LC-MS/MS法测定人血浆中布康唑浓度的不确定度评定
|
摘要
目的:评定LC-MS/MS法测定人血浆中布康唑浓度的不确定度。方法:分析测定过程中不确定度的来源,包括对照品的称量、仪器误差、标准溶液的配制、含药血浆样品的配制、血浆样品的处理、标准曲线的拟合、基质效应、重复性等,评定各来源分量的不确定度,计算合成不确定度和扩展不确定度。结果:人血浆中低(60.0 pg·mL~(-1))、中(600.0 pg·mL~(-1))、高(6 400.0 pg·mL~(-1))浓度布康唑的扩展不确定度分别为5.62,63.90,626.26 pg·mL~(-1)(k=2,P=95%)。结论:LC-MS/MS法测定人血浆中布康唑浓度的不确定度主要由基质效应、血浆样品的处理(提取回收率),仪器误差、重复性(精密度)引入。
OBJECTIVE To evaluate the uncertainty of the determination of butoconazole in human plasma by LC-MS/MS. METHODS The sources of uncertainty in the determination process were analyzed, including the weighing of reference substances, instrumental errors, preparation of standard solutions, preparation of drug-containing plasma samples, processing of plasma samples, fitting of standard curve, matrix effect, repeatability, etc. The uncertainty of each source component was evaluated to calculate combined uncertainty and expanded uncertainty. RESULTS The expanded uncertainties of low(60.0 pg·mL~(-1)), medium(600.0 pg·mL~(-1)) and high(6 400.0 pg·mL~(-1)) level of butoconazole in human plasma was 5.62, 63.90, 626.26 pg·mL~(-1), respectively(k=2, P=95%). CONCLUSION The uncertainty of the determination of butoconazole by LC-MS/MS is mainly caused by matrix effect, pretreatment of plasma samples, instrumental error and repeatability.
OBJECTIVE To evaluate the uncertainty of the determination of butoconazole in human plasma by LC-MS/MS. METHODS The sources of uncertainty in the determination process were analyzed, including the weighing of reference substances, instrumental errors, preparation of standard solutions, preparation of drug-containing plasma samples, processing of plasma samples, fitting of standard curve, matrix effect, repeatability, etc. The uncertainty of each source component was evaluated to calculate combined uncertainty and expanded uncertainty. RESULTS The expanded uncertainties of low(60.0 pg·mL~(-1)), medium(600.0 pg·mL~(-1)) and high(6 400.0 pg·mL~(-1)) level of butoconazole in human plasma was 5.62, 63.90, 626.26 pg·mL~(-1), respectively(k=2, P=95%). CONCLUSION The uncertainty of the determination of butoconazole by LC-MS/MS is mainly caused by matrix effect, pretreatment of plasma samples, instrumental error and repeatability.
引文
[1] Tatum DM,Eggleston M.Butoconazole nitrate [J].Infect Cont Hosp Ep,1988,9(3):122-124.
[2] Jacobson JB,Hajman AJ,Wiese J,et al.A new vaginal antifungal agent-butoconazole nitrate[J].Acta Obstet Gyn Scan,1985,64(3):241-244.
[3] Bradbeer CS,Mayhew SR,Barlow D.Butoconazole and miconazole in treating vaginal candidiasis[J].Genitourin Med,1985,61(4):270-272.
[4] Brown Jr D,Henzl MR,LePage ME,et al.Butoconazole vaginal cream in the treatment of vulvovaginal candidiasis.Comparison with miconazole nitrate and placebo[J].J Reprod Med,1986,31(11):1045-1048.
[5] Henzl MR.Metabolism of butoconazole [J].J Reprod Med,1986,31(7):658-659.
[6] Liu YN,Ma L,Liu JM,et al.Evaluation of uncertainty for the determination of cefotetan disodium in human plasma by HPLC [J].Chin Hosp Pharm J (中国医院药学杂志),2013,33(20):1695-1698.
[7] Huang YF,Ma L,Li WY,et al.Uncertainty Evaluation of the Determination of Levosulpiride in Human Plasma by LC-MS/MS [J].China Pharmacist (中国药师),2016,19(12):2369-2372.
[8] Evaluation and Expression of Uncertainty in Measurement,JJF 1059.1-2012 (测量不确定度评定与表示).2012:12.
[9] Ni YC.Practical Evaluation of Uncertainty in Measurement (实用测量不确定度评定) [M].Beijing (北京):China Mensuration Press,2004:180.
[10] Shi CY.Guidelines for Evaluation and Expression of Uncertainty in Measurement (测量不确定度评定与表示指南) [M].Beijing (北京):China Mensuration Press,2005:32.
[11] Jia MM,Zhou Y,He XM,et al.Development of liquid chromatography-tandem mass spectrometry method for determination of butoconazole nitrate in human plasma and its application to a pharmacokinetic study [J].J Huazhong Univ Sci Tech Med Sci,2014,34(3):431-436.
[2] Jacobson JB,Hajman AJ,Wiese J,et al.A new vaginal antifungal agent-butoconazole nitrate[J].Acta Obstet Gyn Scan,1985,64(3):241-244.
[3] Bradbeer CS,Mayhew SR,Barlow D.Butoconazole and miconazole in treating vaginal candidiasis[J].Genitourin Med,1985,61(4):270-272.
[4] Brown Jr D,Henzl MR,LePage ME,et al.Butoconazole vaginal cream in the treatment of vulvovaginal candidiasis.Comparison with miconazole nitrate and placebo[J].J Reprod Med,1986,31(11):1045-1048.
[5] Henzl MR.Metabolism of butoconazole [J].J Reprod Med,1986,31(7):658-659.
[6] Liu YN,Ma L,Liu JM,et al.Evaluation of uncertainty for the determination of cefotetan disodium in human plasma by HPLC [J].Chin Hosp Pharm J (中国医院药学杂志),2013,33(20):1695-1698.
[7] Huang YF,Ma L,Li WY,et al.Uncertainty Evaluation of the Determination of Levosulpiride in Human Plasma by LC-MS/MS [J].China Pharmacist (中国药师),2016,19(12):2369-2372.
[8] Evaluation and Expression of Uncertainty in Measurement,JJF 1059.1-2012 (测量不确定度评定与表示).2012:12.
[9] Ni YC.Practical Evaluation of Uncertainty in Measurement (实用测量不确定度评定) [M].Beijing (北京):China Mensuration Press,2004:180.
[10] Shi CY.Guidelines for Evaluation and Expression of Uncertainty in Measurement (测量不确定度评定与表示指南) [M].Beijing (北京):China Mensuration Press,2005:32.
[11] Jia MM,Zhou Y,He XM,et al.Development of liquid chromatography-tandem mass spectrometry method for determination of butoconazole nitrate in human plasma and its application to a pharmacokinetic study [J].J Huazhong Univ Sci Tech Med Sci,2014,34(3):431-436.