An improved high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) method has been developed for sensitive and rapid determination of albendazole(ABZ) and its active metabolite,albendazole sulfo...An improved high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) method has been developed for sensitive and rapid determination of albendazole(ABZ) and its active metabolite,albendazole sulfoxide(ABZSO),in the positive ionization mode.The method utilized solid phase extraction(SPE) for sample preparation of the analytes and their deuterated internal standards(ISs) from100 μL human plasma.The chromatography was carried out on Hypurity C_(18) column using acetonitrile-2.0 mM ammonium acetate,pH 5.0(80:20,v/v) as the mobile phase.The assay exhibited a linear response over the concentration range of 0.200-50.0 ng/mL for ABZ and 3.00-600 ng/mL for ABZSO.The recoveries of the analytes and ISs ranged from 86.03%-89.66%and 89.85%-98.94%,respectively.Matrix effect,expressed as IS-normalized matrix factors,ranged from 0.985 to 1.042 for the both analytes.The method was successfully applied for two separate studies in healthy subjects using single dose of 400 mg conventional tablets and 400 mg chewable ABZ tablets,respectively.展开更多
A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy al...A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy alverine(PHA), in human plasma. For sample preparation, solid phase extraction of analytes was performed on Phenomenex Strata-X cartridges using alverine-d5 as the internal standard. The analytes were separated on Symmetry Shield RP18(150 mm×3.9 mm, 5 μm) column with a mobile phase consisting of acetonitrile and10 mM ammonium formate(65:35, v/v). Detection and quantitation was done by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring. The assay method was fully validated over the concentration range of 15.0–15,000 pg/mL for ALV and 30.0–15,000 pg/mL for PHA. The intra-day and inter-day accuracy and precision(% CV) ranged from 94.00% to 96.00% and 0.48% to 4.15% for both the analytes. The mean recovery obtained for ALV and PHA was 80.59% and 81.26%, respectively. Matrix effect,expressed as IS-normalized matrix factor ranged from 0.982 to 1.009 for both the analytes. The application of the method was demonstrated for the specific analysis of ALV and PHA for a bioequivalence study in 52 healthy subjects using 120 mg ALV capsules. The assay reproducibility was also verified by reanalysis of 175 incurred subject samples.展开更多
基金support and necessary facilities provided by Accutest Research Lab,Ahmedabad,to carry out this work
文摘An improved high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) method has been developed for sensitive and rapid determination of albendazole(ABZ) and its active metabolite,albendazole sulfoxide(ABZSO),in the positive ionization mode.The method utilized solid phase extraction(SPE) for sample preparation of the analytes and their deuterated internal standards(ISs) from100 μL human plasma.The chromatography was carried out on Hypurity C_(18) column using acetonitrile-2.0 mM ammonium acetate,pH 5.0(80:20,v/v) as the mobile phase.The assay exhibited a linear response over the concentration range of 0.200-50.0 ng/mL for ABZ and 3.00-600 ng/mL for ABZSO.The recoveries of the analytes and ISs ranged from 86.03%-89.66%and 89.85%-98.94%,respectively.Matrix effect,expressed as IS-normalized matrix factors,ranged from 0.985 to 1.042 for the both analytes.The method was successfully applied for two separate studies in healthy subjects using single dose of 400 mg conventional tablets and 400 mg chewable ABZ tablets,respectively.
基金the support and necessary facilities provided by Accutest Research Lab,Ahmedabad
文摘A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine(ALV) and its active metabolite, para hydroxy alverine(PHA), in human plasma. For sample preparation, solid phase extraction of analytes was performed on Phenomenex Strata-X cartridges using alverine-d5 as the internal standard. The analytes were separated on Symmetry Shield RP18(150 mm×3.9 mm, 5 μm) column with a mobile phase consisting of acetonitrile and10 mM ammonium formate(65:35, v/v). Detection and quantitation was done by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring. The assay method was fully validated over the concentration range of 15.0–15,000 pg/mL for ALV and 30.0–15,000 pg/mL for PHA. The intra-day and inter-day accuracy and precision(% CV) ranged from 94.00% to 96.00% and 0.48% to 4.15% for both the analytes. The mean recovery obtained for ALV and PHA was 80.59% and 81.26%, respectively. Matrix effect,expressed as IS-normalized matrix factor ranged from 0.982 to 1.009 for both the analytes. The application of the method was demonstrated for the specific analysis of ALV and PHA for a bioequivalence study in 52 healthy subjects using 120 mg ALV capsules. The assay reproducibility was also verified by reanalysis of 175 incurred subject samples.