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目的建立了薄层条带净化与用气相色谱-质谱联用仪(GC-MS)联用快速检测血样及呕吐物样品中毒鼠强的方法,为高灵敏度检测中毒样品中鼠药提供参考。方法样品经过提取、浓缩,在薄层板上通过净化,实现与杂质分离,裁剪目标区条带,用乙酸乙酯进行提取,氮吹浓缩后置于200μl内插管中,用气相色谱-质谱联用仪测定,在SIM模式下进行定量。结果样品基质获得完美净化,摆脱了样品中存在的一些高沸点物质(脂肪、糖类等)干扰,毒鼠强在0.05μg/L~2.0μg/L时线性关系良好,相关系数(r)为0.999 1,方法的最低检出限为1.3μg/L,加标回收率为84.5%~94.7%,相对偏差为3.4%~6.1%(n=6)。结论该方法操作方便、灵敏准确,能满足血液和呕吐物样品中较低浓度的毒鼠强分析要求。
OBJECTIVE: To establish a method for the rapid detection of poisoned rats in blood samples and vomit samples by gas chromatography-mass spectrometry (GC-MS) combined with thin-strip purification and provide a reference for the high sensitive detection of rat poison in poisoned samples. Methods The samples were extracted, concentrated, purified on a thin plate, and separated from the impurities. The target bands were cut and extracted with ethyl acetate. After nitrogen was concentrated, the sample was placed in a 200 μl internal cannula and analyzed by gas chromatography-mass spectrometry Combined measurement, quantitative determination in the SIM mode. Results The sample matrix was perfectly purified and freed from the interference of some high-boiling substances (fat, sugar, etc.) in the samples. The linearity of the tetramine was strong at 0.05μg / L ~ 2.0μg / L with the correlation coefficient 0.999 1. The detection limit of this method was 1.3 μg / L. The spiked recoveries ranged from 84.5% to 94.7%. The relative deviations ranged from 3.4% to 6.1% (n = 6). Conclusion The method is convenient, sensitive and accurate, and can meet the needs of higher concentration of tetramine in blood and vomit samples.