QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中乙撑硫脲残留
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(广东省农业科学院农产品公共监测中心 农业部农产品质量安全检测与评价重点实验室 农业部农产品质量安全风险评估实验室(广州)

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叶倩 女 助理研究员 研究方向为农产品质量安全 E-mail:yeqian.liao@foxmail.com通信作者:┣┣(中)通信作者┫┫万凯 男 副研究员 研究方向为农产品质量安全 E-mail:149431103@qq.com

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广东省农业科学院院长基金项目(201804);广东省农业厅特色蔬菜创新团队-质量安全控制岗位专家项目(2017LM1097)


Determination of ethylenethiourea residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry
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(Key Laboratory of Testing and Evaluation for Agro-Product Safety and Quality, Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Agro-Products (Guangzhou), Ministry of Agriculture, Public Monitoring Center for Agro-Product, Guangdong Academy of Agricultural Sciences,Guangdong Guangzhou 510640, China)

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    摘要:

    目的 建立蔬菜中乙撑硫脲(ethylenethiourea,ETU)的QuEChERS-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)检测方法。方法 样品经氨水乙腈提取,石墨化碳黑净化,以Shim-pack XR-ODSIII C18色谱柱(2.0 mm×150 mm, 1.6 μm)分离待测物,采用电喷雾离子化,正离子扫描和多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。结果 乙撑硫脲在0.005~1.0 mg/L质量浓度范围内线性关系良好,相关系数均大于0.999 1;在0.010、0.10、0.50 mg/kg 3个浓度下,菜心、芹菜和叶用莴苣3种基质中乙撑硫脲的回收率为73.7%~93.3%, 相对标准偏差(RSD)为0.8%~6.6%, 检出限(LOD)为0.002~0.005 mg/kg, 方法定量限(LOQ)为添加的最低浓度0.010 mg/kg。结论 该方法简便、准确、经济、环保,能够满足蔬菜中的快速检测要求。

    Abstract:

    Objective A rapid method for determination of ethylenethiourea (ETU) residues in vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS/MS) was developed. Methods The samples were extracted with acetonitrile containing NH3H2O, and cleaned up by GCB adsorbents. The resulting samples were separated on a Shim-pack XR-ODSIII C18 column (2.0 mm×150 mm, 1.6 μm), and detected under positive polarity multiple reactions monitoring (MRM) mode. Results The matrix-matched external standard calibration curves were used for quantitative analysis. The result indicated that the line arities of ETU was in the concentration range of 0.005-1.0 mg/L with correlation coefficients higher than 0.999 1. The average recoveries of ETU in three vegetables samples at three spiked levels of 0.010,0.10 and 0.50 mg/kg were in the ranges of 73.7%-93.3%,and the relative standard deviations (RSDs) were in the range of 0.8%-6.6%, respectively. The limits of detection (LODs) for these three vegetables were in the range of 0.002-0.005 mg/kg,and the limit of quantification (LOQ) of ETU was 0.010 mg/kg which was the lowest spiked concentration. Conclusion The method was simple, accurate, economic and friendly to the environment, and could meet the requirements for rapid determination of ETU residues in vegetables.

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叶倩,黄聪灵,高毓文,冯若玮,朱富伟,万凯. QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中乙撑硫脲残留[J].中国食品卫生杂志,2018,30(4):382-386.

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  • 收稿日期:2018-04-03
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  • 在线发布日期: 2018-08-16
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