液相色谱串联三重四极杆复合线性离子阱质谱法测定水果和蔬菜中43种杀菌剂残留量
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(1. 沈阳市食品药品检验所,辽宁 沈阳 110136;2. 辽宁省检验检测认证中心,辽宁 沈阳 110036;3. 沈阳医学院公共卫生学院,辽宁 沈阳 110034)

作者简介:

李巧莲,女,沈阳市食品药品检验所高级工程师,硕士。

通讯作者:

王岩松(1980—),男,辽宁省检验检测认证中心正高级工程师,博士。E-mail:121811342@qq.com

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基金项目:

沈阳市科学技术局科技计划项目(编号:22-322-3-37);辽宁省市场监督管理局科技计划项目(编号:2022ZC023)


Simultaneous determination of 43 kinds of fungicides in fruits and vegetables by high performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry
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(1. Shenyang Food and Drug Inspection, Shenyang, Liaoning 110136, China;2. Liaoning Inspection, Examination & Certification Centre, Shenyang, Liaoning 110036, China;3. School of Public Health, Shenyang Medical College, Shenyang, Liaoning 110034, China)

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    摘要:

    [目的]实现蔬菜、水果中多种杀菌剂残留的同时测定。[方法]建立液相色谱串联三重四极杆复合线性离子阱质谱法(LC-QTRAP-MS/MS)同时测定水果和蔬菜中多种杀菌剂残留量。样品以含0.1%乙酸的乙腈溶液为溶剂,乙酸钠和无水硫酸镁进行盐析,使用无水硫酸镁、乙二胺-N-丙基硅烷化硅胶(PSA)、十八烷基硅烷键合硅胶(HC-C18)、多壁碳纳米管(MWCNTs)进行净化处理,质谱采用增强子离子扫描模式(MRM-IDA-EPI)及谱库检索技术,通过对化合物保留时间、离子对及EPI谱库检索对比,外标法定量。[结果]43种杀菌剂在0.2~5.0,2.5~50.0 μg/L质量浓度范围内线性关系良好(R2>0.99);方法检出限为0.1~5.0 μg/kg,定量限为0.4~10.0 μg/kg;在3个质量浓度添加水平下,43种杀菌剂的回收率为65.1%~119.8%,相对标准偏差为0.8%~13.0%。[结论]该方法适用于水果和蔬菜中43种杀菌剂的筛查确证和定量检测。

    Abstract:

    [Objective] This study aims to realize the simultaneous determination of fungicide residues in vegetables and fruits. [Methods] A liquid chromatography-tandem quadrupole composite linear ion TRAP-mass spectrometry (LC-QTRAP-MS/MS) method was established for the simultaneous determination of fungicide residues in fruits and vegetables. The samples were salted out with sodium acetate and anhydrous magnesium sulfate in an acetonitrile solution containing 0.1% acetic acid, magnesium sulfate, ethylenediamine-n-propyl silanized silica gel (PSA), octadecylsilane bonded silica gel (HC-C18) and multi-walled carbon nanotubes (MWCNTs) were used for purification. Mass spectrometry was conducted utilizing the enhanced ion scanning mode (MRM-IDA-EPI) and spectral library retrieval technology. The compounds were quantified using an external standard approach, comparing the retention time, ion pairs, and EPI spectral library retrieval. [Results] The 43 kinds of fungicides had a good linear relationship in the mass concentration range of 0.2~5.0 μg/L and 2.5~50.0 μg/L (R2>0.99). The limit of detection (LOD) was 0.1~5.0 μg/kg, and the limit of quantification (LOQ) was 0.4~10.0 μg/kg. The recoveries of the 43 kinds of fungicides were 65.1%~119.8% at three concentration levels, and the relative standard deviations were 0.8%~13.0%. [Conclusion] The established method is rapid, simple, and highly qualitative, and can be used for the screening, confirming and quantitative detection of 43 kinds of fungicides in fruits and vegetables.

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李巧莲,王岩松,罗景阳,等.液相色谱串联三重四极杆复合线性离子阱质谱法测定水果和蔬菜中43种杀菌剂残留量[J].食品与机械,2024,40(7):53-62.
LI Qiaolian, WANG Yansong, LUO Jingyang, et al. Simultaneous determination of 43 kinds of fungicides in fruits and vegetables by high performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry[J]. Food & Machinery,2024,40(7):53-62.

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  • 收稿日期:2023-09-14
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  • 在线发布日期: 2024-09-12
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