建立了在线固相萃取-液相色谱法测定水中3种微囊藻毒素的方法。采用Acclaim PA Cartridge在线固相萃取小柱（10mm×4．3mm，5μm），以KH2P04缓冲溶液-甲醇为富集流动相，进样体积为10mL。以KH2PO4缓冲溶液-乙腈为洗脱流动相，采用...建立了在线固相萃取-液相色谱法测定水中3种微囊藻毒素的方法。采用Acclaim PA Cartridge在线固相萃取小柱（10mm×4．3mm，5μm），以KH2P04缓冲溶液-甲醇为富集流动相，进样体积为10mL。以KH2PO4缓冲溶液-乙腈为洗脱流动相，采用二极管阵列检测器进行检测，检测波长为238nm。微囊藻毒素MC-LR，MC-RR在0．1～10．0μg／L范围内线性关系良好，MC-YR线性范围则为0．1-5．0μg／L，相关系数，不小于0．998，3种微囊藻毒素MC0尺，MC-RR，MC-YR的检出限均为0．1μg／L（S／N=3），水源水加标回收率为96．9％-105.4％，测定结果的相对标准偏差为3．55％-6．46％（n=12）。该方法适用于水源水及饮用水中3种微囊藻毒素的快速测定。展开更多
A quantitative method for clopidogrel using online-SPE tandem LC–MS/MS was developed and fully validated according to the well-established FDA guidelines.The method achieves adequate sensitivity for pharmacokinetic s...A quantitative method for clopidogrel using online-SPE tandem LC–MS/MS was developed and fully validated according to the well-established FDA guidelines.The method achieves adequate sensitivity for pharmacokinetic studies,with lower limit of quantifications(LLOQs)as low as 10 pg/m L.Chromatographic separations were performed on reversed phase columns Kromasil Eternity-2.5-C18-UHPLC for both methods.Positive electrospray ionization in multiple reaction monitoring(MRM)mode was employed for signal detection and a deuterated analogue(clopidogrel-d_4)was used as internal standard(IS).Adjustments in sample preparation,including introduction of an online-SPE system proved to be the most effective method to solve the analyte back-conversion in clinical samples.Pooled clinical samples(two levels)were prepared and successfully used as real-sample quality control(QC)in the validation of back-conversion testing under different conditions.The result showed that the real samples were stable in room temperature for 24 h.Linearity,precision,extraction recovery,matrix effect on spiked QC samples and stability tests on both spiked QCs and real sample QCs stored in different conditions met the acceptance criteria.This online-SPE method was successfully applied to a bioequivalence study of75 mg single dose clopidogrel tablets in 48 healthy male subjects.展开更多
文摘建立了在线固相萃取-液相色谱法测定水中3种微囊藻毒素的方法。采用Acclaim PA Cartridge在线固相萃取小柱（10mm×4．3mm，5μm），以KH2P04缓冲溶液-甲醇为富集流动相，进样体积为10mL。以KH2PO4缓冲溶液-乙腈为洗脱流动相，采用二极管阵列检测器进行检测，检测波长为238nm。微囊藻毒素MC-LR，MC-RR在0．1～10．0μg／L范围内线性关系良好，MC-YR线性范围则为0．1-5．0μg／L，相关系数，不小于0．998，3种微囊藻毒素MC0尺，MC-RR，MC-YR的检出限均为0．1μg／L（S／N=3），水源水加标回收率为96．9％-105.4％，测定结果的相对标准偏差为3．55％-6．46％（n=12）。该方法适用于水源水及饮用水中3种微囊藻毒素的快速测定。
文摘A quantitative method for clopidogrel using online-SPE tandem LC–MS/MS was developed and fully validated according to the well-established FDA guidelines.The method achieves adequate sensitivity for pharmacokinetic studies,with lower limit of quantifications(LLOQs)as low as 10 pg/m L.Chromatographic separations were performed on reversed phase columns Kromasil Eternity-2.5-C18-UHPLC for both methods.Positive electrospray ionization in multiple reaction monitoring(MRM)mode was employed for signal detection and a deuterated analogue(clopidogrel-d_4)was used as internal standard(IS).Adjustments in sample preparation,including introduction of an online-SPE system proved to be the most effective method to solve the analyte back-conversion in clinical samples.Pooled clinical samples(two levels)were prepared and successfully used as real-sample quality control(QC)in the validation of back-conversion testing under different conditions.The result showed that the real samples were stable in room temperature for 24 h.Linearity,precision,extraction recovery,matrix effect on spiked QC samples and stability tests on both spiked QCs and real sample QCs stored in different conditions met the acceptance criteria.This online-SPE method was successfully applied to a bioequivalence study of75 mg single dose clopidogrel tablets in 48 healthy male subjects.
