安徽医药
安徽醫藥
안휘의약
ANHUI MEDICAL AND PHARMACEUTICAL JOURNAL
2015年
4期
627-631
,共5页
过林%裘福荣%王猛猛%贺敏%蒋健
過林%裘福榮%王猛猛%賀敏%蔣健
과림%구복영%왕맹맹%하민%장건
双氯芬酸钠%LC-MS/MS%血药浓度%不确定度
雙氯芬痠鈉%LC-MS/MS%血藥濃度%不確定度
쌍록분산납%LC-MS/MS%혈약농도%불학정도
diclofenac sodium%LC-MS/MS%plasma concentration%uncertainty
目的:研究高效液相色谱—串联质谱法( LC-MS/MS)法测定人血浆中双氯芬酸浓度的不确定度评定方法。方法对双氯芬酸浓度测定全过程进行分析,包括测定精密度、称量、标准溶液的配制、蛋白沉淀过程、标准曲线拟合等进行分析评定,最后根据各分量计算出合成不确定度并进行了扩展。结果置信概率为95%时,人血浆中2.0、50.0、1600μg· L-1浓度双氯芬酸的扩展不确定度分别为(1.97±1.482)、(46.97±3.72)、(1494±87.2)μg· L-1。结论该方法不确定度主要来自标准曲线的拟合过程,该法适用于评定LC-MS/MS法测定血浆中双氯芬酸的不确定度研究。
目的:研究高效液相色譜—串聯質譜法( LC-MS/MS)法測定人血漿中雙氯芬痠濃度的不確定度評定方法。方法對雙氯芬痠濃度測定全過程進行分析,包括測定精密度、稱量、標準溶液的配製、蛋白沉澱過程、標準麯線擬閤等進行分析評定,最後根據各分量計算齣閤成不確定度併進行瞭擴展。結果置信概率為95%時,人血漿中2.0、50.0、1600μg· L-1濃度雙氯芬痠的擴展不確定度分彆為(1.97±1.482)、(46.97±3.72)、(1494±87.2)μg· L-1。結論該方法不確定度主要來自標準麯線的擬閤過程,該法適用于評定LC-MS/MS法測定血漿中雙氯芬痠的不確定度研究。
목적:연구고효액상색보—천련질보법( LC-MS/MS)법측정인혈장중쌍록분산농도적불학정도평정방법。방법대쌍록분산농도측정전과정진행분석,포괄측정정밀도、칭량、표준용액적배제、단백침정과정、표준곡선의합등진행분석평정,최후근거각분량계산출합성불학정도병진행료확전。결과치신개솔위95%시,인혈장중2.0、50.0、1600μg· L-1농도쌍록분산적확전불학정도분별위(1.97±1.482)、(46.97±3.72)、(1494±87.2)μg· L-1。결론해방법불학정도주요래자표준곡선적의합과정,해법괄용우평정LC-MS/MS법측정혈장중쌍록분산적불학정도연구。
Objective To develop a method to evaluate the uncertainty in the determination of diclofenac in human plasma by LC-MS/MS.Methods The uncertainty sources were obtained from the determination of the whole procedure,including repeatability,weighing, solution preparation,protein precipitation process,the apparatus and calibration fitting.The combined uncertainty and expanded uncer-tainty were calculated accordingly.Results The expanded uncertainty for 2.0,50.0,1 600μg· L-1 level of diclofenac was (1.97 ± 1.482)、(46.97 ±3.72),and(1 494 ±87.2)μg· L-1 respectively (P=95%).Conclusion The uncertainty is mainly caused by calibration curve.This method is suitable for the uncertainty evaluation in human plasma by LC-MS/MS.