摘要
目的评定超高液相色谱-串联质谱法(UPLC-MS/MS)测定大鼠尿样中26-OH-PD浓度的不确定度。方法分析UPLC-MS/MS法测定大鼠尿样中26-OH-PD浓度的不确定度来源,根据各分量计算出合成不确定度并进行了扩展。结果大鼠尿样中低浓度(6.16 ng/m L)、中浓度(97.94 ng/m L)和高浓度(398.02ng/m L)26-OH-PD的扩展不确定度分别为1.44、6.97、22.05 ng/m L(P=95%,k=2)。结论 UPLC-MS/MS法测定大鼠尿样中26-OH-PD低浓度样品的不确定度主要分别由线性拟合引入,中、高浓度样品的不确定度主要由仪器允差引入。该法适用于评定UPLC-MS/MS法测定尿样中26-OH-PD的不确定度研究,能为复杂生物样品分析过程的不确定度评定提供一定参考。
Objective To evaluate the uncertainty in 26-OH-PD determination in human urine by UPLC-MS/MS. Methods The whole proces of the 26-OH-PD determination was analyzed and the uncertainty from various sources were calculated, and then the combined and expanded uncertainty were also evaluated. Results The expanded uncertainty of 26-OH-PD at low （6.16 ng/mL）, medium （97.94 ng/mL） and high （398.02 ng/mL） level was 1.44 ng/mL, 6.97 ng/mL and 22.05 ng/mL （P= 95%, k = 2）. Conclusion Calibration curve fitting was the main source of uncertainty for the low concentration of 26-OH-PD, and instrument tolerance were the main source of uncertainty for the determination of 26-OH-PD at high and medium concentration. This method could be used to evaluate the uncertainty of 26-OH-PD determination in urine. Reference was also provided for the uncertainty evaluation in drug analysis.
作者
林美妤
张楠淇
王翠竹
朱海林
刘金平
李平亚
LIN Meiyu;ZHANG Nanqi;WANG Cuizhu;ZHU Hailin;LIU Jinping;LI Pingya(Hunan University of Chinese Medicine, Changsha 410013, China;School of Pharmaceutical Sciences, Jilin University, Changchun 130021, China)
出处
《药物评价研究》
CAS
2018年第4期582-588,共7页
Drug Evaluation Research
