LC-MS/MS法测定人血浆中利血平浓度的不确定度评定
|
摘要
目的:评定LC-MS/MS法测定人血浆中利血平浓度的不确定度。方法:对血浆中利血平浓度测定过程中各影响因素,包括测定精密度、称量、标准溶液的配制、含药血浆的配制、血浆样品提取、仪器、标准曲线拟合等进行分析,计算各变量的不确定度和合成不确定度,最终计算扩展不确定度。结果:置信概率P为95%时,血浆低、中、高(20,10,300 pg·m L~(-1))质量浓度利血平的扩展不确定度分别为21.64,19.71和30.11 pg·m L~(-1)。结论:本方法适用于LC-MS/MS法测定血浆中利血平浓度的不确定度评定,为复杂生物基质分析过程的不确定度评定提供了参考。
Objective: To evaluate the uncertainty of the determination of reserpine concentration in human plasma by LC-MS / MS. Methods: Various factors influencing the uncertainty in the whole process of determination were analyzed and estimated,including precision,weighing,solution preparation,drug containing plasma preparation,plasma extraction,the apparatus,and calibration curves fitting. The uncertainty and synthetic uncertainty of each variable were calculated. The expanded uncertainty of all the components was analyzed. Results: When the confidence probability was P = 95%,the expanded uncertainty for low,medium and high( 20,100 and 300pg·m L~(-1)) concentrations of reserpine was 21. 64,19. 97,and 30. 11 pg·m L~(-1),respectively. Conclusion: This method is suitable for the uncertainty evaluation for the determination of reserpine concentration in human plasma by LC-MS / MS,and provides a reference for uncertainty evaluation of complex biological matrix analysis.
Objective: To evaluate the uncertainty of the determination of reserpine concentration in human plasma by LC-MS / MS. Methods: Various factors influencing the uncertainty in the whole process of determination were analyzed and estimated,including precision,weighing,solution preparation,drug containing plasma preparation,plasma extraction,the apparatus,and calibration curves fitting. The uncertainty and synthetic uncertainty of each variable were calculated. The expanded uncertainty of all the components was analyzed. Results: When the confidence probability was P = 95%,the expanded uncertainty for low,medium and high( 20,100 and 300pg·m L~(-1)) concentrations of reserpine was 21. 64,19. 97,and 30. 11 pg·m L~(-1),respectively. Conclusion: This method is suitable for the uncertainty evaluation for the determination of reserpine concentration in human plasma by LC-MS / MS,and provides a reference for uncertainty evaluation of complex biological matrix analysis.
引文
[1]MENG F,LIU R,GAO M,et al.Pinocembrin attenuates bloodbrain barrier injury induced by global cerebral ischemia-reperfusion in rats[J].Brain Res,1391(2011):93-101.
[2]严蓓,杨晨,李扬,等.HPLC法测定人血浆中奥硝唑浓度的不确定度评定[J].药物分析杂志,2011,31(9):1797-1803.
[3]曹国颖,齐文渊,张帅,等.LC-MS/MS法测定人血浆中齐多夫定浓度的不确定度评价[J].中国药房,2014,25(38):3595-3599.
[4]过林,裘福荣,王猛猛,等.人血浆中依折麦布浓度测定方法的不确定度评定[J].中南药学,2014,12(11):1099-1103.
[5]安胜男.HPLC-MS/MS法测定人血浆中硫酸双肼屈嗪浓度的不确定度评价[J].中国新药杂志,2015,24(19):2191-2196.
[6]赵娜萍.LC/MS/MS法测定人血浆中雷贝拉唑含量的不确定度评定[J].中国新药杂志,2014,23(02):210-214.
[7]齐会红.HPLC-MS/MS法测定人血浆中马来酸甲麦角新碱浓度的不确定度评价[J].中国新药杂志,2014,23(10):1127-1132.
[2]严蓓,杨晨,李扬,等.HPLC法测定人血浆中奥硝唑浓度的不确定度评定[J].药物分析杂志,2011,31(9):1797-1803.
[3]曹国颖,齐文渊,张帅,等.LC-MS/MS法测定人血浆中齐多夫定浓度的不确定度评价[J].中国药房,2014,25(38):3595-3599.
[4]过林,裘福荣,王猛猛,等.人血浆中依折麦布浓度测定方法的不确定度评定[J].中南药学,2014,12(11):1099-1103.
[5]安胜男.HPLC-MS/MS法测定人血浆中硫酸双肼屈嗪浓度的不确定度评价[J].中国新药杂志,2015,24(19):2191-2196.
[6]赵娜萍.LC/MS/MS法测定人血浆中雷贝拉唑含量的不确定度评定[J].中国新药杂志,2014,23(02):210-214.
[7]齐会红.HPLC-MS/MS法测定人血浆中马来酸甲麦角新碱浓度的不确定度评价[J].中国新药杂志,2014,23(10):1127-1132.