摘要
采用分散固相萃取和分散液液微萃取方法,建立了气相色谱法快速检测甘蓝中氟氯氰菊酯、氯氰菊酯、溴氰菊酯及氰戊菊酯4种拟除虫菊酯农药残留量的分析方法.使用乙腈作为萃取溶剂,经乙二胺-N-丙基硅烷固相萃取吸附剂净化提取液,分散液液微萃取将农药富集到50 μL二甲苯中后,采用气相色谱-电子捕获检测器进行分析.考察了萃取溶剂的种类与体积、分散剂体积及盐效应等因素对分散液液微萃取萃取效率的影响.结果表明：除氟氯氰菊酯在0.01 ～0.1 mg/L范围外,其余3种拟除虫菊酯农药均在0.01 ～5.0mg/L范围内线性关系良好,相关系数为0.997 9～0.999 2;加标浓度为0.02～0.5 μg/g时,除氟氯氰菊酯外其他拟除虫菊酯农药的平均回收率为81.9％ ～ 93.5％,相对标准偏差为9.5％ ～ 20.7％.该方法简单、高效、重现性好、富集倍数高,可用于甘蓝中拟除虫菊酯类农药的快速检测.
A gas chromatographic method for the determination of pyrethroid pesticide residues （e.g.cyfluthrin,cypermethrin,deltamethrin and fenvalerate） in cabbage was developed using dispersive solid-phase extraction and dispersive liquid-liquid microextraction as sample preparation methods.The samples were extracted with acetonitrile,purified with primary secondary amine as sorbents,and concentrated into 50 μL dimethyl benzene by dispersive liquid-liquid microextraction.The analytes were analyzed by gas chromatography with electron capture detector.Factors affecting the extraction efficiency such as type and volume of extraction solvent,volume of dispersive solvent and salt effect,were investigated.Under the optimized conditions,the enrichment factors （EF）for four pyrethroid pesticides ranged from 100 to 297.The calibration curves were linear in the range of 0.01-0.1 mg/L for cyfluthrin,and 0.01-5 mg/L for the rest of targeted compounds,with correlation coefficients of 0.997 9-0.999 2.The limits of detection for cyfluthrin,cypermethrin,fenvalerate and deltamethrin were 0.03,0.02,0.01,0.01 μg/kg,and the limits of quantitation were 0.10,0.06,0.04,0.04 μg/kg,respectively.Except of cyfluthrin,the recoveries of other three compounds at spiked levels of 0.02-0.5 μg/g ranged from 81.9% to 93.5%,with RSDs of 9.5% -20.7%.With the advantage of quickness,low toxicity and high enrichment factors,the proposed method is applicable for the analysis of pyrethroid pesticide residues in cabbage samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第2期192-196,共5页
Journal of Instrumental Analysis
基金
北京市农林科学院青年基金项目(QNJJ201310)
北京市农林科学院创新平台项目(KJCX201103002)
关键词
分散液液微萃取
分散固相萃取
气相色谱
农药残留
甘蓝
dispersive liquid-liquid microextraction
dispersive solid-phase extraction
gas chromatography
pesticide residue
cabbage
