CAJ | 학술논문

目的:建立人尿中睾内脂的LC-MS/MS检测方法.方法:采用Agilent Zorbax XDB-C_(18)柱(2.1×50mm,3.5μm),流动相采用pH3.5甲酸铵缓冲液(A)和乙腈(B)进行梯度洗脱,离子检测方式为多反应离子检测(MRM);离子极性为正离子,定量的离子对为m/z 301→121,定性的离子对为m/z 301→225.结果:测定人尿中内源性物质不干扰样品和内标,样品分析时间为7分钟,睾内脂线性范围为0.1～50μg/ml,提取回收率大约为60%,日内和日间的RSD均小于10%.结论:本方法经考察符合国际反兴奋剂机构(WADA)的要求,可以应用于常规的兴奋剂检测工作.
목적:건립인뇨중고내지적LC-MS/MS검측방법.방법:채용Agilent Zorbax XDB-C_(18)주(2.1×50mm,3.5μm),류동상채용pH3.5갑산안완충액(A)화을정(B)진행제도세탈,리자검측방식위다반응리자검측(MRM);리자겁성위정리자,정량적리자대위m/z 301→121,정성적리자대위m/z 301→225.결과:측정인뇨중내원성물질불간우양품화내표,양품분석시간위7분종,고내지선성범위위0.1～50μg/ml,제취회수솔대약위60%,일내화일간적RSD균소우10%.결론:본방법경고찰부합국제반흥강제궤구(WADA)적요구,가이응용우상규적흥강제검측공작.
Objecave To develop a sensitive and specific LC-MS/MS method for determination of testolactone in human urine.Methods A C_(18 )column(2.1×50mm,3.5μm) was used.The mobile phase Was a mixture of acetonitrile and the buffer solution(ammonium acetate-water solution adjusted with formic acid to pH 3.5)at a flow rate of 0.5ml/min.A mass spectrometer equipped with electrospray ionization source was used as a detector and operated in the positive mode.In multiple reaction monitoring(MRM)mode,the ion transitions of m/z 301→121 and m/z 301→25 was used to qualify and quantify the testolactone,respectively.Results Chromatograms showed no endogenous interfering peaks with the urine blank sample.Each analysis was completed within 7min The calibration wag linear in the concentration range within 0.1～50μg/ml.The intra-batch and inter-batch RSD were less than 10%.The recovery rate of the extraction was about 60%.Conclusions The method is proved to meet the requirements of WADA and be suitable for routine screening.