色谱

色谱 ›› 2019, Vol. 37 ›› Issue (7): 729-734.DOI: 10.3724/SP.J.1123.2019.01026

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定稻田水产品中毒死蜱残留

彭婕1, 甘金华1,2, 居小倩1, 陈建武1, 何力1,2   

  1. 1. 中国水产科学研究院长江水产研究所, 农业农村部淡水鱼类种质监督检验测试中心, 农业农村部水产品质量安全风险评估实验室(武汉), 湖北 武汉 430223;
    2. 农业农村部水产品质量安全控制实验室, 北京 100141
  • 收稿日期:2019-01-21 出版日期:2019-07-08 发布日期:2015-05-21
  • 通讯作者: 何力.Tel:(027)81780268,E-mail:1170746090@qq.com.
  • 基金资助:
    中国水产科学研究院基本科研业务费（2018HY-ZD0603）；国家农产品质量安全风险评估项目（GJFP201800902）.

Determination of chlorpyrifos residues in the paddy field aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

PENG Jie1, GAN Jinhua1,2, JU Xiaoqian1, CHEN Jianwu1, HE Li1,2   

  1. 1. Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Fishery Quality Supervision and Testing Center, Ministry of Agriculture and Rural Affairs of the P. R. China, Fishery Products Quality Safety Risk Assessment Laboratory(Wuhan) of Ministry of Agriculture and Rural Affairs of the P. R. China, Wuhan 430223, China;
    2. Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs of the P. R. China, Beijing 100141, China
  • Received:2019-01-21 Online:2019-07-08 Published:2015-05-21
  • Supported by:
    Central Public-Interest Scientific Institution Basal Research Fund, Chinese Academy of Fishery Sciences (CAFS) (No. 2018HY-ZD0603); National Agricultural Product Quality Safety Risk Assessment Project (No. GJFP201800902).

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摘要： 以QuEChERS作为样品前处理手段，采用超高效液相色谱-串联质谱（UPLC-MS/MS）检测技术，建立了稻田水产品中毒死蜱残留的检测方法。样品经乙腈提取，由0.2 g乙二胺-N-丙基硅烷（PSA）和1.2 g无水硫酸镁分散萃取净化，采用Hypersil GOLD C18色谱柱（100 mm×2.1 mm，5 μm）进行分离，用加热大气压电喷雾电离源、正离子模式进行扫描，在选择反应监测模式下检测，基质匹配标准曲线外标法定量。结果表明，毒死蜱在0.5~100.0 μg/L范围内线性关系良好，相关系数大于0.999；毒死蜱的加标回收率为86.2%~103.6%，相对标准偏差为3.5%~7.6%（n=6），检出限为0.25 μg/kg，定量限为0.5 μg/kg。该方法简单、快速、灵敏，能够满足稻田水产品中毒死蜱残留的检测需求。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 稻田水产品, 毒死蜱

Abstract: A method was developed for the determination of chlorpyrifos residues in paddy field aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with acetonitrile and purified by using 0.2 g primary secondary amine (PSA) sorbent and 1.2 g MgSO4. The target compound was separated on a Hypersil GOLD C18 column (100 mm×2.1 mm, 5 μm), and was determined using a heated electrospray ionization (HESI) source in the positive ion selective reaction monitoring (SRM) mode. The analyte was quantified with external standard using the matrix-matched standard calibration curve method. The results showed that good linearities were obtained in the range of 0.5-100.0 μg/L, and the correlation coefficients were greater than 0.999. The spiked recoveries of chlorpyrifos ranged from 86.2% to 103.6% with RSDs of 3.5%-7.6% (n=6). The limits of detection and quantification were 0.25 μg/kg and 0.5 μg/kg, respectively. This method is simple, quick, sensitive, and suitable for the rapid determination and analysis of chlorpyrifos residues in paddy field aquatic products.

Key words: chlorpyrifos, paddy field aquatic products, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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