QuEChERS净化—液相色谱串联质谱法测定血浆中8种抗凝血灭鼠剂  

Determination of 8 anticoagulant rodenticides in plasma by Qu ECh ERS cleanup-liquid chromatography-tandem mass spectrometry

作　　者：谢维平[1] 欧阳燕玲[1] 苏碧玲[1] 

机构地区：[1]福建省泉州市疾病预防控制中心理化检验科,福建泉州362000

出　　处：《现代预防医学》2016年第12期2229-2233,共5页Modern Preventive Medicine

基　　金：泉州市重点科技计划项目(2012Z79)

摘　　要：目的建立Qu ECh ERS净化,同位素稀释液相色谱串联质谱法(LC-MS/MS)测定血浆中大隆、溴敌隆、杀鼠醚、杀鼠灵、氯杀鼠灵、敌鼠、氯敌鼠、杀鼠酮抗凝血灭鼠剂的检测方法。方法血浆样品经Qu ECh ERS方法前处理,以杀鼠灵-D5作为同位素内标,采用BDS HYPERSIL C18(4.6 mm i.d×100 mm,2.4μm)分离,以甲醇-乙酸铵缓冲液梯度洗脱,流速为0.50 ml/min。采用电喷雾电离(ESI)负离子质谱在多反应监测(MRM)模式下检测。结果 8种抗凝血灭鼠剂在0.20μg/L^25.0μg/L(或者0.50μg/L^25.0μg/L)范围内有良好的线性关系(r>0.999),检测限为0.044~0.19μg/L,平均加标回收率为70.4%~101.5%(n=7),相对标准偏差1.7%~8.9%(n=7)。结论该方法快速、简单,灵敏度高,可应用于中毒病人血样中8种抗凝血灭鼠剂的同时检测。Objective The study was conducted to develop a method for determination of 8 anticoagulant rodenticides including brodifacoum, bromadiolone, eoumatetralyl, warfarin, coumachlor, diphenadione, ehlorophacinone, and pindone, in plasma by QuEChERS cleanup coupled with isotope dilution and liquid chromatography-tandem mass spectrometry （LC-MS/ MS）. Methods Plasma samples were pre-treated by QuEChERS method, and warfarin-D5 was adopted as the isotopic internal standard. The compounds were separated on a BDS HYPERSIL C18 column （4.6 mm i.d×100 mm, 2.4μ m） and eluted by methanol-ammonium acetate buffer gradient with a flow rate of 0.50 ml/min. The 8 anticoagulant rodentieides were detected by electrospray ionization （ESI）-negative ion mass spectrometry under the multiple-reaction monitoring （MRM） mode. Results A good linearity was observed in the range of 0.20 μg/L-25.0 μg/L （or 0.50 μg/L-25.0μg/L）（r〉0.999） of the anticoagulant rodenticides. The detection limit of the method was 0.044-0.19 μg/L, the average sample recovery rate ranged between 70.4% and 101.5% （n=7）, and the relative standard deviation （RSD） was 1.7%-8.9% （n=7）. Conclusion The method is fast, simple, highly sensitive, and can be adopted for simultaneous detection of the 8 anticoagulant rodenticides in plasma of intoxicated patients.

关 键 词：高效液相色谱-串联质谱法 抗凝血灭鼠剂 QU ECh ERS 同位素稀释法 血浆 

分 类 号：R319[医药卫生—基础医学]