deuterium labeled internal standards (IS). Urine samples (120 μL) mixed with 80 μL of the IS solution were centrifuged. An aliquot (5 μL) of the sample solution was directly injected into the LC-MS/MS system for analysis. The mobile phases consisted of water and acetonitrile containing 2mM ammonium trifluoroacetate and 0.2% acetic acid. The analytical column was a Zorbax SB-C18 (100 mm × 2.1 mm i.d., 3.5 μm, Agilent). The separation and detection of 18 analytes were achieved within 10 min. Calibration curves were linear over the concentration ranges of 0.5-20 ng/mL (zolpidem), 1.0-40 ng/mL (flurazepam and temazepam), 2.5-100 ng/mL (7-aminoclonazepam, 1-hydroxymidazolam, midazolam, flunitrazepam and alprazolam), 5.0-200 ng/mL (zolpidem phenyl-4-carboxylic acid, α-hydroxyalprazolam, oxazepam, nordiazepam, triazolam, diazepam and α-hydroxytriazolam), 10-400 ng/mL (lorazepam and desalkylflurazepam) and 10-100 ng/mL (N-desmethylflunitrazepam) with the coefficients of determination (r(2)) above 0.9971. The dilution integrity of the analytes was examined for supplementation of short linear range. Dilution precision and accuracy were tested using two, four and ten-folds dilutions and they ranged from 3.7 to 14.4% and -12.8 to 12.5%, respectively. The process efficiency for this method was 63.0-104.6%. Intra- and inter-day precisions were less than 11.8% and 9.1%, while intra- and inter-day accuracies were less than -10.0 to 8.2%, respectively. The lower limits of quantification were lower than 10 ng/mL for each analyte. The applicability of the developed method was successfully

  19. Applicability of the direct injection liquid chromatographic tandem mass spectrometric analytical approach to the sub-ngL-1 determination of perfluoro-alkyl acids in waste, surface, ground and drinking water samples.

    Science.gov (United States)

    Ciofi, Lorenzo; Renai, Lapo; Rossini, Daniele; Ancillotti, Claudia; Falai, Alida; Fibbi, Donatella; Bruzzoniti, Maria Concetta; Santana-Rodriguez, José Juan; Orlandini, Serena; Del Bubba, Massimo

    2018-01-01

    The applicability of a direct injection UHPLC-MS/MS method for the analysis of several perfluoroalkyl acids (PFAAs) in a wide range of water matrices was investigated. The method is based on the direct injection of 100µL of centrifuged water sample, without any other sample treatment. Very good method detection limits (0.014-0.44ngL -1 ) and excellent intra and inter-day precision (RSD% values in the range 1.8-4.4% and 2.7-5.7%, respectively) were achieved, with a total analysis time of 20min per sample. A high number of samples - i.e. 8 drinking waters (DW), 12 ground waters (GW), 13 surface waters (SW), 8 influents and 11 effluents of wastewater treatment plants (WWTP IN and WWTP OUT ) were processed and the extent of matrix effect (ME) was calculated, highlighting the strong prevalence of |ME| 50% was occasionally observed only for perfluorooctanesulphonic and perfluorodecanoic acids. Linear discriminant analysis highlighted the great contribution of the sample origin (i.e. DW, GW, SW, WWTP IN and WWTP OUT ) to the ME. Partial least square regression (PLS) and leave-one-out cross-validation were performed in order to interpret and predict the signal suppression or enhancement phenomena as a function of physicochemical parameters of water samples (i.e. conductivity, hardness and chemical oxygen demand) and background chromatographic area. The PLS approach resulted only in an approximate screening, due to the low prediction power of the PLS models. However, for most analytes in most samples, the fitted and cross-validated values were such as to correctly distinguish between | ME | higher than 20% or below this limit. PFAAs in the aforementioned water samples were quantified by means of the standard addition method, highlighting their occurrence mainly in WWTP influents and effluents, at concentrations as high as one hundred of µgL -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Chromatographic Techniques for Rare Earth Elements Analysis

    Science.gov (United States)

    Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

    2017-04-01

    The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

  1. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  2. Chromatographic separation of radioactive noble gases from xenon

    Science.gov (United States)

    Akerib, D. S.; Araújo, H. M.; Bai, X.; Bailey, A. J.; Balajthy, J.; Beltrame, P.; Bernard, E. P.; Bernstein, A.; Biesiadzinski, T. P.; Boulton, E. M.; Bramante, R.; Cahn, S. B.; Carmona-Benitez, M. C.; Chan, C.; Chiller, A. A.; Chiller, C.; Coffey, T.; Currie, A.; Cutter, J. E.; Davison, T. J. R.; Dobi, A.; Dobson, J. E. Y.; Druszkiewicz, E.; Edwards, B. N.; Faham, C. H.; Fiorucci, S.; Gaitskell, R. J.; Gehman, V. M.; Ghag, C.; Gibson, K. R.; Gilchriese, M. G. D.; Hall, C. R.; Hanhardt, M.; Haselschwardt, S. J.; Hertel, S. A.; Hogan, D. P.; Horn, M.; Huang, D. Q.; Ignarra, C. M.; Ihm, M.; Jacobsen, R. G.; Ji, W.; Kamdin, K.; Kazkaz, K.; Khaitan, D.; Knoche, R.; Larsen, N. A.; Lee, C.; Lenardo, B. G.; Lesko, K. T.; Lindote, A.; Lopes, M. I.; Manalaysay, A.; Mannino, R. L.; Marzioni, M. F.; McKinsey, D. N.; Mei, D.-M.; Mock, J.; Moongweluwan, M.; Morad, J. A.; Murphy, A. St. J.; Nehrkorn, C.; Nelson, H. N.; Neves, F.; O'Sullivan, K.; Oliver-Mallory, K. C.; Palladino, K. J.; Pease, E. K.; Pech, K.; Phelps, P.; Reichhart, L.; Rhyne, C.; Shaw, S.; Shutt, T. A.; Silva, C.; Solovov, V. N.; Sorensen, P.; Stephenson, S.; Sumner, T. J.; Szydagis, M.; Taylor, D. J.; Taylor, W.; Tennyson, B. P.; Terman, P. A.; Tiedt, D. R.; To, W. H.; Tripathi, M.; Tvrznikova, L.; Uvarov, S.; Verbus, J. R.; Webb, R. C.; White, J. T.; Whitis, T. J.; Witherell, M. S.; Wolfs, F. L. H.; Yazdani, K.; Young, S. K.; Zhang, C.

