液相色谱-电喷雾串联质谱法快速测定人体血液中左旋甲基炔诺酮的含量  

Rapid determination of Levonorgestrel in human serum by high-performance liquid chromatography-tandem mass spectrometry with electroyspray ionization

作　　者：王鹏[1] 朱宽正[2] 林雁飞 罗静 梅素容[2] 周宜开[2] 

机构地区：[1]湖北省出入境检验检疫局,湖北武汉430022 [2]华中科技大学同济医学院公共卫生学院

出　　处：《山西师范大学学报（自然科学版）》2006年第2期54-58,共5页Journal of Shanxi Normal University(Natural Science Edition)

基　　金：国家自然科学基金(20407009);湖北省自然科学基金(2003ABA060)

摘　　要：建立了快速测定人体血液中左旋甲基炔诺酮的液相色谱-串联质谱法.样品加入内标后,经过一个简单的预处理,以电喷雾正离子多反应监测方式进行定性定量分析,并且优化了液相和质谱条件.方法简单快速,一个样品的分析时间仅需10min;方法的检出限为0.2 ng/mL,线性范围为0.625ng/mL^35.0ng/mL,测定结果重复性很好,日内和日间的相对标准偏差均小于3.74%,在添加浓度为1.25ng/mL、5.0ng/mL3、5.0 ng/mL时,回收率分别为(92.1±2.8)%,(95.7±3.4)%,(105.8±3.1)%.通过以与新鲜血液比较,经过冷冻~解冻后的血液样品测量值稳定.结果表明,本方法适合于人体血清中左旋甲基炔诺酮含量的测定.A LC-MS/MS method was developed for rapid determination of Levonorgestrel(LNG) in human serum.After addition of Mifepristone as the internal standard,serum samples were extracted with the mixture of aether and chloroform(60∶40,v∶v) without any additional clean up procedures.Analytical identification and quantification were performed using multiple reaction monitoring(MRM) and electrospray ionization in positive mode.The total chromatographic runtime of this method was 10.0 min per sample.The assay was linear over the range of 0.625ng/mL^35ng/mL and the detection limit of this method was 0.2ng/mL.The analytical precision,estimated as both the inter-assay and intra-assay was consistently less than 3.74%.The recovery of LNG from fortified serum samples were 92.1%±2.8%,95.7%±3.4% and 105.8%±3.1% at 1.25,5.0ng/mL and 35 ng/mL,respectively.The result for the stability of LNG under freeze-thaw demonstrated little difference,compared with the freshly prepared samples.These results suggested this method was robust and suitable for determination of LNG in human serum.

关 键 词：液相色谱-串联质谱 左旋甲基炔诺酮 人体血液 

分 类 号：O657.63[理学—分析化学] O625.42[理学—化学]