CAJ | 학술논문

目的：液相色谱－串联质谱法（ LC－MS／MS）评价人血浆头孢替安浓度测定的不确定度。方法对LC－MS／MS法测定血浆中头孢替安浓度的全过程各影响因素进行分析，包括精密度、称量、标准溶液的配制、含药血浆的配制、血浆样品预处理、仪器、标准曲线拟合等。用A类评定程序评价了分析过程中随机效应引起不确定度，用B类评定程序评价了分析过程的其他因素引起的不确定度，最后根据各分量计算出合成不确定度，并进行了扩展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。结果人血浆中200 ng · mL－1头孢替安的扩展不确定度为46.68 ng· mL－1（P＝95％，k＝2），标准曲线拟合产生的不确定度分量为1.16×10－1。结论 LC－MS／MS法测定人血浆中头孢替安浓度的不确定度主要是由标准曲线拟合、溶液配制和LC－MS／MS允差引入。
목적：액상색보－천련질보법（ LC－MS／MS）평개인혈장두포체안농도측정적불학정도。방법대LC－MS／MS법측정혈장중두포체안농도적전과정각영향인소진행분석，포괄정밀도、칭량、표준용액적배제、함약혈장적배제、혈장양품예처리、의기、표준곡선의합등。용A류평정정서평개료분석과정중수궤효응인기불학정도，용B류평정정서평개료분석과정적기타인소인기적불학정도，최후근거각분량계산출합성불학정도，병진행료확전계산각변량적불학정도화합성불학정도，최종계산확전불학정도。결과인혈장중200 ng · mL－1두포체안적확전불학정도위46.68 ng· mL－1（P＝95％，k＝2），표준곡선의합산생적불학정도분량위1.16×10－1。결론 LC－MS／MS법측정인혈장중두포체안농도적불학정도주요시유표준곡선의합、용액배제화LC－MS／MS윤차인입。
Objective To evaluate the uncertainty of cefotiam determi-nation in human plasma by LC -MS/MS method.Methods The uncer-tainty caused by various factors in the whole process of determination , such as repeatability , weighing , solution preparation , sample preparation process , the apparatus and calibration fitting , was estimated.The uncer-tainty caused by random effects and others was evaluated with type A and type B , respectively.The combined uncertainty was analyzed with all the components.Results The expanded uncertainty for cefotiam ( 200 ng· mL-1 ) was 46.68 ng· mL-1 ( P=95%, k=2).The largest uncer-tainty obtained from calibration curve was 1.16 ×10 -1.Conclusion The uncertainty of this method was mainly caused by calibration curve fit-ting, solution preparation and LC -MS/MS error.