    2018-01-01

    The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85Kr and 39Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search experiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

  3. Easy-to-use procedure to optimise a chromatographic method. Application in the determination of bisphenol-A and phenol in toys by means of liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Arce, M M; Sanllorente, S; Ortiz, M C; Sarabia, L A

    2018-01-26

    other chromatographic optimization. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Study of stationary phase stability from a column with chromatographic material for steady state treatment of an effluent and/or waste containing Th-232

    International Nuclear Information System (INIS)

    Felinto, Maria Claudia Franca da Cunha; Martinz, Daniel Ortiz

    1999-01-01

    This work relates the behavior of a new chromatographic material, AMBERCMPO I, that has been studied to remove actinide elements from the High Level Liquid Waste. It gives emphasis to the behavior of chromatographic materials to the extraction of Th 4+ and its performance after some operation cycle. (author)

  5. Development and validation of a high performance liquid chromatographic method for the determination of oxcarbazepine and its main metabolites in human plasma and cerebrospinal fluid and its application to pharmacokinetic study.

    Science.gov (United States)

    Kimiskidis, Vasilios; Spanakis, Marios; Niopas, Ioannis; Kazis, Dimitrios; Gabrieli, Chrysi; Kanaze, Feras Imad; Divanoglou, Daniil

    2007-01-17

    An isocratic reversed-phase HPLC-UV procedure for the determination of oxcarbazepine and its main metabolites 10-hydroxy-10,11-dihydrocarbamazepine and 10,11-dihydroxy-trans-10,11-dihydrocarbamazepine in human plasma and cerebrospinal fluid has been developed and validated. After addition of bromazepam as internal standard, the analytes were isolated from plasma and cerebrospinal fluid by liquid-liquid extraction. Separation was achieved on a X-TERRA C18 column using a mobile phase composed of 20 mM KH(2)PO(4), acetonitrile, and n-octylamine (76:24:0.05, v/v/v) at 40 degrees C and detected at 237 nm. The described assay was validated in terms of linearity, accuracy, precision, recovery and lower limit of quantification according to the FDA validation guidelines. Calibration curves were linear with a coefficient of variation (r) greater than 0.998. Accuracy ranged from 92.3% to 106.0% and precision was between 2.3% and 8.2%. The method has been applied to plasma and cerebrospinal fluid samples obtained from patients treated with oxcarbazepine, both in monotherapy and adjunctive therapy.

  6. Modeling the Rapid Boil-Off of a Cryogenic Liquid When Injected into a Low Pressure Cavity

    Science.gov (United States)

    Lira, Eric

    2016-01-01

    Many launch vehicle cryogenic applications require the modeling of injecting a cryogenic liquid into a low pressure cavity. The difficulty of such analyses lies in accurately predicting the heat transfer coefficient between the cold liquid and a warm wall in a low pressure environment. The heat transfer coefficient and the behavior of the liquid is highly dependent on the mass flow rate into the cavity, the cavity wall temperature and the cavity volume. Testing was performed to correlate the modeling performed using Thermal Desktop and Sinda Fluint Thermal and Fluids Analysis Software. This presentation shall describe a methodology to model the cryogenic process using Sinda Fluint, a description of the cryogenic test set up, a description of the test procedure and how the model was correlated to match the test results.

  7. Determination of biologically active phenols and polyphenols in various objects by chromatographic techniques

    International Nuclear Information System (INIS)

    Kochetova, M V; Semenistaya, E N; Larionov, Oleg G; Revina, A A

    2007-01-01

    Chromatographic techniques for determination of biologically active phenols and polyphenols are considered. Various methods for sample preparation and detection are compared. The advantages of high performance liquid chromatography with spectrophotometric detection for determination of antioxidants are demonstrated. Data on determination of biologically active phenols and polyphenols published in the period from 1995 to 2005 are analysed.

  8. Functional Durability of a Quartz Crystal Microbalance Sensor for the Rapid Detection of Salmonella in Liquids from Poultry Packaging

    National Research Council Canada - National Science Library

    Olsen, Eric

    2000-01-01

    .... A rapid, sensitive (350 +/- 150 cells ml/cm) quartz crystal microbalance biosensor, layered with heat-treated anti-Salmonella-phospholipid monolayers by the Langmuir-Blodgett technique, has been evaluated by immersion testing in chicken exudate...

  9. Simple, rapid, and sensitive liquid chromatography-fluorescence method for the quantification of tranexamic acid in blood

    NARCIS (Netherlands)

    Huertas-Pérez, José Fernando; Heger, Michal; Dekker, Henk; Krabbe, Hans; Lankelma, Jan; Ariese, Freek

    2007-01-01

    Tranexamic acid (TA) is a synthetic antifibrinolytic agent that is being considered as a candidate adjuvant drug for site-specific pharmaco-laser therapy of port wine stains. For drug utility studies, a high-performance liquid chromatography (HPLC)-fluorescence method was developed for the

  10. Modeling Aquatic Toxicity through Chromatographic Systems.

    Science.gov (United States)

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Farré, Sandra; Muñoz-Pascual, Laura; Abraham, Michael H; Fuguet, Elisabet; Rosés, Martí

    2017-08-01

    Environmental risk assessment requires information about the toxicity of the growing number of chemical products coming from different origins that can contaminate water and become toxicants to aquatic species or other living beings via the trophic chain. Direct toxicity measurements using sensitive aquatic species can be carried out but they may become expensive and ethically questionable. Literature refers to the use of chromatographic measurements that correlate to the toxic effect of a compound over a specific aquatic species as an alternative to get toxicity information. In this work, we have studied the similarity in the response of the toxicity to different species and we have selected eight representative aquatic species (including tadpoles, fish, water fleas, protozoan, and bacteria) with known nonspecific toxicity to chemical substances. Next, we have selected four chromatographic systems offering good perspectives for surrogation of the eight selected aquatic systems, and thus prediction of toxicity from the chromatographic measurement. Then toxicity has been correlated to the chromatographic retention factor. Satisfactory correlation results have been obtained to emulate toxicity in five of the selected aquatic species through some of the chromatographic systems. Other aquatic species with similar characteristics to these five representative ones could also be emulated by using the same chromatographic systems. The final aim of this study is to model chemical products toxicity to aquatic species by means of chromatographic systems to reduce in vivo testing.

