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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: To establish a method for the determination of plasma levels of Dalong, bromadiolone, warfarin, warfarin, chlorpromazine, dipyridamole and chloroparasite in rats by LC-MS / MS with QuECh ERS purifying and isotope dilution liquid chromatography tandem mass spectrometry Determination of rat and naloxone anticoagulant rodenticides. Methods Plasma samples were pretreated with Qu ECh ERS method and warfarin-D5 was used as an internal standard. The plasma samples were separated by BDS HYPERSIL C18 (4.6 mm id × 100 mm, 2.4 μm) and eluted with methanol-ammonium acetate buffer. The flow rate was 0.50 ml / min. Electrospray ionization (ESI) negative ion mass spectrometry was used in multiple reaction monitoring (MRM) mode. Results The results showed that there was a good linearity (r> 0.999) for the eight anticoagulant rodenticides in the range of 0.20μg / L ~ 25.0μg / L (or 0.50μg / L ~ 25.0μg / L) with the detection limit of 0.044 ~ 0.19 μg / L. The average recoveries were 70.4% ~ 101.5% (n = 7) and the relative standard deviations were 1.7% ~ 8.9% (n = 7). Conclusion The method is rapid, simple and sensitive and can be applied to the simultaneous detection of 8 anticoagulant rodenticides in blood samples of poisoning patients.