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中国农学通报 ›› 2021, Vol. 37 ›› Issue (35): 110-117.doi: 10.11924/j.issn.1000-6850.casb2021-0684

所属专题: 植物保护

• 食品·营养·检测·安全 • 上一篇    下一篇

改良QuEChERS方法结合气相色谱测定红甜菜中20种农药残留

刘琳1(), 马腾飞1, 贾孙悦2, 周芹1,3,4(), 王皙玮1,3,4()   

  1. 1黑龙江大学现代农业与生态环境学院,哈尔滨 150080
    2黑龙江大学化学化工与材料学院,哈尔滨 150080
    3农业农村部甜菜品质监督检验测试中心,哈尔滨150080
    4农业农村部糖料产品质量安全风险评估实验室,哈尔滨 150080
  • 收稿日期:2021-07-09 修回日期:2021-09-30 出版日期:2021-12-15 发布日期:2022-01-07
  • 通讯作者: 周芹,王皙玮
  • 作者简介:刘琳,女,1997年出生,河南信阳人,硕士研究生,主要从事农产品质量检验方面的工作。通信地址:150080 哈尔滨市南岗区学府路74号 黑龙江大学农学楼223,E-mail: liulin_1217@163.com
  • 基金资助:
    现代农业产业技术体系建设专项资金“质量安全与营养品质评价”(CARS-170503);黑龙江省高校基本科研业务经费(KJCX201919)

Determination of 20 Pesticide Residues in Red Beet by Modified QuEChERS Method Combined with Gas Chromatography

Liu Lin1(), Ma Tengfei1, Jia Sunyue2, Zhou Qin1,3,4(), Wang Xiwei1,3,4()   

  1. 1Modern Agriculture and the Ecological Environment Academy of Heilongjiang University, Harbin 150080
    2School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080
    3Beet Quality Supervision, Inspection and Test Center Ministry of Agriculture and Rural Affairs, Harbin 150080
    4Laboratory of Quality & Safety Risk Assessment for Sugar Crops Products, Ministry of Agriculture and Rural Affairs, Harbin 150080;
  • Received:2021-07-09 Revised:2021-09-30 Online:2021-12-15 Published:2022-01-07
  • Contact: Zhou Qin,Wang Xiwei

摘要:

建立了改良的QuEChERS法结合气相色谱-电子捕获检测器用于红甜菜中20种农药残留的联合测定方法。样品中农药残留以乙腈作为提取溶剂,多壁碳纳米管分散固相萃取去除杂质,过滤后经RTX-1色谱柱分离,GC-ECD检测,外标法定量。探讨了气相色谱的程序升温条件,考察了不同提取溶剂及不同的净化方法对检测结果的影响。结果表明:在优化的色谱条件下,20种农药在0.01~0.50 mg/L(莠去津为0.03~0.50 mg/L)范围内线性关系良好,相关系数(R2)均大于0.99,并且得到很好的分离;乙腈与样品的比例为1:2,多壁碳纳米管用量为10 mg的前处理条件下,红甜菜样品在3个浓度的平均回收率为62.0%~116.5%之间,相对标准偏差为1.9%~10.9%,检出限为0.12 µg/L~0.063 mg/L,定量限为0.4 µg/L~0.21 mg/L。该方法操作简单、快速、准确,适用于红甜菜中有机氯及拟除虫菊酯类多农药残留的检测。

关键词: QuEChERS, 气相色谱, 多壁碳纳米管, 红甜菜, 农药残留

Abstract:

A method was developed to determine 20 pesticide residues in red beet by modified QuEChERS method combined with gas chromatography-electron capture detector. The pesticide residues in the samples were extracted by acetonitrile and cleaned up by dispersive solid-phase extraction using MWCNTs, after filtration, they were separated on RTX-1 chromatographic column, determined by gas chromatography, and quantified by the external standard method. The temperature-programmed conditions of gas chromatography were tested, and the effects of different extraction solvents and purification methods on the detection results were investigated. The results showed that under the optimized conditions, good linear relations were obtained in the range of 0.01-0.50 mg/L (Atrazine was in the range of 0.03-0.50 mg/L), the correlation coefficients (R2) were all higher than 0.99, and 20 pesticides were well separated. The pre-treatment condition was as follow: acetonitrile: sample was 2:1, and the amount of MWCNTs was 10 mg. The average recoveries of red beet were 62.0%-116.5% at three spiked concentration levels with relative standard deviations (RSDs) of 1.9%-10.9%, the limits of detection were 0.12 μg/L - 0.063 mg/L, and the limits of quantitation were 0.4 μg/L - 0.21 mg/L. This method is simple, rapid, accurate, and could be used for the determination of organochlorine and pyrethroid residues in red beet.

Key words: QuEChERS, gas chromatography, multi-walled carbon nanotubes, red beet, pesticide residue

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