Displaying publications 41 - 60 of 151 in total

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  1. Method development for determination of fluroxypyr in water
    Halimah M, Tan YA, Aini K, Ismail BS
    J Environ Sci Health B, 2003 Jul;38(4):429-40.
    PMID: 12856925
    Improved methods for extraction and clean up of fluroxypyr residue in water have been established. Two methods of fluroxypyr extraction were used, namely, Direct Measurement of fluroxypyr and Concentration of fluroxypyr onto A Solid Phase Extraction (SPE) Adsorbent, followed by elution with solvent before determination of fluroxypyr. The recovery for Direct Measurement of fluroxypyr in water containing 8-100 microg L(-1), ranged from 86 to 110% with relative standard deviation of 0.7 to 2.15%. For the second method, three types of SPE were used, viz. C18, C18 end-capped and polyvinyl dibenzene (ISOLUTE ENV+). The procedure involved concentrating the analyte from fluroxypyr-spiked water at pH 3, followed by elution of the analyte with 4 mL of acentonitrile. The recovery of fluroxypyr from the spiked sample at 1 to 50 microg L(-1) after eluting through either C18 or C18 end-capped ranged from 40-64% (with relative standard deviation of 0.7 to 2.15) and 41-65% (with standard deviation of 1.52 to 11.9). The use of ISOLUTE ENV+, gave better results than the C18, C18 end-capped or the Direct Measurement Methods. The recovery and standard deviation of fluroxypyr from spiked water using ISOLUTE ENV+ ranged from 91-102% and 2.5 to 5.3, respectively.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  2. Fulltext Chromatographic analyses of tocopherols and tocotrienols in palm oil
    Han NM, May CY
    J Chromatogr Sci, 2012 Mar;50(3):283-6.
    PMID: 22337806 DOI: 10.1093/chromsci/bms002
    Analyses of tocols (tocopherols and tocotrienols) in palm oil have been extensively reported in the past. However, due to the scarcity of individual tocotrienol standards, calibrations have mostly been carried out using only α-tocopherol as standard. Moreover, even if the individual tocotrienols are being used, their reliability is often questioned, because tocotrienols are highly susceptible to oxidation and deterioration. This paper reports on the study of the deterioration rate of individual tocotrienol standards upon storage as well as different calibration methods for the tocols in palm oil.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  3. A ferulic acid ester of sucrose and other constituents of Bhesa paniculata
    Harrison LJ, Sia GL, Sim KY, Tan HT, Connolly JD, Lavaud C, et al.
    Phytochemistry, 1995 Apr;38(6):1497-500.
    PMID: 7786481
    A novel derivative of sucrose, beta-(3,6-di-O-feruloyl)-fructofuranosyl-alpha-(2,3,4,6-tetra-O-ac etyl)- glucopyranoside, was isolated from the wood of Bhesa paniculata. Its structure was determined by a combination of 2D 1H-1H and 1H-13C correlation NMR spectroscopy. The known compounds, glycerol 1-9',12'-octadecadienoate, beta-sitosterol, (+/-)-pinoresinol, methyl 3,4-dihydroxybenzoate, 4-hydroxy-3-methoxybenzoic acid, anofinic acid and 2-(1'-methylethenyl)-benzofuran-5-carboxylic acid were also isolated.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods
  4. Fulltext Triterpene composition and bioactivities of Centella asiatica
    Hashim P, Sidek H, Helan MH, Sabery A, Palanisamy UD, Ilham M
    Molecules, 2011;16(2):1310-22.
