微型固相萃取柱结合胃袋式大体积进样-气相色谱-质谱法对食品中205种农药残留快速测定研究

Rapid Determination of 205 Pesticide Residues in Foods by Stomach Large Volume Injection-Gas Chromatography-Mass Spectrometry with Mini Solid Phase Extraction

分别选取菠菜、洋白菜、苹果、大米和大豆5种基质，利用微型固相萃取柱对样品进行前处理，采用胃袋式大体积进样技术结合气相色谱-质谱（GC-MS），建立了同时测定13本通关检测项目要求的205种农药残留的快速分析方法。通过增加进样量提高检测灵敏度，通过减少样品处理量缩短前处理时间，以保留时间和特征离子丰度比进行定性，以特征离子强度进行定量。该方法与日本通知法进行了比对，结果表明两种方法净化效果、检出限、回收率和RSD等指标水平相当，平均回收率在80％-120％之间，RSD（n=7）小于10％，满足残留分析方法的要求。

A large volume injection-gas chromatography- mass spectrometry （LVI -GC -MS ） method for the determination of 205 pesticide residues in spinach, cabbage, apple, rice and bean samples was developed. Pesticides were determined by GC - MS under the selective-ion monitoring （SIM） mode and identified by their retention times and characteristic ions. This method is equivalent to the Japanese Standard Method in terms of detecting levels and purifying effects. Over 95% of the compounds have mean recoveries of 80%-120% , and the RSD （n =7） is less than 10%.