  11. Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

    Energy Technology Data Exchange (ETDEWEB)

    Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

    1992-09-01

    On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

  12. Simple and rapid determination of 5-nitroimidazoles and metabolites in fish roe samples by salting-out assisted liquid-liquid extraction and UHPLC-MS/MS.

    Science.gov (United States)

    Hernández-Mesa, Maykel; Cruces-Blanco, Carmen; García-Campaña, Ana M

    2018-06-30

    A novel multiresidue method is proposed for the determination of 12 5-nitroimidazoles and their metabolites in fish roe samples using UHPLC-MS/MS. A salting-out assisted liquid-liquid extraction procedure was performed prior to sample analysis. The separation of compounds was accomplished using a C18 Zorbax Eclipse Plus column (50 mm × 2.1 mm, 1.8 µm) at 25 °C and a mobile phase consisting of 0.025% (v/v) aqueous formic acid and pure MeOH at a flow rate of 0.5 mL/min. Parameters involved in ionization and fragmentation were also optimized. The method was characterized in terms of linearity (R 2  ≥ 0.9992), extraction efficiency (≥68.9%), repeatability (RSD ≤ 9.8%), reproducibility (RSD ≤ 13.9%) and trueness (recoveries ≥81.4%). Decision limits (CCα) and detection capabilities (CCβ) were obtained in the ranges 0.1-1.0 and 0.2-1.7 µg/kg, respectively. Copyright © 2018 Elsevier Ltd. All rights reserved.

  13. RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaee

    2015-05-01

    Full Text Available A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA followed by graphite furnace atomic absorption spectrometry (GFAAS. Ammonium pyrrolidine dithiocarbamate (APDC was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

  14. Liquid Phase Separation and the Aging Effect on Mechanical and Electrical Properties of Laser Rapidly Solidified Cu100−xCrx Alloys

    Directory of Open Access Journals (Sweden)

    Song-Hua Si

    2015-11-01

    Full Text Available Duplex structure Cu-Cr alloys are widely used as contact materials. They are generally designed by increasing the Cr content for the hardness improvement, which, however, leads to the unfavorable rapid increase of the electrical resistivity. The solidification behavior of Cu100−xCrx (x = 4.2, 25 and 50 in wt.% alloys prepared by laser rapid solidification is studied here, and their hardness and electrical conductivity after aging are measured. The results show that the Cu-4.2%Cr alloy has the most desirable combination of hardness and conductive properties after aging in comparison with Cu-25%Cr and Cu-50%Cr alloys. Very importantly, a 50% improvement in hardness is achieved with a simultaneous 70% reduction in electrical resistivity. The reason is mainly attributed to the liquid phase separation occurring in the Cu-4.2%Cr alloy, which introduces a large a

  15. Optimisation of pressurised liquid extraction (PLE) for rapid and efficient extraction of superficial and total mineral oil contamination from dry foods.

    Science.gov (United States)

    Moret, Sabrina; Scolaro, Marianna; Barp, Laura; Purcaro, Giorgia; Sander, Maren; Conte, Lanfranco S

    2014-08-15

    Pressurised liquid extraction (PLE) represents a powerful technique which can be conveniently used for rapid extraction of mineral oil saturated (MOSH) and aromatic hydrocarbons (MOAH) from dry foods with a low fat content, such as semolina pasta, rice, and other cereals. Two different PLE methods, one for rapid determination of superficial contamination mainly from the packaging, the other for efficient extraction of total contamination from different sources, have been developed and optimised. The two methods presented good performance characteristics in terms of repeatability (relative standard deviation lower than 5%) and recoveries (higher than 95%). To show their potentiality, the two methods have been applied in combination on semolina pasta and rice packaged in direct contact with recycled cardboard. In the case of semolina pasta it was possible to discriminate between superficial contamination coming from the packaging, and pre-existing contamination (firmly enclosed into the matrix). Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. Rapid Characterization and Identification of Flavonoids in Radix Astragali by Ultra-High-Pressure Liquid Chromatography Coupled with Linear Ion Trap-Orbitrap Mass Spectrometry.

    Science.gov (United States)

    Zhang, Jing; Xu, Xiao-Jie; Xu, Wen; Huang, Juan; Zhu, Da-yuan; Qiu, Xiao-Hui

    2015-07-01

    A simple and effective method was established for separation and characterization of flavonoid constituents in Radix Astragali (RA) by combination of ultra-high-pressure liquid chromatography with LTQ-Orbitrap tandem mass spectrometry (u-HPLC-LTQ-Orbitrap-MS(n)). For three major structural types of flavonoids, the proposed fragmentation pathways and major diagnostic fragment ions of isoflavones, pterocarpans and isoflavans were investigated to trace isoflavonoid derivatives in crude plant extracts. Based on the systematic identification strategy, 48 constituents were rapidly detected and characterized or tentatively identified, many of which were first reported in RA. The u-PHLC-LTQ-Orbitrap MS(n) platform was proved as an effective tool for rapid qualitative analysis of secondary metabolite productions from natural resources. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  17. A rapid monitoring method for inorganic arsenic in rice flour using reversed phase-high performance liquid chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Narukawa, Tomohiro; Chiba, Koichi; Sinaviwat, Savarin; Feldmann, Jörg