    PMID: 21278681 DOI: 10.3390/molecules16021310
    Leaves of Centella asiatica (Centella) were analysed for their triterpene composition and bioactivity such as collagen enhancement, antioxidant, anticellulite and UV protection capacity properties. Triterpenes of Centella were measured using HPLC-PAD on an Excil ODS 5 mm (C18) column for the simultaneous determination of asiatic acid, madecassic acid, asiaticoside and madecassoside. Centella was found to contain significant amounts of madecassoside (3.10 ± 4.58 mg/mL) and asiaticoside (1.97 ± 2.65 mg/mL), but was low in asiatic and madecassic acid. The highest collagen synthesis was found at 50 mg/mL of Centella extracts. The antioxidant activity of Centella (84%) was compared to grape seed extract (83%) and Vitamin C (88%). Its lipolytic activity was observed by the release of glycerol (115.9 µmol/L) at 0.02% concentration. Centella extracts exhibited similar UV protection effect to OMC at 10% concentration. In view of these results, the potential application of Centella in food and pharmaceutical industries is now widely open.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods
  5. Combination of Cyclodextrin and Ionic Liquid in Analytical Chemistry: Current and Future Perspectives
    Hui BY, Raoov M, Zain NNM, Mohamad S, Osman H
    Crit Rev Anal Chem, 2017 Sep 03;47(5):454-467.
    PMID: 28453309 DOI: 10.1080/10408347.2017.1320936
    The growth in driving force and popularity of cyclodextrin (CDs) and ionic liquids (ILs) as promising materials in the field of analytical chemistry has resulted in an exponentially increase of their exploitation and production in analytical chemistry field. CDs belong to the family of cyclic oligosaccharides composing of α-(1,4) linked glucopyranose subunits and possess a cage-like supramolecular structure. This structure enables chemical reactions to proceed between interacting ions, radical or molecules in the absence of covalent bonds. Conversely, ILs are an ionic fluids comprising of only cation and anion often with immeasurable vapor pressure making them as green or designer solvent. The cooperative effect between CD and IL due to their fascinating properties, have nowadays contributed their footprints for a better development in analytical chemistry nowadays. This comprehensive review serves to give an overview on some of the recent studies and provides an analytical trend for the application of CDs with the combination of ILs that possess beneficial and remarkable effects in analytical chemistry including their use in various sample preparation techniques such as solid phase extraction, magnetic solid phase extraction, cloud point extraction, microextraction, and separation techniques which includes gas chromatography, high-performance liquid chromatography, capillary electrophoresis as well as applications of electrochemical sensors as electrode modifiers with references to recent applications. This review will highlight the nature of interactions and synergic effects between CDs, ILs, and analytes. It is hoped that this review will stimulate further research in analytical chemistry.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods
  6. An RP-HPLC-UV method with SPE for cefotaxime in all-in-one total parenteral nutritional admixtures: application to stability studies
    Iqbal MS, Bahari MB, Darwis Y, Iqbal MZ, Hayat A, Venkatesh G
    J AOAC Int, 2013 6 19;96(2):290-4.
    PMID: 23767352
    A simple and selective RP-HPLC-UV method with SPE was developed and validated for the quantification of cefotaxime in all-in-one total parenteral nutrition (AIO-TPN) admixtures. Chromatographic separation was achieved on a 5 pm particle size C18 DB column (250 x 4.6 mm id) using the mobile phase ammonium acetate (25 mM, pH 4.0)-50% acetonitrile in methanol (80 + 20, v/v). The flow rate was 0.9 mL/min and the detection wavelength was 254 nm. The analyte was extracted from AIO-TPN admixtures by means of an SPE method. The cefotaxime calibration curve was linear over a concentration range of 100-1400 microg/mL with a correlation coefficient of > or = 0.9994. The intraday accuracy and precision for cefotaxime were < or = -3.15 and < or = 3.08%, respectively, whereas the interday accuracy and precision were < or = -2.48 and < or = 2.25%, respectively. The method was successfully applied to stability studies of cefotaxime in the presence of micronutrients together with low and high concentrations of macronutrients in AIO-TPN admixtures. Cefotaxime was degraded by 13.00 and 26.05% at room temperature (25 +/- 2 degrees C) after 72 h in low and high macronutrient concentration formulations of AIO-TPN admixtures, respectively. The values of cefotaxime degradation rates for low and high macronutrient concentration formulations of AIO-TPN admixtures were -0.164 and -0.353, respectively. These results indicated that there was a higher rate of degradation in the AIO-TPN admixture formulations containing high concentrations of macronutrients.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  7. Simple high-performance liquid chromatographic method for determination of pentoxifylline in human plasma
    Jia Woei Wong, Kah Hay Yuen, Kok Khiang Peh
    J Chromatogr B Biomed Sci Appl, 1998 Sep 25;716(1-2):387-91.
