薄层条带净化技术在气相色谱-质谱联用仪检测毒鼠强方面的应用研究

The application study of thin layer slide technique in the detection of tetramine with gas chromatography-mass spectrometry

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 rapid analysis of tetramine presented in blood and vomiting sample with the combination of thin layer chromatography slide and gas chromatography- mass spectrometry（ GC- MS）,so as to provide reference for detection of mice drug in poising sample with high sensitivity. Methods After a serial of extraction,concentration,and clean- up steps on the thin layer slides,to obtain separation with interference presented in samples. When target zone was cut off from thin layer slide,extracted with ethyl acetate and concentrated with N2 flow,sample liquid was transferred into200 μl insert tube. Finally,concentrated sample solution was analyzed by GC- MS under SIM mode. Results The sample matrix obtained satisfactory clean- up,with getting rid of the interference from some high- boiling compounds,such as fat or sugar in samples. The linear range was good when the concentration of tetramine was among 0. 05 μg / L- 2. 0 μg / L,with the coefficience（ r） of 0. 999 1,the detection limit of 1. 3 μg / L,the recovery rate among 84. 5%- 94. 7%,and RSD among3. 4%- 6. 1%（ n = 6）. Conclusion This method is easy for operation,sensitive and precise,which can meet the requirement of analysis of low- content tetramine in poising samples blood and vomiting samples.