    2017-01-06

    A new rapid monitoring method by means of high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) following the heat-assisted extraction was developed for measurement of total inorganic arsenic species in rice flour. As(III) and As(V) eluted at the same retention time and completely separated from organoarsenic species by an isocratic elution program on a reversed phase column. Therefore, neither ambiguous oxidation of arsenite to arsenate nor the integration of two peaks were necessary to determine directly the target analyte inorganic arsenic. Rapid injection allowed measuring 3 replicates within 6min and this combined with a quantitative extraction of all arsenic species from rice flour by a 15min HNO 3 -H 2 O 2 extraction makes this the fastest laboratory based method for inorganic arsenic in rice flour. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Rapid determination of hydrophilic phenols in olive oil by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and screen-printed carbon electrodes.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Canals, Antonio

    2018-05-01

    A novel approach is presented to determine hydrophilic phenols in olive oil samples, employing vortex-assisted reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation and screen-printed carbon electrodes for voltammetric analysis. The oxidation of oleuropein, hydroxytyrosol, caffeic acid, ferulic acid and tyrosol was investigated, being caffeic acid and tyrosol selected for quantification. A matrix-matching calibration using sunflower oil as analyte-free sample diluted with hexane was employed to compensate matrix effects. Samples were analyzed under optimized RP-DLLME conditions, i.e., extractant phase, 1M HCl; extractant volume, 100µL; extraction time, 2min; centrifugation time, 10min; centrifugation speed, 4000rpm. The working range showed a good linearity between 0.075 and 2.5mgL -1 (r = 0.998, N = 7) for caffeic acid, and between 0.075 and 3mgL -1 (r = 0.999, N = 8) for tyrosol. The methodological limit of detection was empirically established at 0.022mgL -1 for both analytes, which is significantly lower than average contents found in olive oil samples. The repeatability was evaluated at two different spiking levels (i.e., 0.5mgL -1 and 2mgL -1 ) and coefficients of variation ranged from 8% to 11% (n = 5). The applicability of the proposed method was tested in olive oil samples of different quality (i.e., refined olive oil, virgin olive oil and extra virgin olive oil). Relative recoveries varied between 83% and 108% showing negligible matrix effects. Finally, fifteen samples were analyzed by the proposed method and a high correlation with the traditional Folin-Ciocalteu spectrophotometric method was obtained. Thereafter, the concentrations of the fifteen oil samples were employed as input variables in linear discriminant analysis in order to distinguish between olive oils of different quality. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Mid-infrared and near-infrared spectroscopy for rapid detection of Gardeniae Fructus by a liquid-liquid extraction process.

    Science.gov (United States)

    Tao, Lingyan; Lin, Zhonglin; Chen, Jiashan; Wu, Yongjiang; Liu, Xuesong

    2017-10-25

    Gardeniae Fructus is widely used in the pharmaceutical industry, and many studies have confirmed its medical and economic value. In this study, samples collected from different liquid-liquid extraction batches of Gardeniae Fructus were detected by mid-infrared (MIR) and near-infrared (NIR) spectroscopy. Seven analytes, neochlorogenic acid (5-CQA), cryptochlorogenic acid (4-CQA), chlorogenic acid (3-CQA), geniposidic acid (GEA), deacetyl-asperulosidic acid methyl ester (DAAME), genipin-gentiobioside (GGB), and gardenoside (GA), were chosen as quality property indexes of Gardeniae Fructus. The two kinds of spectra were each used to build models by single partial least squares (PLS). Additionally, both spectral data were combined and modeled by multiblock PLS. For single spectroscopy modeling results, NIR had a better prediction for high-concentration analytes (3-CQA, DAAME, GGB, and GA) whereas MIR performed better for low-concentration analytes (5-CQA, 4-CQA, and GEA). The multiblock methodology was found to be better compared to single spectroscopy models for all seven analytes. Specifically, the coefficients of determination (R 2 ) of the NIR, MIR, and multiblock PLS calibration models of all seven components were higher than 0.95. Relative standard errors of prediction (RSEP) were all less than 7%, except for models of GGB, which were 10.36%, 13.24%, and 8.15% for the NIR-PLS, MIR-PLS, and multiblock models, respectively. These results indicate that MIR and NIR spectrographic techniques could provide a new choice for quality control in industrial production of Gardeniae Fructus. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Development and validation of a sensitive liquid chromatographic-tandem mass spectrometric method for the simultaneous analysis of granisetron and 7-hydroxy granisetron in human plasma and urine samples: application in a clinical pharmacokinetic study in pregnant subject.

    Science.gov (United States)

    Zhao, Yang; Chen, Hui-Jun; Caritis, Steve; Venkataramanan, Raman

    2016-02-01

    A liquid chromatography-tandem mass spectrometric method for the quantification of granisetron and its major metabolite, 7-hydroxy granisetron in human plasma and urine samples was developed and validated. Respective stable isotopically labeled granisetron and 7-hydroxy granisetron were used as internal standards (IS). Chromatography was performed using an Xselect HSS T3 analytical column with a mobile phase of 20% acetonitrile in water (containing 0.2 mM ammonium formate and 0.14% formic acid, pH 4) delivered in an isocratic mode. Tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring was used for quantification. The standard curves were linear in the concentration ranges of 0.5-100 ng/mL for granisetron and 0.1-100 ng/mL for 7-hydroxy granisetron in human plasma samples, and 2-2000 ng/mL for granisetron and 2-1000 ng/mL for 7-hydroxy granisetron in human urine samples, respectively. The accuracies were >85% and the precision as determined by the coefficient of variations was granisetron or 7-hydroxy granisetron in either plasma or urine samples. Granisetron was stable under various storage and experimental conditions. This validated method was successfully applied to a pharmacokinetic study after intravenous administration of 1 mg granisetron to a pregnant subject. Copyright © 2015 John Wiley & Sons, Ltd.

