血浆甲氧基去甲肾上腺素候选参考方法的建立及其在室间质量评价计划中的应用  

Establishment of a candidate reference method for plasma normetanephrine and its application in the external quality assessment program

作　　者：刘庆香 周伟燕[2] 邓宇航 刘珍妮 张传宝[1] Liu Qingxiang;Zhou Weiyan;Deng Yuhang;Liu Zhenni;Zhang Chuanbao(Chinese Academy of Medical Sciences and Peking Union Medical College,National Center for Clinical Laboratories,Beijing Engineering Research Center of Laboratory Medicine,Beijing Hospital,National Center of Gerontology,Institute of Geriatric Medicine,Chinese Academy of Medical Sciences,Beijing 100730,China;National Center for Clinical Laboratories,Beijing Engineering Research Center of Laboratory Medicine,Beijing Hospital,National Center of Gerontology,Institute of Geriatric Medicine,Beijing 100730,China)

机构地区：[1]北京医院国家老年医学中心中国医学科学院老年医学研究院国家卫生健康委临床检验中心北京市临床检验工程技术研究中心中国医学科学院北京协和医学院,北京100730 [2]北京医院国家老年医学中心中国医学科学院老年医学研究院国家卫生健康委临床检验中心北京市临床检验工程技术研究中心,北京100730

出　　处：《中华检验医学杂志》2021年第8期736-742,共7页Chinese Journal of Laboratory Medicine

基　　金：北京自然科学基金(7212087);北京市科协“金桥工程种子资金”。

摘　　要：目的建立同位素稀释液相色谱串联质谱法(ID-LC/MS/MS)测定人血浆甲氧基去甲肾上腺素的候选参考方法,并对方法性能进行评价。采用该方法对室间质量评价计划样品进行定值,初步评价血浆甲氧基去甲肾上腺素的检测现状。方法采用甲氧基去甲肾上腺素同位素标准溶液为内标,重量法进行取样,标准曲线法进行定量;采用蛋白沉淀结合弱阳离子固相萃取进行前处理,采用超高液相色谱耦联三重四极杆质谱仪进行液质联用分析。根据相关EP文件对方法的特异性、基质效应、检测限、定量限、精密度、正确度和不确定度等性能指标进行了评价。采用该方法对2020年国家卫生健康委临床检验中心甲氧基去甲肾上腺素室间质量评价计划样品进行定值,以该定值结果为靶值,生物学变异最佳可允许总误差标准为评价限,对实验室的检测质量进行评价。结果方法特异性良好,干扰物和基质效应均不影响检测结果。血浆甲氧基去甲肾上腺素测定的检测限及定量限分别为1.08 pg/g和3.54 pg/g,批内变异系数(CV)和批总CV分别为0.43%~1.10%、0.61%~1.42%,相对回收率为98.5%~101.9%,4种血浆样品的相对扩展不确定度分别为3.10%、2.34%、2.16%、1.73%。室间质量评价计划结果显示,实验室测定202013和202014样品的及格率分别为80%和85%。结论本研究建立了ID-LC/MS/MS测定人血浆甲氧基去甲肾上腺素的候选参考方法,方法准确、精密、简便,有望作为血浆甲氧基去甲肾上腺素测定的参考方法,可应用于室间质量评价计划样本的定值。Objectives To establish a candidate reference method of isotope dilution liquid chromatography tandem mass spectrometry(ID-LC/MS/MS)for the determination of human plasma normetanephrine,and to evaluate the performance of the method.The method was used to quantify the samples of the external quality assessment program,and to initially evaluate the detection status of plasma normetanephrine.Methods The isotope standard solution of normetanephrine was selected as the internal standard,the gravimetric method was used for sampling,and the standard curve method was used for quantification.Protein precipitation combined with weak cation solid phase extraction was used for pretreatment,and ultra-high liquid chromatography-coupled triple quadrupole mass spectrometry was used for LC/MS analysis.According to the relevant EP documents,the specificity,matrix effect,detection limit,quantification limit,precision,accuracy,and uncertainty of the method were estimated.This method is used to quantify the samples of the 2020 National Center for Clinical Laboratories external quality assessment program of normetanephrine.Taking the average value of this method as the target value,the optimal allowable total error standard of biological variation as the evaluation limit,the quality of the laboratory testing was evaluated.Results The method had good specificity,and the interferences and matrix effects did not affect the detection results.The detection limit and quantification limit of plasma normetanephrine were 1.08 pg/g and 3.54 pg/g,respectively.The intra-batch coefficient of variation(CV)and total CV were 0.43%-1.10%and 0.61%-1.42%,respectively.The relative recovery rates were 98.5%~101.9%.The relative expansion uncertainty of the four plasma samples were 3.10%,2.34%,2.16%,and 1.73%,respectively.The results of the external quality assessment program showed that the pass rates of the 202013 and 202014 samples were 80%and 85%,respectively.Conclusions The study established a candidate reference method of ID-LC/MS/MS for the measureme

关 键 词：同位素稀释液相色谱串联质谱 甲氧基去甲肾上腺素 室间质量评价计划 

分 类 号：R446.11[医药卫生—诊断学]