快速滤过型净化法结合高效液相色谱-串联质谱同时检测人参中的5种农药残留
投稿时间:2018-11-13      点此下载全文 HTML
引用本文:郝东宇,席兴军,初侨,等.快速滤过型净化法结合高效液相色谱-串联质谱同时检测人参中的5种农药残留[J].农药学学报,2019,21(1):82-88.
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作者单位E-mail
郝东宇 齐齐哈尔大学 化学与化学工程学院, 黑龙江 齐齐哈尔 161006
中国标准化研究院, 北京 100191 
 
席兴军 中国标准化研究院, 北京 100191  
初侨 中国标准化研究院, 北京 100191  
于聪聪 中国标准化研究院, 北京 100191  
王婷 中国标准化研究院, 北京 100191  
兰韬 中国标准化研究院, 北京 100191 lantao@cnis.gov.cn 
潘灿平 中国农业大学 理学院, 北京 100193 canpingp@cau.edu.cn 
基金项目:国家重点研发计划(2017YFF0207800);中央级公益性科研院所基本科研业务费(562017Y-5284);科技部“十三五”农药化肥减量课题(2017YFD0800701)
中文摘要:基于人参样品基质特点,采用快速滤过型净化法(m-PFC)结合高效液相色谱-串联质谱(HPLC-MS/MS),建立了人参中嘧菌酯、苯醚甲环唑、吡虫啉、茚虫威和噻嗪酮5种农药残留同时检测的分析方法。该方法具有较低的检出限(0.03~0.18 μg/kg)和定量限(0.11~0.59 μg/kg),其定量限较中国国家标准GB 2763—2016中规定的对人参中苯醚甲环唑和嘧菌酯的最大残留限量(MRL)(0.5~1 mg/kg)低3个数量级,5种农药的线性范围在1~500 μg/L之间。在2、10、50、100和300 μg/kg的添加水平下,方法的平均回收率均在76%~115%之间,相对标准偏差(RSD)均小于11%,回收率较好且方法稳定。与传统样品前处理方法相比,该方法具有操作简单、省时省力和灵敏度高等优点。将该方法应用于市售6份人参样品中5种农药残留的检测,结果未检出相应的农药残留。该方法为研发建立更快速、准确地检测人参中农药残留的方法提供了思路,也为后续中国国家标准修订人参中农药最大残留限量提供了参考。
中文关键词:快速滤过型净化 (m-PFC)  高效液相色谱-串联质谱  人参  苯醚甲环唑  嘧菌酯  多残留
 
Simultaneous detection of five pesticide residues in ginseng by multi-plug filtration cleanup method combined with high performance liquid chromatography-tandem mass spectrometry
Abstract:Based on the characteristics of ginseng samples matrix, a method for simultaneous determination of azoxystrobin, difenoconazole, imidacloprid, indoxacarb and thiazinone residues in ginseng was established by multi-plug filtration cleanup (m-PFC) method combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). A low detection limits (LOD,0.03-0.18 μg/kg) and quantitative limits (LOQ,0.11-0.59 μg/kg) were obtained. The LOQ is three orders lower than the limit for azoxystrobin (1 mg/kg) and difenoconazole (0.5 mg/kg) in ginseng in GB 2763-2016. The linear range for five pesticides can reach to 1-500 μg/L. The average recovery rate of the method was between 76% and 115%, with RSD less than 11% at the spiking levels of 2, 10, 50, 100 and 300 μg/kg. Compared with the traditional sample pretreatment method, the new method has the advantages of simple operation, time-saving, labor-saving, and high sensitivity. The method was successfully applied to the detection of five pesticides in six ginseng samples. No corresponding pesticide residues were detected. This method provides a direction for rapid and accurate detection of pesticide residues in ginseng. It also provides a reference for revising the maximum residue limits of pesticides in ginseng in the national standard.
Key words:multi-plug filtration cleanup (m-PFC)  high performance liquid chromatography-tandem mass spectrometry  ginseng  difenoconazole  azoxystrobin  multi-residues
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