    PMID: 9824257
    A simple high-performance liquid chromatographic method using ultraviolet detection was developed for the determination of pentoxifylline in human plasma. Prior to analysis, pentoxifylline and the internal standard (chloramphenicol) were extracted from plasma sample using dichloromethane. The mobile phase comprised 0.02 M phosphoric acid adjusted to pH 4, methanol and tetrahydrofuran (55:45:1, v/v). Analysis was run at a flow-rate of 1.4 ml/min with the detector operated at a wavelength of 273 nm. The method was specific and sensitive with a detection limit of approximately 3.0 ng/ml at a signal to noise ratio of 3:1, while the limit of quantification was 12.5 ng/ml. Mean recovery value of the extraction procedure was about 99.9%, while the within-day and between-day coefficient of variation and percent error values of the assay method were all less than 10.0%. The calibration curve was linear over a concentration range of 12.5-400.0 ng/ml.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  8. Application of Box-Behnken design for ultrasound-assisted extraction and recycling preparative HPLC for isolation of anthraquinones from Cassia singueana
    Jibril S, Basar N, Sirat HM, Wahab RA, Mahat NA, Nahar L, et al.
    Phytochem Anal, 2019 Jan;30(1):101-109.
    PMID: 30288828 DOI: 10.1002/pca.2795
    INTRODUCTION: Cassia singueana Del. (Fabaceae) is a rare medicinal plant used in the traditional medicine preparations to treat various ailments. The root of C. singueana is a rich source of anthraquinones that possess anticancer, antibacterial and antifungal properties.

    OBJECTIVE: The objective of this study was to develop an ultrasound-assisted extraction (UAE) method for achieving a high extraction yield of anthraquinones using the response surface methodology (RSM), Box-Behnken design (BBD), and a recycling preparative high-performance liquid chromatography (HPLC) protocol for isolation of anthraquinones from C. singueana.

    METHODOLOGY: Optimisation of UAE was performed using the Box-Behnken experimental design. Recycling preparative HPLC was employed to isolate anthraquinones from the root extract of C. singueana.

    RESULTS: The BBD was well-described by a quadratic polynomial model (R2  = 0.9751). The predicted optimal UAE conditions for a high extraction yield were obtained at: extraction time 25.00 min, temperature 50°C and solvent-sample ratio of 10 mL/g. Under the predicted conditions, the experimental value (1.65 ± 0.07%) closely agreed to the predicted yield (1.64%). The obtained crude extract of C. singueana root was subsequently purified to afford eight anthraquinones.

    CONCLUSION: The extraction protocol described here is suitable for large-scale extraction of anthraquinones from plant extracts.

    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  9. Determination of plasma concentrations of dapsone, monoacetyl dapsone and pyrimethamine in human subjects dosed with maloprim
    Jones CR, Ovenell SM
    J. Chromatogr., 1979 Jun 11;163(2):179-85.
    PMID: 541369
    A high-performance liquid chromatographic method was developed to enable dapsone, monoacetyl dapsone and pyrimethamine to be measured simultaneously in plasma samples from volunteers in England and Malaysia who had been dosed with Maloprim. Mean half-lives of 25 and 80 h were calculated for dapsone and pyrimethamine, respectively, but there was wide individual variation. All subjects were found to be classifiable as "slow acetylators".
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  10. Simple high-performance liquid chromatographic method for determination of alpha-tocopherol in human plasma
    Julianto T, Yuen KH, Noor AM
    J Chromatogr B Biomed Sci Appl, 1999 Sep 10;732(1):227-31.
