蔬菜中11种有机磷农药残留的气相色谱检测及其对蔬菜基质的影响  

Determination of 11 Organophosphorus Pesticide Residues in Vegetables by Gas Chromatography and Its Effect on Matrix

作　　者：吴晖[1] 朱珍[1] 风华亮[1] 李晓凤[1] 

机构地区：[1]华南理工大学轻工与食品学院,广东广州510640

出　　处：《食品科学》2011年第6期198-203,共6页Food Science

基　　金：教育部"新世纪优秀人才支持计划"项目(NCET-060746);教育部高校博士点基金项目(200805611022);华南理工大学"SRP"项目(Y1090250)

摘　　要：建立蔬菜中11种农药多残留的气相色谱分析方法。对NY/T 761—2008《蔬菜和水果中有机磷、有机氮、拟除虫菊酯和氨基甲酸酯类农药多残留的测定》标准的蔬菜前处理方法进行改进,并探讨蔬菜基质对检测的影响。使用DB-17毛细管柱分离,FPD检测器进行检测。结果显示:11种有机磷农药分离效果好,在黄瓜、西红柿、生姜中的3个添加水平,回收率为71.2%～117.9%,相对标准偏差(RSD)为2.1%～11.2%,最低检出限为0.005～0.060mg/kg,保留时间为6.396～19.400min。在各自线性范围内线性关系好(r>0.999);使用40℃加热氮吹浓缩,可分别提高敌敌畏、甲拌磷回收率至95.00%和103.30%;在被测的13种蔬菜中,甘蓝、娃娃菜、上海青有少量杂峰影响农药检出;韭菜有大量的基质峰干扰农药检出。In order to establish a gas chromatography method for 11 kinds of pesticide residues in vegetables,the pre-treatment method for vegetables according to the standard of NY/T 761-2008 entitled Determination of organic phosphorus,organic nitrogen,pyrethroid and carbamate pesticide residues in fruits and vegetables was modified.Meanwhile,the effect of vegetable matrix on determination efficiency of pesticide residues was explored.During the determination of pesticide residues,DB-17 capillary separation column and flame photometric detector（FPD） were used.The results indicated that 11 organophosphorus pesticide residues could be effectively separated.The recovery rates of 11 pesticides in cucumber,tomato and ginger with three spiked levels were in the range of 71.2%-117.9%.The relative standard deviation（RSD） was in the range of 2.1% to 11.2%.The detection limit of this method was 0.005-0.060 mg/kg for DB-17 column,and the retention time was 6.396-19.400 min.The calibration curves revealed a good linear relationship with correlation coefficients of more than 0.999.Under the heating at 40 ℃ by N2,the recovery rates of dichlorovos and phorate could be enhanced up to 95.00%-103.3%,respectively.A small amount of impure peaks in cabbage,baby vegetables and Shanghai green,and a large number of matrix peaks in garlic chive could interfere with the detection of pesticide residues.

关 键 词：气相色谱(GC) 有机磷农药残留 蔬菜 基质 

分 类 号：O657.7[理学—分析化学] TS207.5[理学—化学]