液液萃取-固相萃取气相色谱法测定火腿中有机磷农药残留量

Determination of Organophosphate Pesticide Residues in Ham Using Liquid-liquid Extraction/Solid-Phase Extraction with Gas Chromatography

[目的]建立火腿中多种有机磷农药残留量同时测定的方法。[方法]火腿中有机磷农药经乙腈提取后,用乙腈-正己烷液液萃取除去脂类和色素,再经石墨碳黑固相萃取小柱净化,气相色谱-火焰光度检测器(GC-FPD)测定。[结果]16种有机磷农药在DB-17、DB-1色谱柱上均获得良好分离,在0.05~1.00μg/m L范围内,农药残留量色谱分析的线性关系良好,满足定量分析要求,加标水平为0.08和0.20 mg/kg时,农药的平均回收率在71.96%~117.21%,变异系数为1.73%~12.84%。方法的检出限为0.005 3~0.011 8 mg/kg。[结论]该方法具有前处理简单、净化效果好、方法准确、灵敏度高、杂质干扰少的特点,适合火腿中有机磷农药残留量的分析。

[ Objective] A novel method for the determination of organophosphate pesticide residues in ham at the same time was established. [ Method] Organophosphate pesticide residues in ham were extracted by aeetonitrile, the liquid-liquid extraction using aeetonitrile and n-hexane as the extraction volvent was used to remove the grease and pigment and then, the solution was purified by carbon solid phase extraction column, detected by the flame photometry detector of gas chromatograph. [ Result] Experimental results showed that 16 species of organophosphate pesticides were well separated in DB-17 and DB-1. Within the scope of 0.05 to 1.00 μg/mL, pesticide residues chromatography analysis of the linear relationship was good to meet quantitative analysis requirements. The average recoveries of organic phosphorus pesticides were 71.96% - 117.21%, spiked at 0.08 and 0.20 mg/kg level. The relative standard deviations for all the compounds were 1.73 % - 12.84 %. The detection hmit of the method varied between 0. 005 3 - 0.011 8 mg/kg. [ Conclusion] The method is simple, precise, sensitive, and has a good separation effect, it can be applied to the routine analysis for organophosphate pesticide residues in ham.