    PMID: 10517240
    A simple high-performance liquid chromatographic method using UV detection was developed for the determination of alpha-tocopherol in human plasma. The method entailed direct injection of the plasma sample after deproteinization using acetonitrile-tetrahydrofuran (3:2). The mobile phase comprised methanol-tetrahydrofuran (94:6) and analysis was run at a flow-rate of 1.5 ml/min with the detector operating at 292 nm. A Crestpak C18S (5 microm, 250 mm x 4.6 mm ID) was used for the chromatographic separation. The method had a mean recovery of 93%, while the within-day and between-day coefficients of variation and percentage errors were all less than 7%. The speed, specificity, sensitivity and reproducibility of this method make it particularly suitable for routine determination of alpha-tocopherol in human plasma. Moreover, only a small sample plasma volume (100 microl) is required for the analysis.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  11. Simple high-performance liquid chromatographic method for the determination of metformin in human plasma
    Kah Hay Yuen, Kok Khiang Peh
    J Chromatogr B Biomed Sci Appl, 1998 Jun 12;710(1-2):243-6.
    PMID: 9686895
    A simple high-performance liquid chromatographic method using ultraviolet detection was developed for the determination of metformin in human plasma. The method entailed direct injection of the plasma sample after deproteination using perchloric acid. The mobile phase comprised 0.01 M potassium dihydrogen orthophosphate (pH 3.5) and acetonitrile (60:40, v/v). Analyses were run at a flow-rate of 1.0 ml/min with the detector operating at a detection wavelength of 234 nm. The method is specific and sensitive, with a quantification limit of approximately 60 ng/ml and a detection limit of 15 ng/ml at a signal-to-noise ratio of 3:1. The mean absolute recovery value was about 97%, while the within-day and between-day coefficient of variation and percent error values of the assay method were all less than 8%. The calibration curve was linear over a concentration range of 62.5-4000 ng/ml.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  12. Improvement of COD removal by controlling the substrate degradability during the anaerobic digestion of recalcitrant wastewater
    Kawai M, Nagao N, Kawasaki N, Imai A, Toda T
    J Environ Manage, 2016 Oct 01;181:838-846.
    PMID: 27449962 DOI: 10.1016/j.jenvman.2016.06.057
    The recalcitrant landfill leachate was anaerobically digested at various mixing ratios with labile synthetic wastewater to evaluate the degradation properties of recalcitrant wastewater. The proportion of leachate to the digestion system was increased in three equal steps, starting from 0% to 100%, and later decreased back to 0% with the same steps. The chemical oxygen demand (COD) for organic carbon and other components were calculated by analyzing the COD and dissolved organic carbon (DOC), and the removal efficiencies of COD carbon and COD others were evaluated separately. The degradation properties of COD carbon and COD others shifted owing to changing of substrate degradability, and the removal efficiencies of COD carbon and COD others were improved after supplying 100% recalcitrant wastewater. The UV absorptive property and total organic carbon (TOC) of each molecular size using high performance liquid chromatography (HPLC)-size exclusion chromatography (SEC) with UVA and TOC detectors were also investigated, and the degradability of different molecular sizes was determined. Although the SEC system detected extracellular polymeric substances (EPS), which are produced by microbes in stressful environments, during early stages of the experiment, EPS were not detected after feeding 100% recalcitrant wastewater. These results suggest that the microbes had acclimatized to the recalcitrant wastewater degradation. The high removal rates of both COD carbon and COD others were sustained when the proportion of labile wastewater in the substrate was 33%, indicating that the effective removal of recalcitrant COD might be controlled by changing the substrate's degradability.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods
  13. Micro-solid phase extraction with liquid chromatography-tandem mass spectrometry for the determination of aflatoxins in coffee and malt beverage
    Khayoon WS, Saad B, Salleh B, Manaf NH, Latiff AA
    Food Chem, 2014 Mar 15;147:287-94.
