HPLC-APCIMS联用法测定全血中杀鼠迷  

Characterization of Coumatetralyl in Whole Blood by Liquid Chromatography-Mass Spectrometry with Atmospheric Pressure Chemical Ionization Interface

作　　者：金米聪[1] 符展明[1] 王立[1] 

机构地区：[1]宁波市疾病预防控制中心,浙江宁波315010

出　　处：《分析测试学报》2006年第2期97-99,共3页Journal of Instrumental Analysis

基　　金：宁波市医学科研基金项目(200456;200543)

摘　　要：全血样品中痕量杀鼠迷经乙酸乙酯萃取，离心沉淀分离后，以甲醇-0．1％乙酸（体积比65：35，为流动相，通过大气压化学电离离子化技术及提取离子检测模式（EIC）进行测定。线性范围为0．30～100．0μg／L，定量下限为0．30μg／L，方法回收率在94％-105％范围，RSD小于10％。建立的方法具有简便、灵敏、准确的优点．与LC／UV法相比，本法约灵敏660倍。用于实际样品的检测，结果满意。A method is presented for characterization of coumatetralyl in whole blood by high performance liquid chromatography - mass spectrometry with an atmospheric pressure chemical ionization interface（HPLC -APCI MS）. Coumatetralyl in whole blood was extracted by ethyl acetate. Satisfactory separation was achieved on Zorbax XDB C18 column（ 150 mm ×4.6 mm × 5 μm） using a mobile phase consisting of CH3OH -0. 1% HAc（65 ： 35 by volume）. Ionization was performed in the APCI（ ＋ ） mode and quantitative analysis was carried out using the extracted ion chromatography （EIC） mode at m/z 293 [ M ＋ H ]^ ＋ The linear range was 0.30 - 100.0 μg/L and the limit of quantification was found to be 0. 30 μg/L. The extraction recoveries were between 94% - 105% with relative standard deviations of less than 10%. This method was sensitive, fast, and accurate in characterizing trace coumatetralyl in whole blood and can be carried out in the diagnosis of clinically poisoned patients.

关 键 词：全血 杀鼠迷 液相色潜-质谱联用 大气压化学电离 

分 类 号：O657.63[理学—分析化学] R979.8[理学—化学]