肝中对硫磷的固相萃取—电子捕获检测气相色谱分析法

目的建立肝中对硫磷的快速、灵敏、可靠的GC／ECD分析方法。方法肝匀浆加内标甲基对硫磷,用乙腈浸提,浸提液加6％高氯酸稀释,稀释的上清液用GDX403树脂进行固相提取,提取物用HP-5色谱柱和电子捕获检测器进行气相色谱分析。结果提取率92.3％,检测限7.8ng／g,线性范围0.04～4.0μg／g,回收率99.6％±6.2％(Mean±CV,n=5)。结论方法简便、灵敏适合于实际案件检验。

The Analysis of Parathion in liver by gas chromatography and electron-capture detection

Objective To develop a sensitive, reliable, and rapid method for determination of Paration in liver by gas chromatography and electron-capture detection. Methods The homogenized liver samples to which methyl parathion (I.S) was added were impregnated with acetonitrile, and then diluted with 6% perchloric acid. The supernatants were extracted with GDX403 porous resin by solid-phase and eluted with ethyl ether. The extractives were chromatographed on HP-5 column and detected by electron capture detector. Results The extraction efficiency was 92.3% , and the limit of detection was 7.8ng/g with good linearity ranging between 0.04μg/g and 4μg/g. The average recovery was 99.6% and its CV was 6.2%. Conclusion The method is applicable to determination of Parathion in liver in practice.