固相萃取_双柱双检测器_气相色谱法同时测定蔬菜中多种类农药残留.docx

·化学测定方法·固相萃取 － 双柱双检测器 － 气相色谱法同时测定 蔬菜中多种类农药残留胡浩军，黄方取金华市疾病预防控制中心，浙江 金华 321000摘要: 目的 建立蔬菜中三大类农药的固相萃取 － 双柱双检测器 － 同一升温程序下气相色谱同时测定法。方法 样 品经乙腈溶剂匀浆提取，Carb － NH2 柱净化，样品间隔 60 s 进样 2 次，先经 CP － Sil 5CB 柱分离后进入 NPD 检测器进行 有机磷和氨基甲酸酯类农药测定，然后经 CP － Sil 24CB 柱分离后进入 ECD 检测器进行有机氯和拟除虫菊酯测定，阳性样品双柱检测器端互换双柱验证。结果 三大类农药在 0． 01 μg / ml ～ 2． 0 μg / ml 范围内质量浓度与峰面积有良好的线 性关系，方法检测限在 0． 0001 mg / kg ～ 0． 010 mg / kg，加标回收率在 76% ～ 124% 之间，相对标准偏差( ＲSD) 在 0． 95% ～ 4． 7% 。结论 该方法简便、快速，结果准确，能满足蔬菜中多种类农药残留同时分析的要求。关键词: 固相萃取; 双柱双检测器; 气相色谱; 多种类农药残留中图分类号: O657． 7 + 1 文献标识码: A 文章编号: 1004 － 8685( 2014) 03 － 0324 － 04Simultaneous determination of multiple pesticides residues in vegetables by solid phase extraction － double columns and doubledetectors － gas chromatographyHU Hao － jun，HUANG Fang － quJinhua District Center for Disease Control and Prevention，Jinhua 321000，ChinaAbstract: Objective To establish a method for simultaneous detection of three categories of pesticide residues in vegetables by SPE － dual column － dual detector － gas chromatography under the same temperature program． Methods The samples were extracted by acetonitrile，purified with Carb － NH2 SPE column and injected twice with interval of 60 s for determination of or- ganophosphorus and carbamate pesticides by CP － Sil 5CB － NPD，organochlorine and pyrethroid by CP － Sil 24CB － ECD re- spectively． The positive samples were determined again by interchangeable column． Ｒesults The three large categories of pes- ticides showed good linearity in the range of 0． 01 μg / ml ～ 2． 0 μg / ml，the detection limit was 0． 0001 mg / kg ～ 0． 010 mg / kg， the recovery rate ranged from 76% to 124% ，and the relative standard deviation varied between 0． 95% and 4． 7% ． Conclu- sion This method is simple，rapid and accurate，it can meet the analysis requirements of many kinds of pesticide residues in vegetables．Key Words: Solid phase extraction; Double columns and double detectors; Gas chromatography; Multiple pesticides residues有机氯、有机磷、氨基甲酸酯类和拟除虫菊酯类