  1. Evaluation of glycidyl methacrylate-based monolith functionalized with weak anion exchange moiety inside 0.5 mm i.d. column for liquid chromatographic separation of DNA

    Directory of Open Access Journals (Sweden)

    Aprilia Nur Tasfiyati

    2016-03-01

    Full Text Available In this study, the organic polymer monolith was developed as a weak anion exchanger column in high performance liquid chromatography for DNA separation. Methacrylate-based monolithic column was prepared in microbore silicosteel column (100 × 0.5 mm i.d. by in-situ polymerization reaction using glycidyl methacrylate as monomer; ethylene dimethacrylate as crosslinker; 1-propanol, 1,4-butanediol, and water as porogenic solvents, with the presence of initiator α,α′-azobisisobutyronitrile (AIBN. The monolith matrix was modified with diethylamine to create weak anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by SEM. The properties of the monolithic column, such as permeability, mechanical stability, binding capacity and pore size distribution, were characterized in detail. From the results of the characterization, monoliths poly-(GMA-co-EDMA with total monomer percentage (%T 40 and crosslinker percentage (%C 25 was found to be the ideal composition of monomer and crosslinker. It has good mechanical stability and high permeability, adequate molecular recognition sites (represented with binding capacity value of 36 mg ml−1, and has relatively equal proportion of flow-through pore and mesopores (37.2% and 41.1% respectively. Poly-(GMA-co-EDMA with %T 40 and %C 25 can successfully separate oligo(dT12–18 and 50 bp DNA ladder with good resolution.

  2. Chromatographic retention prediction and octanol-water partition coefficient determination of monobasic weak acidic compounds in ion-suppression reversed-phase liquid chromatography using acids as ion-suppressors.

    Science.gov (United States)

    Ming, Xin; Han, Shu-ying; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2009-08-15

    Although simple acids, replacing buffers, have been widely applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography (RPLC), none of the previously reported works focused on the systematic studies about the retention behavior of the acidic solutes in this ion-suppression RPLC mode. The subject of this paper was therefore to investigate the retention behavior of monobasic weak acidic compounds using acetic, perchloric and phosphoric acids as the ion-suppressors. The apparent octanol-water partition coefficient (K" ow) was proposed to calibrate the octanol-water partition coefficient (K(ow)) of these weak acidic compounds, which resulted in a better linear correlation with log k(w), the logarithm of the hypothetical retention factor corresponding to neat aqueous fraction of hydroorganic mobile phase. This log K" ow-log k w linear correlation was successfully validated by the results of monocarboxylic acids and monohydrating phenols, and moreover by the results under diverse experimental conditions for the same solutes. This straightforward relationship not only can be used to effectively predict the retention values of weak acidic solutes combined with Snyder-Soczewinski equation, but also can offer a promising medium for directly measuring K(ow) data of these compounds via Collander equation. In addition, the influence of the different ion-suppressors on the retention of weak acidic compounds was also compared in this RPLC mode.

  3. Cetylpyridinium chloride functionalized silica-coated magnetite microspheres for the solid-phase extraction and pre-concentration of ochratoxin A from environmental water samples with high-performance liquid chromatographic analysis.

    Science.gov (United States)

    Hu, Meihua; Huang, Pengcheng; Suo, Lili; Wu, Fangying

    2017-06-01

    A new method based on cetylpyridinium chloride coated ferroferric oxide/silica magnetic microspheres as an efficient solid-phase adsorbent was developed for the extraction and enrichment of ochratoxin A. The determination of ochratoxin A was obtained by high-performance liquid chromatography with fluorescence detection. In the presence of cetylpyridinium chloride, the adsorption capacity of ferroferric oxide/silica microspheres was 5.95 mg/g for ochratoxin A. The experimental parameters were optimized, including the amounts of ferroferric oxide/silica microspheres (20 mg) and cetylpyridinium chloride (0.18 mL, 0.5 mg/mL), pH value of media (9), ultrasonic time (5 min), elution solvent and volume [2(1 + 1) mL (washed twice, 1 mL each time) 1% acetic acid acetonitrile]. Under optimal experiment conditions, ochratoxin A had good linearity in the range of 2.5-250.0 ng/L in water samples with correlation coefficient of the calibration curve 0.9995. The limit of detection for ochratoxin A was 0.83 ng/L, and the recoveries were 89.8-96.8% with the relative standard deviation of 1.5-3.5% in environmental water samples. Furthermore, ferroferric oxide/silica microspheres show excellent reusability during extraction procedures for no less than six times. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Validation of a reversed-phase high-performance liquid chromatographic method for the determination of free amino acids in rice using l-theanine as the internal standard.

    Science.gov (United States)

    Liyanaarachchi, G V V; Mahanama, K R R; Somasiri, H P P S; Punyasiri, P A N

    2018-02-01

    The study presents the validation results of the method carried out for analysis of free amino acids (FAAs) in rice using l-theanine as the internal standard (IS) with o-phthalaldehyde (OPA) reagent using high-performance liquid chromatography-fluorescence detection. The detection and quantification limits of the method were in the range 2-16μmol/kg and 3-19μmol/kg respectively. The method had a wide working range from 25 to 600μmol/kg for each individual amino acid, and good linearity with regression coefficients greater than 0.999. Precision measured in terms of repeatability and reproducibility, expressed as percentage relative standard deviation (% RSD) was below 9% for all the amino acids analyzed. The recoveries obtained after fortification at three concentration levels were in the range 75-105%. In comparison to l-norvaline, findings revealed that l-theanine is suitable as an IS and the validated method can be used for FAA determination in rice. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Radioactivity monitor for high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Reeve, D.R.; Crozier, A.

    1977-01-01

    The coupling of a homogeneous radioactivity monitor to a liquid chromatograph involves compromises between the sensitivity of the monitor and the resolution and speed of analysis of the chromatograph. The theoretical relationships between these parameters are considered and expressions derived which make it possible to calculate suitable monitor operating conditions for most types of high-performance liquid chromatography

  6. Chromatographic and biological aspects of organomercurials

    Energy Technology Data Exchange (ETDEWEB)

    Fishbein, L

    1970-01-01

    A thorough review on the biological and chromatographic aspects of methylmercury, phenylmercurials, and miscellaneous organomercurials is presented. Areas covered include ecology, epidemiology, paper chromatography, thin-layer chromatography, gas chromatography, metabolism and toxicity, and environmental degradation. 183 references.

