分散固相萃取-气相色谱法快速测定食用植物油中66种农药残留

建立分散固相萃取法结合气相色谱技术同时快速测定食用植物油中有机磷、有机氯和拟除虫菊酯66种农药残留的方法。样品经乙腈溶剂3次提取后,使用PSA(Primary secondary Amine,N-丙基乙二胺)和C18分散固相萃取净化,提取溶液经氮吹浓缩过滤后一部分注入气相色谱-电子捕获检测器检测,另一部分经气相色谱-火焰光度检测器检测。样品在0.08、0.16和0.40 mg/kg添加水平的回收率试验中,平均回收率为62.3%~112.3%,相对标准偏差不大于8.6%,检出限在0.001~0.018 mg/kg之间,基本满足国内外对食用植物油中农药最低残留限量的标准要求。

Rapid Determination of 66 Pesticides Residues in Edible Vegetable Oil by Dispersive Solid Phase Extraction Method-Gas ChromatographyS

A method was established for the quick determination of 66 organophosphorus, organochlorine and pyrethroid pesticides residues in edible vegetable oil, samples were purified by dispersive solid phase extraction method and detected by gas chromatography (with FPD/ECD detector). Samples were extracted by acetonitrile for three times, and purified by PSA and C18 using dispersive solid phase extraction method. After nitrogen flushing concentration and filtration, samples were detected by GC-FPD and GC-ECD. At the fortification level of 0.08 mg/kg, 0.16 mg/kg and 0.40 mg/kg, the average recoveries ranged from 62.3% to 112.3%, and the relative standard deviations (RSDs, n=6) were less than 8.6%, limit of detections (LODs) were 0.001 mg/kg~0.018 mg/kg, this method can basically meet the standard request of peptide residue MRLs in edible vegetable oil at home and abroad.