QuEChERS-LC-MS/MS测定芹菜中吡虫啉和唑螨酯

doi:10.3969/j.issn.1004-1524.2018.02.12

浙江农业学报 ›› 2018, Vol. 30 ›› Issue (2): 261-267.DOI: 10.3969/j.issn.1004-1524.2018.02.12

QuEChERS-LC-MS/MS测定芹菜中吡虫啉和唑螨酯

刘英^{1, 2}, 李韵之², 陈列忠², 王彦华², 许振岚², 蒋金花², 汤涛², 陈文学¹, 王强^{1, 2, *}, 张昌朋^{2, *}

1.海南大学食品学院,海南海口 570228;
2.浙江省农业科学院农产品质量标准研究所,省部共建国家重点实验室培育基地——浙江省植物有害生物防控重点实验室,农业部农药残留检测重点实验室,浙江杭州 310021

收稿日期:2017-05-18 出版日期:2018-02-20 发布日期:2018-02-11
通讯作者: 王强,E-mail:qiangwang_zaas@163.com;张昌朋,E-mail:cpzhang1215@126.com
作者简介:刘英(1992—),女,江西吉安人,硕士研究生,研究方向为食品质量与安全。E-mail:2269521979@qq.com
基金资助:
国家重点研发项目子课题(2016YFD0200204-4); 公益性行业(农业)科研专项经费项目(201503107-12)

Determination of imidacloprid and fenpyroximate in celery by QuEChERS-LC-MS/MS

LIU Ying^{1, 2}, LI Yunzhi², CHEN Liezhong², WANG Yanhua², XU Zhenlan², JIANG Jinhua², TANG Tao², CHEN Wenxue¹, WANG Qiang^{1, 2, *}, ZHANG Changpeng^{2, *}

1. College of Food Science and Technology, Hainan University, Haikou 570228, China;
2. State Key Lab Breeding Base for Zhejiang Sustainable Plant Pest Control, MOA Key Lab for Pesticide Residue Detection, Institute of Quality and Standard for Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2017-05-18 Online:2018-02-20 Published:2018-02-11

摘要/Abstract

摘要： 为建立芹菜根、茎、叶中吡虫啉、唑螨酯残留的QuEChERS-LC-MS/MS分析方法,采用QuEChERS方法对样品进行提取和净化,通过液相色谱-串联三重四极杆质谱联用仪(LC-MS/MS)测定样品中吡虫啉、唑螨酯残留。结果表明:添加质量分数为0.05~1.00 mg·kg^-1时,吡虫啉在芹菜根、茎、叶中的平均添加回收率为77.15%~103.48%,RSDs为1.40%~9.97%;唑螨酯在芹菜根、茎、叶中的平均添加回收率为77.35%~100.42%,RSDs为2.01%~6.95%。吡虫啉、唑螨酯的检出限(LODs)分别是0.120、0.015 μg·kg^-1;吡虫啉在芹菜根、茎、叶的定量限(LOQs)分别为1.65、0.87、1.08 μg·kg^-1;唑螨酯在芹菜根、茎、叶的LOQs分别是1.24、0.75、0.78 μg·kg^-1。该方法操作简单,回收率、精密度均符合农药残留分析的要求,适合实验室大量样品的检测。

关键词: 芹菜, 吡虫啉, 唑螨酯, QuEChERS, 液相色谱-串联三重四极杆质谱联用仪

Abstract: In this study, a simple and practical QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established to detect the residues of imidacloprid and fenpyroximate in the roots, stems, leaves of celery. The samples were extracted and purified by QuEChERS method, and analyzed by LC-MS/MS. Results showed that the average recoveries of imidacloprid in roots, stems, leaves of celery were 77.15%-103.48% at three spiking levels from 0.05 mg·kg^-1 to 1.00 mg·kg^-1 with relative standard deviations (RSDs) of 1.40%-9.97%. The average recoveries of fenpyroximate in roots, stems, leaves of celery were 77.35%-100.42% at three spiking levels from 0.05 mg·kg^-1 to 1.00 mg·kg^-1 with relative standard deviations (RSDs) of 2.01%-6.95%. Limit of detections (LODs) were estimated to be 0.120 μg·kg^-1 for imidacloprid, and 0.015 μg·kg^-1 for fenpyroximate, respectively. Limit of quantitations (LOQs) for imidacloprid in the roots, stems, leaves of celery were 1.65, 0.87 and 1.08 μg·kg^-1, respectively. LOQs for fenpyroximate were 1.24 μg·kg^-1 (roots), 0.75 μg·kg^-1 (stems) and 0.78 μg·kg^-1 (leaves). The celery samples were detected using this established method, the recovery and the precision were in accordance with the requirements of pesticide residue analysis. The method was suitable for the detection of a large number of samples in the laboratory.

Key words: celery, imidacloprid, fenpyroximate, QuEChERS, liquid chromatography-tandem mass spectrometry

中图分类号:

S481⁺.8

刘英, 李韵之, 陈列忠, 王彦华, 许振岚, 蒋金花, 汤涛, 陈文学, 王强, 张昌朋. QuEChERS-LC-MS/MS测定芹菜中吡虫啉和唑螨酯[J]. 浙江农业学报, 2018, 30(2): 261-267.

LIU Ying, LI Yunzhi, CHEN Liezhong, WANG Yanhua, XU Zhenlan, JIANG Jinhua, TANG Tao, CHEN Wenxue, WANG Qiang, ZHANG Changpeng. Determination of imidacloprid and fenpyroximate in celery by QuEChERS-LC-MS/MS[J]. , 2018, 30(2): 261-267.

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QuEChERS-LC-MS/MS测定芹菜中吡虫啉和唑螨酯

Determination of imidacloprid and fenpyroximate in celery by QuEChERS-LC-MS/MS

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