  7. A Quantitative Gas Chromatographic Ethanol Determination.

    Science.gov (United States)

    Leary, James J.

    1983-01-01

    Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

  8. Determination of biocides as well as some biocide metabolites from facade run-off waters by solid phase extraction and high performance liquid chromatographic separation and tandem mass spectrometry detection.

    Science.gov (United States)

    Bester, K; Lamani, X

    2010-08-06

    Biocides are used to protect buildings, boats, and other materials from microbial infestations. A huge variety of compounds are being used: isothiazolinones, e.g., to prevent bacterial growth in paints, triazines and phenylureas against algal growth on water exposed materials while carbamates are used against fungal investations. However these biocides can be leached from the respective materials. As these are very effective compounds it is important to know the concentrations of these biocides in the leachates as well as their leaching behaviour to assess their risk to the environment. In this study, a method for the determination of biocides from facade material run-off water by means of high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed. Due to the amphiphilic character and the expected varying pH-values in the samples, the extractions as well as the HPLC-method development proved to be demanding. The water samples (leachates) were buffered with a phosphate buffer to pH 7. As some of the biocides are very hydrophilic, different SPE cartridges were tested to identify the SPE material with the highest recovery rates for all compounds. For gaining a good separation, analyte trapping was performed on the HPLC column. Quantification was performed using a mass spectrometer in multi-reaction monitoring with two transitions per compound. The final recovery rates were conducted using a cartridge with a divenylbenzyl polymer sorbent. A combination of methanol and acetonitrile as eluents was used to reach recovery rates in the range of 70-100%. The limit of quantification for the compounds of interest ranged from 0.01 to 0.1 microg/L. Copyright 2010 Elsevier B.V. All rights reserved.

  9. A 2H nuclear magnetic resonance study of the state of water in neat silica and zwitterionic stationary phases and its influence on the chromatographic retention characteristics in hydrophilic interaction high-performance liquid chromatography.

    Science.gov (United States)

    Wikberg, Erika; Sparrman, Tobias; Viklund, Camilla; Jonsson, Tobias; Irgum, Knut

    2011-09-23

    2H NMR has been used as a tool for probing the state of water in hydrophilic stationary phases for liquid chromatography at temperatures between -80 and +4 °C. The fraction of water that remained unfrozen in four different neat silicas with nominal pore sizes between 60 and 300 Å, and in silicas with polymeric sulfobetaine zwitterionic functionalities prepared in different ways, could be determined by measurements of the line widths and temperature-corrected integrals of the 2H signals. The phase transitions detected during thawing made it possible to estimate the amount of non-freezable water in each phase. A distinct difference was seen between the neat and modified silicas tested. For the neat silicas, the relationship between the freezing point depression and their pore size followed the expected Gibbs-Thomson relationship. The polymeric stationary phases were found to contain considerably higher amounts of non-freezable water compared to the neat silica, which is attributed to the structural effect that the sulfobetaine polymers have on the water layer close to the stationary phase surface. The sulfobetaine stationary phases were used alongside the 100 Å silica to separate a number of polar compounds in hydrophilic interaction (HILIC) mode, and the retention characteristics could be explained in terms of the surface water structure, as well as by the porous properties of the stationary phases. This provides solid evidence supporting a partitioning mechanism, or at least of the existence of an immobilized layer of water into which partitioning could be occurring. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

    International Nuclear Information System (INIS)

    Ghersini, G.; Cerrai, E.

    1978-01-01

    Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

  11. Chromatographic Methods for the Analysis of Polyphenols in Wines

    Directory of Open Access Journals (Sweden)

    Medić-Šarić, M.

    2009-03-01

    Full Text Available Wine is an excellent source of various classes of polyphenols, including phenolic acids, flavonoids, and trihydroxystilbene resveratrol (Fig.1. Polyphenols play a major role in wine quality since they contribute to the sensory characteristics of wine, particularly color and astringency. A recent interest in these substances has been stimulated by abundant evidence of their beneficial effects on human health, such as anticarcinogenic, antiinflamatory and antimicrobial activities. Therefore, numerous studies have been performed in the attempt to analyze polyphenols in wine. This paper reviews the current advances in the determination of polyphenols in wine by the major chromatographic techniques such as thin-layer chromatography (TLC and high-performance liquid chromatography (HPLC.The great complexity of the polyphenolic content of wine and the difficulty in obtaining some of the standards usually require sample preparation before analysis. Two methods for sample preparation, liquid-liquid extraction and solid-phase extraction, are most commonly applied. Hydrolysis is applied frequently, but not exclusively, to remove the sugar moieties from glycosides.TLC on silica gel plates is useful for the rapid and low-cost separation and identification of the polyphenols present in wine (Fig. 2. Densitometric quantitative analysis of polyphenols in wine extracts is usually performed by scanning the TLC plates with UV light at wavelengths of 350–365 nm or 250–260 nm (Fig. 3. For the evaluation of the most efficient mobile phase and an optimal choice of the combination of two or more mobile phases, two methods may be applied: information theory and numerical taxonomy. HPLC currently represents the most popular technique for the analysis of polyphenols in wine. For this purpose, a reversed-phase HPLC method that uses gradient elution with binary elution system is usually employed. Routine detection is based on measurement of UV-Vis absorption with a diode

  12. Rapid quantitative analysis of individual anthocyanin content based on high-performance liquid chromatography with diode array detection with the pH differential method.

