超临界色谱串联静电场轨道阱质谱法测定蔬菜水果中高极性农药残留
作者:
作者单位:

上海市疾病预防控制中心,上海 200336

作者简介:

徐骞 男 技师 研究方向为农药残留分析 E-mail: xuqian@scdc.sh.cn

通讯作者:

金玉娥 女 副主任技师 研究方向为痕量有机污染物分析 E­mail: jinyue@scdc.sh.cn

中图分类号:

R155

基金项目:

国家重点研发计划(2017YFC1601300);上海市科学技术委员会项目(19142201900);食品司安全风险预测预警项目


Determination of polar pesticide residues in vegetable and fruit by supercritical fluid chromatography­Q­Orbitrap
Author:
Affiliation:

Shanghai Municipal Center for Disease Control and Prevention, Shanghai 200336, China

Fund Project:

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    摘要:

    目的 建立基于超临界色谱技术(SFC)结合静电场轨道阱质谱法(Q-Orbitrap)对蔬菜水果中12种高极性农药残留量的测定方法。方法 样品用1%酸化甲醇提取,提取液经分散固相萃取净化,以Ultra Silica柱(150 mm×2.1 mm, 3 μm)和Obelisc R柱(150 mm×2.1 mm, 5 μm)为分离柱,使用超临界色谱-串联静电场轨道阱质谱(SFC-Q-Orbitrap)测定,以分段式混合产物离子扫描,采用同位素内标校准曲线定量。结果 12种农药在20.0~500 μg/L范围内线性关系良好,决定系数(R2)均>0.997,在0.05、0.20 mg/kg 2个加标浓度下的平均回收率为80.2%~120%,相对标准偏差(RSD,n=6)为2.14%~14.6%,方法的检出限为0.010 1~0.016 2 mg/kg,定量下限为0.050 mg/kg。结论 方法具有操作简单、专一性强、定量准确、测定高效等优点,经实际样品测试,可满足蔬菜水果中高极性农药残留的检测。

    Abstract:

    Objective To establish a method for determination of 12 polar pesticide residues in vegetables and fruits by supercritical fluid chromatography-Q-Orbitrap (SFC-Q-Orbitrap).Methods The samples were extracted with 1% acidified methanol,and the extract was purified by dispersed solid phase extraction, separated by ultra silica column (150 mm× 2.1 mm, 3 μm) and obelisc r column (150 mm× 2.1 mm, 5 μm), determined by SFC-Q-Orbitrap, scanned by segmented mixed product ions, and quantified by isotope internal standard calibration curve.Results The calibration curves for 12 pesticides exhibited good linearity in the range of 20.0-500 μg/L, with the correlation coefficients(R2) above 0.997. The average recoveries at 0.05 and 0.20 mg/kg spiked levels were in the range of 80.2%-120% and the relative standard deviations (RSD,n=6) were in the range of 2.14%-14.6%. The limits of detection and the limits of quantification were 0.010 1-0.016 2 mg/kg and 0.050 mg/kg.Conclusion The method has the advantages of simple operation, accurate quantification and high efficiency. It can meet the requirements determination of high polar pesticide residues in vegetables and fruits.

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徐骞,卢大胜,邱歆磊,冯超,林元杰,乐孙阳,陈宇航,金玉娥.超临界色谱串联静电场轨道阱质谱法测定蔬菜水果中高极性农药残留[J].中国食品卫生杂志,2022,34(2):254-261.

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  • 收稿日期:2021-09-30
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  • 在线发布日期: 2022-05-18
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