A liquid chsomatographic-tandem mass spectrometric method was used to simultaneously determine four tobacco-specific nitrosamines in cigarette mainstream smoke.Cigarette smoke particulate,obtained under standardized m...A liquid chsomatographic-tandem mass spectrometric method was used to simultaneously determine four tobacco-specific nitrosamines in cigarette mainstream smoke.Cigarette smoke particulate,obtained under standardized machine smoking,was collected on a Cambridge filter pad.The particulate was co-extracted with citric acid-phosphate buffer and cyclohexane and further purified by solid-phase extraction.Analyte identification and quantification were performed using multiple reaction monitoring with one precursor ion and two product ions as identifiers and electrospray ionization in positive mode.The limits of detection were in the range of 0.05～0.24ng/mL using an injection volume of 20μL,linear range over 2.5～1000ng/mL,linear correlation coefficients above 0.998,and recoveries 90.2%～95.1%.展开更多
目的:建立LC/MS/MS法测定人血浆中非那雄胺的浓度,并研究其在中国男性健康人体内的药代动力学。方法:采用LC/MS/MS(APCI源)测定非那雄胺的血浆浓度,并计算其药代动力学参数。结果:非那雄胺线性范围为0.2～50.0μg·L^(-1),定量下限...目的:建立LC/MS/MS法测定人血浆中非那雄胺的浓度,并研究其在中国男性健康人体内的药代动力学。方法:采用LC/MS/MS(APCI源)测定非那雄胺的血浆浓度,并计算其药代动力学参数。结果:非那雄胺线性范围为0.2～50.0μg·L^(-1),定量下限为0.2μg·L^(-1)。日内、日间精密度(RSD)均小于10%,准确度(PE)在±3％内。应用本法测得18名中国男性健康志愿者口服5mg非那雄胺片后主要药代动力学参数为:t_(1/2ke)为5.57±1.60h,K_e为0.12±0.06H^(-1),t_(max)为2.31±0.82h,C_(max)为4O.31±10.89μg L^(-1);AUC_(0-t)和AUC(0-∞)分别为267.9±75.0μg h L^(-1)和286.6±88.6μghL^(-1)。结论:该法操作简便、快速、灵敏,可用于测定血浆中非那雄胺浓度。展开更多
To study Saikosaponins in a Chinese traditional compound medicine by LC/MS. Saikosaponin A and D, which were the bioactive components of Bupleurum falcatum L., were not found in the medicine. And three isomeric compou...To study Saikosaponins in a Chinese traditional compound medicine by LC/MS. Saikosaponin A and D, which were the bioactive components of Bupleurum falcatum L., were not found in the medicine. And three isomeric compounds of Saikosaponin A and D were detected instead. Saikosaponin A and D were found have turned into two other isomers after treated by acid water, but keep unchanged when treated by neutral water. Two of the isomeric compounds which found in the Compound medicine were determined as Saikosaponin B1 and B2 . This work is helpful for quality control of the medicine and also is useful for supervising the procedures of manufacture.展开更多
文摘A liquid chsomatographic-tandem mass spectrometric method was used to simultaneously determine four tobacco-specific nitrosamines in cigarette mainstream smoke.Cigarette smoke particulate,obtained under standardized machine smoking,was collected on a Cambridge filter pad.The particulate was co-extracted with citric acid-phosphate buffer and cyclohexane and further purified by solid-phase extraction.Analyte identification and quantification were performed using multiple reaction monitoring with one precursor ion and two product ions as identifiers and electrospray ionization in positive mode.The limits of detection were in the range of 0.05～0.24ng/mL using an injection volume of 20μL,linear range over 2.5～1000ng/mL,linear correlation coefficients above 0.998,and recoveries 90.2%～95.1%.
文摘目的:建立LC/MS/MS法测定人血浆中非那雄胺的浓度,并研究其在中国男性健康人体内的药代动力学。方法:采用LC/MS/MS(APCI源)测定非那雄胺的血浆浓度,并计算其药代动力学参数。结果:非那雄胺线性范围为0.2～50.0μg·L^(-1),定量下限为0.2μg·L^(-1)。日内、日间精密度(RSD)均小于10%,准确度(PE)在±3％内。应用本法测得18名中国男性健康志愿者口服5mg非那雄胺片后主要药代动力学参数为:t_(1/2ke)为5.57±1.60h,K_e为0.12±0.06H^(-1),t_(max)为2.31±0.82h,C_(max)为4O.31±10.89μg L^(-1);AUC_(0-t)和AUC(0-∞)分别为267.9±75.0μg h L^(-1)和286.6±88.6μghL^(-1)。结论:该法操作简便、快速、灵敏,可用于测定血浆中非那雄胺浓度。
文摘To study Saikosaponins in a Chinese traditional compound medicine by LC/MS. Saikosaponin A and D, which were the bioactive components of Bupleurum falcatum L., were not found in the medicine. And three isomeric compounds of Saikosaponin A and D were detected instead. Saikosaponin A and D were found have turned into two other isomers after treated by acid water, but keep unchanged when treated by neutral water. Two of the isomeric compounds which found in the Compound medicine were determined as Saikosaponin B1 and B2 . This work is helpful for quality control of the medicine and also is useful for supervising the procedures of manufacture.