    Science.gov (United States)

    Wang, Huayin

    2014-09-01

    A new quantitative technique for the simultaneous quantification of the individual anthocyanins based on the pH differential method and high-performance liquid chromatography with diode array detection is proposed in this paper. The six individual anthocyanins (cyanidin 3-glucoside, cyanidin 3-rutinoside, petunidin 3-glucoside, petunidin 3-rutinoside, and malvidin 3-rutinoside) from mulberry (Morus rubra) and Liriope platyphylla were used for demonstration and validation. The elution of anthocyanins was performed using a C18 column with stepwise gradient elution and individual anthocyanins were identified by high-performance liquid chromatography with tandem mass spectrometry. Based on the pH differential method, the high-performance liquid chromatography peak areas of maximum and reference absorption wavelengths of anthocyanin extracts were conducted to quantify individual anthocyanins. The calibration curves for these anthocyanins were linear within the range of 10-5500 mg/L. The correlation coefficients (r(2)) all exceeded 0.9972, and the limits of detection were in the range of 1-4 mg/L at a signal-to-noise ratio ≥5 for these anthocyanins. The proposed quantitative analysis was reproducible with good accuracy of all individual anthocyanins ranging from 96.3 to 104.2% and relative recoveries were in the range 98.4-103.2%. The proposed technique is performed without anthocyanin standards and is a simple, rapid, accurate, and economical method to determine individual anthocyanin contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Rapid ultrasound-induced transient-liquid-phase bonding of Al-50Si alloys with Zn interlayer in air for electrical packaging application.

    Science.gov (United States)

    Wang, Qian; Chen, Xiaoguang; Zhu, Lin; Yan, Jiuchun; Lai, Zhiwei; Zhao, Pizhi; Bao, Juncheng; Lv, Guicai; You, Chen; Zhou, Xiaoyu; Zhang, Jian; Li, Yuntao

    2017-01-01

    Al-50Si alloys were joined by rapid ultrasound-induced transient-liquid-phase bonding method using Zn foil as interlayer at 390°C in air, below the melt point of interlayer. The fracture of oxide films along the edge of Si particles led to contact and inter-diffusion between aluminum substrate and Zn interlayer, and liquefied Zn-Al alloys were developed. The width of Zn-Al alloys gradually decreased with increasing the ultrasonic vibration time due to liquid squeezing out and accelerated diffusion. A stage of isothermal solidification existed, and the completion time was significantly shortened. In the liquid metal, the acoustic streaming and ultrasonic cavitations were induced. As the process developed, much more Si particles, which were particulate-reinforced phases of Al-50Si, gradually migrated to the center of soldering seam. The highest average shear strength of joints reached to 94.2MPa, and the fracture mainly occurred at the base metal. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Development and application of a validated stability-indicating high-performance liquid chromatographic method using photodiode array detection for simultaneous determination of granisetron, methylparaben, propylparaben, sodium benzoate, and their main degradation products in oral pharmaceutical preparations.

    Science.gov (United States)

    Hewala, Ismail; El-Fatatry, Hamed; Emam, Ehab; Mabrouk, Mokhtar

    2011-01-01

    A simple, rapid, and sensitive RP-HPLC method using photodiode array detection was developed and validated for the simultaneous determination of granisetron hydrochloride, 1-methyl-1H-indazole-3-carboxylic acid (the main degradation product of granisetron), sodium benzoate, methylparaben, propylparaben, and 4-hydroxybenzoic acid (the main degradation product of parabens) in granisetron oral drops and solutions. The separation of the compounds was achieved within 8 min on a SymmetryShield RP18 column (100 x 4.6 mm id, 3.5 microm particle size) using the mobile phase acetonitrile--0.05 M KH2PO4 buffered to pH 3 using H3PO4 (3+7, v/v). The photodiode array detector was used to test the purity of the peaks, and the chromatograms were extracted at 240 nm. The method was validated, and validation acceptance criteria were met in all cases. The robust method was successfully applied to the determination of granisetron and preservatives, as well as their degradation products in different batches of granisetron oral drops and solutions. The method proved to be sensitive for determination down to 0.04% (w/w) of granisetron degradation product relative to granisetron and 0.03% (w/w) 4-hydroxybenzoic acid relative to total parabens.

  15. Comparison of various liquid chromatographic methods involving UV and atmospheric pressure chemical ionization mass spectrometric detection for the efficient trace analysis of phenylurea herbicides in various types of water samples.

    Science.gov (United States)

    van der Heeft, E; Dijkman, E; Baumann, R A; Hogendoorn, E A

    2000-05-19

    The performance of mass spectrometric (MS) detection and UV detection in combination with reversed-phase liquid chromatography without and with the use of coupled column RPLC (LC-LC) has been compared for the trace analysis of phenylurea herbicides in environmental waters. The selected samples of this comparative study originated from an inter-laboratory study. For both detection modes, a 50 mm x 4.6 mm I.D. column and a 100 mm x 4.6 mm I.D. column packed with 3 microm C18 were used as the first (C-1) and second (C-2) column, respectively. Atmospheric pressure chemical ionization mass spectrometry was performed on a magnetic sector instrument. The LC-LC-MS analysis was carried out on-line by means of direct large volume (11.7 ml) injection (LVI). The performance of both on-line (LVI, 4 ml of sample) and off-line LC-LC-UV (244 nm) analysis was investigated. The latter procedure consisted of a solid-phase extraction (SPE) of 250 ml of water sample on a 500 mg C18 cartridge. The comparative study showed that LC-LC-MS is more selective then LC-LC-UV and, in most cases, more sensitive. The LVI-LC-LC-MS approach combines direct quantification and confirmation of most of the analytes down to a level of 0.01 microg/l in water samples in less then 30 min. As regards LC-LC-UV, the off-line method appeared to be a more viable approach in comparison with the on-line procedure. This method allows the screening of phenylurea's in various types of water samples down to a level of at least 0.05 microg/l. On-line analysis with LVI provided marginal sensitivity (limits of detection of about 0.1 microg/l) and selectivity was sometimes less in case of surface water samples. Both the on-line LVI-LC-LC-MS method and the LC-LC-UV method using off-line SPE were validated by analysing a series of real-life reference samples. These samples were part of an inter-laboratory test and contained residues of herbicides ranging from 0.02 to 0.8 microg/l. Beside good correlation between the methods

  16. Two-phase mixture level swell and liquid entrainment/off-take in a vessel during rapid depressurization

    International Nuclear Information System (INIS)

