气相色谱-质谱法测定果蔬中四氯虫酰胺和腈吡螨酯  

Determination of SYP 9080 and cyenopyrafen residues in fruits and vegetables by GC-MS

作　　者：崔淑华[1] 郭庆龙 王英华 张谦 刘宏玉 张晓梅[1] 张鸿伟[1] CUI Shu-hua;GUO Qing-long;WANG Ying-hua;ZHANG Qian;LIU Hong-yu;ZHANG Xiao-mei;ZHANG Hong-wei(Inspection and Quarantine Technology Center of Shandong Exit/Entry Inspection and Quarantine Bureau, Qingdao 266002;Huangdao Customs, Qingdao 266555)

机构地区：[1]山东出入境检验检疫局检验检疫技术中心,青岛266002 [2]黄岛海关,青岛266555

出　　处：《分析试验室》2019年第6期670-674,共5页Chinese Journal of Analysis Laboratory

基　　金：山东出入境检验检疫科研项目(SK201425);青岛市民生科技计划(18-6-1-107-nsh)项目资助

摘　　要：建立了蔬菜和水果中腈吡螨酯和四氯虫酰胺残留量的气相色谱-电子轰击离子源质谱(GC-EI-MS)分析方法。用乙腈均质提取果蔬样品中残留农药,提取液经乙二胺-N-丙基硅烷(PSA)和十八烷基硅烷(C18)基质分散净化,将净化液浓缩转溶后GC-EI-MS定性和定量分析。结果表明,腈吡螨酯在2. 0~200μg/L、四氯虫酰胺在5. 0~200μg/L范围内质量浓度与其对应的峰面积线性关系良好,相关系数均大于0. 9990。在苹果、葡萄、菠菜和洋葱样品中对腈吡螨酯进行0. 0010~2. 0 mg/kg、四氯虫酰胺进行0. 0050~2. 0 mg/kg的加标回收率实验,平均回收率为79. 9%~100. 2%,相对标准偏差为4. 3%~9. 4%,腈吡螨酯和四氯虫酰胺的方法检出限分别为0. 15μg/kg和0. 62μg/kg,定量限分别为1. 0μg/kg和5. 0μg/kg。方法已用于蔬菜和水果中四氯虫酰胺和腈吡螨酯残留检测。A method based on gas chromatography electron impact ion source mass spectrometry( GCEI-MS) was developed for the determination of SYP 9080 and cyenopyrafen residues in fruits and vegetables. The analytes were extracted from the samples using acetonitrile,purified by C18 and PSA as dispersion solid phase extration,then analyzed by GC-EI-MS. The linear ranges of cyenopyrafen and SYP 9080 in different matrices ranged from 2. 00 μg/L to 200 μg/L and 5. 00 μg/L to 200 μg/L,with correlation coefficients of not less than 0. 9990. The recoveries of cyenopyrafen from cucumber,grape,apple and onionsaples at spiked levels of 0. 0010-2. 0 mg/kg and SYP 9080 at spiked levels of0. 0050-2. 0 mg/kg were in the range of 79. 9%-100. 2%,with relative standard deviations( RSDs) of 4. 3%-9. 4%. The limits of detection were 0. 15 μg/kg and 0. 62 μg/kg,the limits of quantification were 1. 0 μg/kg and 5. 0 μg/kg for SYP 9080 and cyenopyrafen,respectively.

关 键 词：气相色谱-电子轰击离子源质谱法(GC-EI-MS) 果蔬 四氯虫酰胺 腈吡螨酯 残留量 

分 类 号：TS207.5[轻工技术与工程—食品科学]