    PMID: 24206720 DOI: 10.1016/j.foodchem.2013.09.049
    A single step extraction-cleanup procedure using porous membrane-protected micro-solid phase extraction (μ-SPE) in conjunction with liquid chromatography-tandem mass spectrometry for the extraction and determination of aflatoxins (AFs) B1, B2, G1 and G2 from food was successfully developed. After the extraction, AFs were desorbed from the μ-SPE device by ultrasonication using acetonitrile. The optimum extraction conditions were: sorbent material, C8; sorbent mass, 20mg; extraction time, 90 min; stirring speed, 1,000 rpm; sample volume, 10 mL; desorption solvent, acetonitrile; solvent volume, 350 μL and ultrasonication period, 25 min without salt addition. Under the optimum conditions, enrichment factor of 11, 9, 9 and 10 for AFG2, AFG1, AFB2 and AFB1, respectively were achieved. Good linearity and correlation coefficient was obtained over the concentration range of 0.4-50 ng g(-1) (r(2) 0.9988-0.9999). Good recoveries for AFs ranging from 86.0-109% were obtained. The method was applied to 40 samples involving malt beverage (19) and canned coffee (21). No AFs were detected in the selected samples.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  14. High performance liquid chromatographic determination of aflatoxins in chilli, peanut and rice using silica based monolithic column
    Khayoon WS, Saad B, Lee TP, Salleh B
    Food Chem, 2012 Jul 15;133(2):489-96.
    PMID: 25683424 DOI: 10.1016/j.foodchem.2012.01.010
    A simple and rapid high performance liquid chromatographic with fluorescence detection method for the determination of the aflatoxin B1, B2, G1 and G2 in peanuts, rice and chilli was developed. The sample was extracted using acetonitrile:water (90:10, v/v%) and then purified by using ISOLUTE® multimode solid phase extraction. After the pre-column derivatisation, the analytes were separated within 3.7 min using Chromolith® performance RP-18e (100-4.6mm) monolithic column. To assess the possible effects of endogenous components in the food items, matrix-matched calibration was used for the quantification and validation. The recoveries of aflatoxins that were spiked into food samples were 86.38-104.5% and RSDs were <4.4%. The method was applied to the determination of aflatoxins in peanut (9), rice (5) and chilli (10) samples. Liquid chromatography-tandem mass spectrometry analysis using triple quadruple analyser and operated in the multiple reaction monitoring modes on the contaminated samples was performed for confirmation.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  15. A reversed phase high performance liquid chromatography method for the determination of fumonisins B1 and B2 in food and feed using monolithic column and positive confirmation by liquid chromatography/tandem mass spectrometry
    Khayoon WS, Saad B, Salleh B, Ismail NA, Abdul Manaf NH, Abdul Latiff A
    Anal Chim Acta, 2010 Oct 29;679(1-2):91-7.
    PMID: 20951862 DOI: 10.1016/j.aca.2010.09.008
    The development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B(1) and fumonisin B(2) by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C(18) solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith(®) RP-18e column (100 mm × 4.6 mm) at 30 °C and eluted with a mobile phase of a mixture of methanol and phosphate buffer pH 3.35 (78:22, v/v) at a flow rate of 1.0 mL min(-1). The fumonisins separation was achieved in about 4 min, compared to approximately 20 min by using a C(18) particle-packed column. The fluorescence excitation and emission were at 335 nm and 440 nm, respectively. The limits of detections were 0.01-0.04 μg g(-1) fumonisin B(1) and fumonisin B(2), respectively. Good recoveries were found for spiked samples (0.1, 0.5, 1.5 μg g(-1) fumonisins B(1) and B(2)), ranging from 84.0 to 106.0% for fumonisin B(1) and from 81.0 to 103.0% for fumonisin B(2). Fifty-three samples were analyzed including 39 food and feeds and 14 inoculated corn and rice. Results show that 12.8% of the food and feed samples were contaminated with fumonisin B(1) (range, 0.01-0.51 μg g(-1)) and fumonisin B(2) (0.05 μg g(-1)). The total fumonisins in these samples however, do not exceed the legal limits established by the European Union of 0.8 μg g(-1). Of the 14 inoculated samples, 57.1% contained fumonisin B(1) (0.16-41.0 μg g(-1)) and fumonisin B(2) (range, 0.22-50.0 μg g(-1)). Positive confirmation of selected samples was carried out using liquid chromatography-tandem mass spectrometry, using triple quadrupole analyzer and operated in the multiple reaction monitoring mode.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods
  16. Carotenoid content of underutilized tropical fruits
    Khoo HE, Ismail A, Mohd-Esa N, Idris S
    Plant Foods Hum Nutr, 2008 Dec;63(4):170-5.