    Kim, Chang Hyun

    2004-02-01

    An experimental study has been performed to analyze the two-phase mixture level swell and the liquid entrainment/off-take through the break in a vessel, which are important phenomena to determine the bleed capacity of the Safety Depressurization System (SDS) of Korea Advanced Power Reactor 1400 (APR1400). Three separate experiments are performed in this study: (a) the depressurization and two-phase mixture level swell experiment: (b) the two-phase mixture level measurement experiment: (c) the liquid entrainment and off-take experiment. A series of experiments has been performed using a scaled pressurized vessel in various depressurization conditions to analyze the two-phase mixture level swell and the liquid entrainment/off-take phenomena from the two-phase mixture surface in the first experiment. The test parameters are the initial pressure (10 - 38.75bars), the initial water level (43.7% - 80.0% of full height), the orifice inner diameter (10mm, 17.5mm, and 20mm). The liquid off-take takes place in certain experimental conditions. The measured parameters in the present experiments are axial void fraction distributions, pressures, temperatures in the test vessel, and the mixture density and mass flowrate through the discharge pipe. An assessment of RELAP5/MOD3 code with the present experimental data has been performed. With appropriate nodalization and time step, RELAP5/MOD3 showed reasonable agreement with the present experimental data for the gradual depressurization without liquid off-take. In the case that the off-take takes place, however, RELAP5/MOD3 under-predicts the amount of liquid entrainment/off-take during depressurization. In the second experiment, an assessment of an ultrasonic sensor and a two-wire type capacitance probe for the two-phase mixture level measurement has been performed under the same experimental conditions to adopt an appropriate measurement method for the two-phase mixture level swell and to investigate pool void fraction by the

  17. [11C]-Flumazenil metabolites: Measurements of unchanged ligand in plasma using thin layer chromatography and rapid liquid chromatography

    International Nuclear Information System (INIS)

    Loc'h, C.; Hantraye, Ph.; Khalili-Varasteh, M.; Maziere, B.; Delforge, J.; Brouillet, E.; Syrota, A.; Maziere, M.

    1990-01-01

    To study in vivo benzodiazepine (BZ) receptors using PET, Flumazenil, an imidazobenzodiazepine with selective antagonistic actions, has been labeled with 11 C on its methyl group. The accurate determination of in vivo binding parameters using biomathematical models requires the knowledge of radioligand metabolism and the measurement of the plasmatic concentration of unchanged radioligand is mandatory. The present report describes and compares rapid and simple analytical procedures to measure unchanged [ 11 C]-Flumazenil in plasma

  18. High-performance liquid chromatography with fluorescence detection for the rapid analysis of pheophytins and pyropheophytins in virgin olive oil.

    Science.gov (United States)

    Li, Xueqi; Woodman, Michael; Wang, Selina C

    2015-08-01

    Pheophytins and pyropheophytin are degradation products of chlorophyll pigments, and their ratios can be used as a sensitive indicator of stress during the manufacturing and storage of olive oil. They increase over time depending on the storage condition and if the oil is exposed to heat treatments during the refining process. The traditional analysis method includes solvent- and time-consuming steps of solid-phase extraction followed by analysis by high-performance liquid chromatography with ultraviolet detection. We developed an improved dilute/fluorescence method where multi-step sample preparation was replaced by a simple isopropanol dilution before the high-performance liquid chromatography injection. A quaternary solvent gradient method was used to include a fourth strong solvent wash on a quaternary gradient pump, which avoided the need to premix any solvents and greatly reduced the oil residues on the column from previous analysis. This new method not only reduces analysis cost and time but shows reliability, repeatability, and improved sensitivity, especially important for low-level samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Rapid and sensitive determination of carbohydrates in foods using high temperature liquid chromatography with evaporative light scattering detection.

    Science.gov (United States)

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2012-04-01

    In the present work, an evaporative light scattering detector was used as a high-temperature liquid chromatography detector for the determination of carbohydrates. The compounds studied were glucose, fructose, galactose, sucrose, maltose, and lactose. The effect of column temperature on the retention times and detectability of these compounds was investigated. Column heating temperatures ranged from 25 to 175°C. The optimum temperature in terms of peak resolution and detectability with pure water as mobile phase and a liquid flow rate of 1 mL/min was 150°C as it allowed the separation of glucose and the three disaccharides here considered in less than 3 min. These conditions were employed for lactose determination in milk samples. Limits of quantification were between 2 and 4.7 mg/L. On the other hand, a temperature gradient was developed for the simultaneous determination of glucose, fructose, and sucrose in orange juices, due to coelution of monosaccharides at temperatures higher than 70°C, being limits of quantifications between 8.5 and 12 mg/L. The proposed hyphenation was successfully applied to different types of milk and different varieties of oranges and mandarins. Recoveries for spiked samples were close to 100% for all the studied analytes. © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Large-Scale Liquid Hydrogen Tank Rapid Chill and Fill Testing for the Advanced Shuttle Upper Stage Concept

    Science.gov (United States)

    Flachbart, R. H.; Hedayat, A.; Holt, K. A.; Sims, J.; Johnson, E. F.; Hastings, L. J.; Lak, T.

    2013-01-01

    Cryogenic upper stages in the Space Shuttle program were prohibited primarily due to a safety risk of a 'return to launch site' abort. An upper stage concept addressed this concern by proposing that the stage be launched empty and filled using shuttle external tank residuals after the atmospheric pressure could no longer sustain an explosion. However, only about 5 minutes was allowed for tank fill. Liquid hydrogen testing was conducted within a near-ambient environment using the multipurpose hydrogen test bed 638.5 ft3 (18m3) cylindrical tank with a spray bar mounted longitudinally inside. Although the tank was filled within 5 minutes, chilldown of the tank structure was incomplete, and excessive tank pressures occurred upon vent valve closure. Elevated tank wall temperatures below the liquid level were clearly characteristic of film boiling. The test results have substantial implications for on-orbit cryogen transfer since the formation of a vapor film would be much less inhibited due to the reduced gravity. However, the heavy tank walls could become an asset in normal gravity testing for on-orbit transfer, i.e., if film boiling in a nonflight weight tank can be inhibited in normal gravity, then analytical modeling anchored with the data could be applied to reduced gravity environments with increased confidence.