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超高效液相色谱-质谱联用法同时测定中毒样品中12种鼠药
Simultaneous detection of 12 kinds of rodenticides in poisoned samples by ultra performance liquid chromatography-tandem mass spectrometry

作  者: ; ; ; ; ; ;

机构地区: 深圳市疾病预防控制中心

出  处: 《中国职业医学》 2019年第1期92-97,共6页

摘  要: 目的建立超高效液相色谱-质谱联用法同时测定疑似鼠药中毒患者残留食物、呕吐物、洗胃液、血清及尿液中毒鼠强、杀鼠灵和杀鼠迷等12种鼠药的方法。方法采集疑似鼠药中毒患者残留食物、呕吐物、洗胃液、血清及尿液;其中食物、呕吐物、洗胃液和尿液样品中先加入浓度为2 mol/L的乙酸铵,随后加入乙酸乙酯重复提取2次,血清样品加入乙腈进行提取。样品经氮气吹干后,以甲醇∶乙酸铵溶液(60∶40,V/V)溶解,离心取上清液经C18柱分离,标准曲线法定量,采用超高效液相色谱-质谱联用仪检测。结果 12种鼠药在疑似鼠药中毒患者残留食物、呕吐物、洗胃液、血清及尿液的定量范围内线性关系良好,相关系数为0.992 3~0.999 9。方法检出限在食物、呕吐物或洗胃液为0.03~0.14μg/kg,在血清、尿液分别为0.10~0.30和0.02~0.04μg/L。加标回收率为84.4%~114.0%,批内、批间相对标准偏差分别为2.7%~6.2%和2.4%~9.5%。结论本方法操作简单、高效、准确,适用于因误食鼠药或投毒引起的中毒事件的应急处理。 Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS) method for simultaneous detection of 12 kinds of rodenticides such as tetramine, warfarin and rodenticide in suspected poisoning patients’ residual food, vomit, gastric lavage, serum and urine. Methods The residual food, vomit, gastric lavage, serum and urine of patients with suspected rodenticide poisoning were collected. The food, vomit, gastric lavage and urine samples were added with ammonium acetate at a concentration of 2 mol/L, and than were repeatedly extracted twice by ethyl acetate. The serum sample was extracted by adding acetonitrile. After the sample was dried by nitrogen, it was dissolved in methanol ∶ammonium acetate(60 ∶40, V/V), and the supernatant was centrifuged and separated by a C18 column, and quantified by a standard curve method. Samples were detected by HPLC-MS. Results The linearity of the 12 kinds of rodenticides in the quantitative range of residual food, vomit, gastric lavage, serum and urine in patients with suspected rodenticide poisoning was good, and the correlation coefficient was 0.992 3-0.999 9. The detection limit of food, vomit or gastric lavage was 0.03-0.14 μg/kg, and that in serum and urine were 0.10-0.30 and 0.02-0.04 μg/L, respectively. The standard recovery rate was 84.4%-114.0%, and the within-run and between-run relative standard deviations were 2.7%-6.2% and 2.4%-9.5%, respectively.Conclusion The method has advantages of simple operation, high efficiency and good accuracy. This method is suitable for emergency treatment of poisoning events caused by rodent drugs or poisoning.

关 键 词: 鼠药 毒鼠强 超高效液相色谱 质谱 串联 联用技术 中毒

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