血浆中可替宁和3-羟基可替宁的固体介质液液萃取-超高效液相色谱-串联质谱同时测定法  

Simultaneous determination of cotinine and 3-hydroxycotinine in plasma by solid-supported liquid-liquid extraction-ultrahigh performance liquid chromatography-tandem mass spectrometry

作　　者：林强 杨超 李美丽 王佳 侯灏然 丁昌明[2] LIN Qiang;YANG Chao;LI Mei-li;WANG Jia;HOU Hao-ran;DING Chang-ming(Department of Physical and Chemical Inspection,Beijing Yanqing District Center for Disease Control and Prevention,Bejing 102100,China)

机构地区：[1]北京市延庆区疾病预防控制中心理化检验科,北京102100 [2]中国疾病预防控制中心环境与健康相关产品安全所

出　　处：《环境与健康杂志》2024年第7期609-611,共3页Journal of Environment and Health

基　　金：国家人体生物监测项目(202101-SWYC)。

摘　　要：目的 建立血浆中可替宁和3-羟基可替宁的固体介质液液萃取-超高效液相色谱-串联质谱同时测定法。方法 在血浆样品中加入同位素内标和氢氧化钾后,使用96孔固体介质液液萃取提取盘净化,净化液经异丙醇二氯甲烷溶液洗脱、氮气吹干,纯水复溶,使用ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以0.1%氨水溶液-乙腈为流动相进行梯度洗脱,使用多反应监测模式采集数据。结果 可替宁和羟基可替宁在0.1~300 ng/ml线性范围内方法线性良好(r>0.999),可替宁方法定量下限为0.03 ng/ml,三羟基可替宁方法定量下限为0.02 ng/ml。可替宁的加标回收率为95.0%~99.4%,RSD为2.1%~3.3%。三羟基可替宁的加标回收率为95.8%~97.4%,RSD为2.1%~4.2%。结论 该方法取样量少、操作简便、方法精密度高,适合大规模样品的筛查检测工作。Objective To establish a method for the determination of cotinine and trihydroxycotinine in plasma.Methods After adding isotope internal standard and potassium hydroxide into the plasma sample,the 96 hole solid medium liquid-liquid extraction tray was used for purification.The purified solution was eluted with isopropanol dichloromethane,dried with nitrogen,and then redissolved with pure water.The ACQUITY UPLC BEH C18 chromatographic column(100 mm×2.1 mm,1.7µm)was used for gradient elution with 0.1%ammonia solution acetonitrile as the mobile phase.The data were collected by using the multi reaction monitoring mode.Results The linearity of cotinine and hydroxy cotinine was good in the linear range of 0.1-300 ng/ml(r>0.999).The limit of detection of for cotinine was 0.03 ng/ml,and that of trihydroxy cotinine method was 0.02 ng/ml.The recovery rate was 95.0%-99.4%,RSD was 2.1%-3.3%.The recovery of trihydroxycotinine was 95.8%-97.4%,RSD was 2.1%-4.2%.Conclusion This method has the advantages of less sampling,simple operation and high precision,and is suitable for screening and testing large scale samples.

关 键 词：固体介质液液萃取-液相色谱-串联质谱 血浆 可替宁 3-羟基可替宁 

分 类 号：O657.6[理学—分析化学]