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目的建立一种抗凝血类鼠药中毒的快速筛查法,即尿样中抗凝血类鼠药代谢产物亚苄基丙酮的气相色谱-质谱(GC-MS)检测方法。方法收集中毒者尿样,用氯仿振摇提取10 min,以4 000 r/min离心5 min,取下层氯仿提取液供气相色谱-质谱仪分离定性,外标法定量。结果在浓度为0.065μg/L~50μg/L时,线性关系良好,线性方程为y=9.686 42x+26.302 5,线性相关系数(r)为0.999 3。方法的检出限为0.065μg/L,定量限为0.216μg/L。在高、低2种加标浓度水平下的回收率分别为87.7%~99.7%,相对标准偏差(RSD)为2.1%~4.5%。结论该法前处理操作简单快速,定性准确,检出限低,回收率高,精密度和准确度高。实际样品检测结果显示,本方法可以满足抗凝血类鼠药中毒快速筛查的要求。
Objective To establish a rapid screening method for anticoagulant poisoning in rats, which is the gas chromatography-mass spectrometry (GC-MS) method for the determination of benzaldehyde acetone in anticoagulant rat urine samples. Methods Urine samples from poisoning were collected and extracted by chloroform for 10 min. The samples were centrifuged at 4 000 r / min for 5 min. The chloroform extracts were separated by gas chromatography - mass spectrometry and quantified by external standard method. Results The linear equation was y = 9.686 42x + 26.302 5 at a concentration of 0.065μg / L ~ 50μg / L with a linear correlation coefficient (r) of 0.999 3. The detection limit of the method was 0.065μg / L, the limit of quantification was 0.216μg / L. The recoveries were 87.7% -99.7% at high and low spiked levels, and the relative standard deviations (RSDs) were 2.1% -4.5%. Conclusion The pretreatment method is simple, rapid, accurate, low detection limit, high recovery rate, high precision and accuracy. The actual sample test results show that this method can meet the requirements of rapid screening of anticoagulant drug poisoning rats.