    PMID: 18810641 DOI: 10.1007/s11130-008-0090-z
    This study was conducted to evaluate the total carotene content (TCC) and beta carotene (BC) in the selected underutilized tropical fruits. TCC of underutilized fruits estimated by spectrophotometric method was in the range of 1.4-19.8 mg/100 g edible portion. The TCC of these fruits decreased in the order: Jentik-jentik > Durian Nyekak 2 > Durian Nyekak 1 > Cerapu 2 > Cerapu 1 > Tampoi Kuning > Bacang 1 > Kuini > Jambu Mawar > Bacang 2 > Durian Daun > Bacang 3 > Tampoi Putih > Jambu Susu. BC contents estimated by HPLC method were highest in Jentik-jentik, followed by Cerapu 2, Durian Nyekak 2, Tampoi Kuning, Durian Nyekak 1, and Cerapu 1, which had a range of 68-92% of BC in TCC. These underutilized fruits have an acceptable amount of carotenoids that are potential antioxidant fruits.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  17. Profiling of colour pigments of chili powders of different origin by high-performance liquid chromatography
    Kósa A, Cserháti T, Forgács E, Morais H, Mota T, Ramos AC
    J Chromatogr A, 2001 Apr 27;915(1-2):149-54.
    PMID: 11358243
    The colour pigments of five chili powders of different origins were separated and quantified by reversed-phase high-performance liquid chromatography (RP-HPLC). The similarities and dissimilarities of pigment composition of chili powders were elucidated by principal component analysis (PCA). RP-HPLC separated 50-100 pigment fractions depending on the detection wavelength and on the origin of chili powder. It was found that the pigment composition of chili powders from Malaysia and China and from India and Pakistan show marked similarities while the composition of colour pigments of chili powder from Thailand was different. It was further established that the chromatograms are similar in the first 5-35 min of development, they are highly different between 35 and 75 min and moderately different at the end of the chromatograms. It was concluded that RP-HPLC followed by PCA can be successfully used for the identification of chili powders according to the composition of their colour pigments.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  18. Validation of high performance liquid chromatography-electrochemical detection methods with simultaneous extraction procedure for the determination of artesunate, dihydroartemisinin, amodiaquine and desethylamodiaquine in human plasma for application in clinical pharmacological studies of artesunate-amodiaquine drug combination
    Lai CS, Nair NK, Muniandy A, Mansor SM, Olliaro PL, Navaratnam V
    J Chromatogr B Analyt Technol Biomed Life Sci, 2009 Feb 15;877(5-6):558-62.
    PMID: 19147417 DOI: 10.1016/j.jchromb.2008.12.037
    With the expanded use of the combination of artesunate (AS) and amodiaquine (AQ) for the treatment of falciparum malaria and the abundance of products on the market, comes the need for rapid and reliable bioanalytical methods for the determination of the parent compounds and their metabolites. While the existing methods were developed for the determination of either AS or AQ in biological fluids, the current validated method allows simultaneous extraction and determination of AS and AQ in human plasma. Extraction is carried out on Supelclean LC-18 extraction cartridges where AS, its metabolite dihydroartemisinin (DHA) and the internal standard artemisinin (QHS) are separated from AQ, its metabolite desethylamodiaquine (DeAQ) and the internal standard, an isobutyl analogue of desethylamodiaquine (IB-DeAQ). AS, DHA and QHS are then analysed using Hypersil C4 column with acetonitrile-acetic acid (0.05M adjusted to pH 5.2 with 1.00M NaOH) (42:58, v/v) as mobile phase at flow rate 1.50ml/min. The analytes are detected with an electrochemical detector operating in the reductive mode. Chromatography of AQ, DeAQ and IB-DeAQ is carried out on an Inertsil C4 column with acetonitrile-KH(2)PO(4) (pH 4.0, 0.05M) (11:89, v/v) as mobile phase at flow rate 1.00ml/min. The analytes are detected by an electrochemical detector operating in the oxidative mode. The recoveries of AS, DHA, AQ and DeAQ vary between 79.1% and 104.0% over the concentration range of 50-1400ng/ml plasma. The accuracies of the determination of all the analytes are 96.8-103.9%, while the variation for within-day and day-to-day analysis are <15%. The lower limit of quantification for all the analytes is 20ng/ml and limit of detection is 8ng/ml. The method is sensitive, selective, accurate, reproducible and suited particularly for pharmacokinetic study of AS-AQ drug combination and can also be used to compare the bioavailability of different formulations, including a fixed-dose AS-AQ co-formulation.
