【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。更多还原

【Abstract】 Objective The study was cond ucted to develop a method for determination of 8 anticoagulant rodenticides including brodifacoum, bromadiolone, coumatetralyl, warfarin, coumachlor,diphenadione, chlorophacinone, and pindone, in plasma by Qu ECh ERS cleanup coupled with isotope dilution and liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods Plasma samples were pre-treated by Qu ECh ERS 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, 2.4 μm) and eluted by methanol-ammonium acetate buffer gradient with a flow rate of 0.50 ml/min. The 8 anticoagulant rodenticides 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-25.0 μg/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.更多还原