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作 者:邹燕[1] 李斌[1] 刘明东[1] 冯德建[1] 王彧婕[1] 马丽侠[1] 周李华[1] ZOU Yan;LI Bin;LIU Mingdong;FENG Dejian;WANG Yujie;MA Lixia;ZHOU Lih ua(Institute of Biology,National Institute of Measurement and Te sting Technology,Chengdu 610021,China)
机构地区:[1]中国测试技术研究院生物研究所,四川成都610021
出 处:《中国测试》2024年第S2期99-108,共10页China Measurement & Test
基 金:国家重点研发计划项目(2021YFF0701900);四川省重要技术标准研究项目(ZYBZ2023-1)
摘 要:该文建立了高效液相色谱-串联质谱法同时测定人体尿液、血清中9种酰基肉碱含量的方法。试样经甲醇沉淀蛋白后,Waters ACQUITY UPLC HSS T3柱(2.1mm×150mm, 1.8μm)分离,正离子多反应监测模式测定,同位素内标法定量。结果表明方法线性关系良好,定量限范围为0.78~7.81μg/L,3个水平的平均加标回收率为91.79%~104.25%,中间精密度的相对标准偏差为1.19%~5.59%。用该方法对39份人血清样本、45份人体尿液样本进行测定,除人体尿液和血清中戊酰基-L-肉碱以及尿液中肉豆蔻酰基-L-肉碱未检出外,其余肉碱的检出率均为100%。该方法具有操作简便、准确性好、重复性佳、检测效率高等特点,且能很好分离4种酰基肉碱同分异构体,可满足人体尿液以及血清中9种酰基肉碱含量的同时准确测定需要。A method was established for simultaneous determination of nine acylcarnitine in human urine and serum with high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)in this article.The sample was purified by methanol,then separated on a Waters ACQUITY UPLC HSS T3 column(2.1mm x 150mm,1.8μm),and detected in positive electrospray(ESI+)under multiple reaction monitoring(MRM)mode.All acylcarnitine showed good linear relationships,and the quantitative limit range of the method was 0.78μg/L to 7.81μg/L,and in three standard levels,the average rate of recovery rate ranged from 91.79%to 104.25%,and the relative standard deviation(RSD)of the relinearity was 1.19%to 5.59%.The results of 39 human serum samples and 45 human urine samples showed that the detection rates of acylcarnitine were 100%,except for myristoyl-L-carnitine Eppenin human urine and valeroyl-L-carnitine in human urine and serum.This method is simple,good accuracy,strong applicability and high detection efficiency.It can also effectively separate four isomers of acylcarnitine and can be used for the simultaneous determination of nine acylcarnitine in human urine and serum.
关 键 词:人体尿液 血清 酰基肉碱 高效液相色谱-串联质谱法 同时测定
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