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  19. Zeolite Linde Type L as micro-solid phase extraction sorbent for the high performance liquid chromatography determination of ochratoxin A in coffee and cereal
    Lee TP, Saad B, Ng EP, Salleh B
    J Chromatogr A, 2012 May 11;1237:46-54.
    PMID: 22444432 DOI: 10.1016/j.chroma.2012.03.031
    Zeolite Linde Type L (LTL) crystals with different length, diameter and particle size (nanosized LTL, rod LTL, cylinder LTL and needle LTL) were synthesized, characterized and were used as sorbent in the micro-solid phase extraction of ochratoxin A (OTA) before the high performance liquid chromatography detection. Under the optimized conditions, the detection limits of OTA for coffee and cereal were 0.09 ng g(-1) and 0.03 ng g(-1), respectively, while the quantification limits were 0.28 ng g(-1) and 0.08 ng g(-1), respectively. The recoveries of OTA of coffee and cereal spiked at 0.5, 10 and 25 ng g(-1) ranged from 91.7 to 101.0%. The proposed method was applied to forty-five samples of coffee and cereal. The presence of OTA was found in twenty-five samples, ranging from 0.28 to 9.33 ng g(-1).
    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
  20. Porous graphitic carbon shows promise for the rapid screening partial DPD deficiency in lymphocyte dihydropyrimidine dehydrogenase in Chinese, Indian and Malay in Singapore by using semi-automated HPLC-radioassay
    Liem LK, Choong LH, Woo KT
    Clin Biochem, 2002 May;35(3):181-7.
    PMID: 12074825
    OBJECTIVE: Dihydropyrimidine dehydrogenase (DPD) catalyzes the degradation of thymine, uracil, and the chemotherapeutic drug 5-Fluorouracil. In general reverse-phase high pressure liquid chromatography is the standard method for separating 5-[2-(14)C]Fluorouracil and 5-[2-(14)C]Fluoro-5,6-dihydrouracil. However, the use of 100% aqueous solution (as HPLC mobile phase) may collapse the C-18 bonded phase and result in a retention time shift. The aim of this study is to develop a rapid, reproducible, sensitive method for screening partial DPD deficiency in healthy volunteers.

    DESIGN AND METHODS: The activity of DPD was measured using 5-[2- (14)C]Fluorouracil (5-[2-(14)C]FUra) followed by separation of substrate and product 5-[2-(14)C]FUraH(2) with a 15 x 4.6 mm I.D., 5 microm particle size (d(p)) porous graphitic carbon (PGC) column (Hypercarb(R)) and HPLC with online detection of the radioactivity. This was standardized using the protein concentration of the cytosol (NanoOrange(R) Protein Quantitation).

    RESULTS: Complete baseline separation of 5-[2-(14)C]Fluorouracil (5-[2-(14)C]FUra) and 5-[2-(14)C]Fluoro-5,6-dihydrouracil (5-[2-(14)C]FUraH(2)) was achieved using a porous graphitic carbon (PGC) column. The detection limit for 5-[2-(14)C]FUraH(2) was 0.4 pmol.

    CONCLUSIONS: By using linear gradient separation (0.1% Trifluoroacetic acid [TFA] in water to 100% Methanol) protocols in concert with PGC columns (Hypercarb(R)), we have demonstrated that a PGC column has a distinct advantage over C-18 reverse phase columns in terms of column stability (pH 1-14). This method provides an improvement on the specific assay for DPD enzyme activity. It is rapid, reproducible and sensitive and can be used for routine screening for healthy and cancer patients for partial and profound DPD deficiency before treatment with 5- FUra.

    Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
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