色谱

色谱 ›› 2020, Vol. 38 ›› Issue (5): 611-616.DOI: 10.3724/SP.J.1123.2019.10009

• 技术与应用 • 上一篇    下一篇

高效液相色谱-三重四极杆质谱法测定克氏原鳌虾中多菌灵残留

李亚梦1,2, 甘金华3, 李晋成2, 吴立冬2, 李芹1,2, 肖雨诗1,2, 彭婕3, 陈建武3, 刘欢2,*()   

  1. 1 上海海洋大学水产与生命学院, 上海 201306
    2 中国水产科学研究院, 农业农村部水产品质量安全控制重点实验室, 北京 100141
    3 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
  • 收稿日期:2019-10-11 出版日期:2020-05-08 发布日期:2020-12-10
  • 通讯作者: 刘欢
  • 作者简介:刘欢.Tel:01068690728, E-mail:Liuh@cafs.ac.cn
  • 基金资助:
    中国水产研究院基本科研业务费(2018HY-ZD0607);现代农业产业技术体系建设专项资金(CARS-48)

Determination of carbendazim residues in Procambarus clarkii by high performance liquid chromatography-triple quadrupole mass spectrometry

LI Yameng1,2, GAN Jinhua3, LI Jincheng2, WU Lidong2, LI Qin1,2, XIAO Yushi1,2, PENG Jie3, CHEN Jianwu3, LIU Huan2,*()   

  1. 1 College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, China
    2 Key Laboratory of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, Chinese Academy of Fishery Sciences, Beijing 100141, China
    3 Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Fishery Quality Supervision and Testing Center, Ministry of Agriculture and Rural Affairs, Fishery Products Quality Safety Risk Assessment Laboratory(Wuhan) of Ministry of Agriculture and Rural Affairs, Wuhan 430223, China
  • Received:2019-10-11 Online:2020-05-08 Published:2020-12-10
  • Contact: LIU Huan
  • Supported by:
    Central Public-Interest Scientific Institution Basal Research Fund, Chinese Academy of Fishery Sciences (CAFS)(2018HY-ZD0607);China Agriculture Research System-48(CARS-48)

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摘要：

建立了高效液相色谱-三重四极杆质谱测定克氏原鳌虾中多菌灵的新方法。样品在碱性条件下经乙酸乙酯提取，离心，上清液经旋转蒸发浓缩并复溶后采用混合型阳离子（MCX）萃取小柱富集净化。以乙腈和水为流动相，采用C18色谱柱进行梯度洗脱分离。在电喷雾正离子源下，采用多反应监测模式检测。结果表明：多菌灵在0.5~50.0 μg/L范围内线性关系良好，相关系数（r2）为0.9985。多菌灵的检出限和定量限分别为0.25 μg/kg和0.50 μg/kg。当加标水平为0.5、1.0、5.0和50.0 μg/kg时，加标回收率为83.9%~105.5%，相对标准偏差为1.1%~3.2%（n=6）。该方法能简单、有效地检测出克氏原鳌虾中多菌灵的残留量，且稳定性好，结果可靠。

关键词: 固相萃取, 高效液相色谱-串联质谱法, 多菌灵, 克氏原螯虾

Abstract:

A novel method based on high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was established for the determination of carbendazim in Procambarus clarkii. The sample was extracted by ethyl acetate under alkaline conditions and centrifuged. The supernatant was concentrated by rotary evaporation, redissolved, and then enriched and purified on a mixed-mode cation exchange solid phase extraction column (MCX). A C18 column was used with acetonitrile and water as mobile phases in a gradient elution. Ionization was performed using an electrospray positive ion source (ESI+), and detection was achieved by MS/MS in multiple reaction monitoring (MRM) mode. The linearity for carbendazim was good in the range of 0.5-50.0 μg/L; the linear equation was y=0.19988x+0.01842; and the correlation coefficient (r2) was 0.9985. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 μg/kg and 0.50 μg/kg, respectively. At spiked levels of 0.5, 1.0, 5.0, and 50.0 μg/kg, the recoveries ranged from 83.9% to 105.5%, and the relative standard deviation ranged from 1.1% to 3.2%. This method is simple and effective for the determination of carbendazim residues in P. clarkii.

Key words: solid phase extraction (SPE), high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), carbendazim, Procambarus clarkii