色谱 ›› 2018, Vol. 36 ›› Issue (6): 552-556.DOI: 10.3724/SP.J.1123.2018.01008

• 研究论文 • 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螯虾中二甲戊灵残留

杨秋红1,2, 刘欢2, 邹谱心3, 戚铭隆3, 刘永涛1,2, 艾晓辉1,2   

  1. 1. 中国水产科学研究院长江水产研究所, 湖北 武汉 430223;
    2. 中国水产科学研究院, 农业部 水产品质量安全控制重点实验室, 北京 100141;
    3. 成都信息工程大学资源环境学院, 四川 成都 610225
  • 收稿日期:2018-01-07 出版日期:2018-06-08 发布日期:2014-04-24
  • 通讯作者: 艾晓辉,Tel:(027)81780298,E-mail:aixh@yfi.ac.cn
  • 基金资助:

    中国水产科学研究院基本科研业务费(2018HY-ZD0606);湖北省第二批现代农业产业技术体系项目(HBHZD-ZB-2017-004).

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

YANG Qiuhong1,2, LIU Huan2, ZOU Puxin3, QI Minglong3, LIU Yongtao1,2, AI Xiaohui1,2   

  1. 1. Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan 430223, China;
    2. Chinese Academy of Fishery Sciences, Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing 100141, China;
    3. Chengdu University of Information Technology, College of Resources and Environment, Chengdu 610225, China
  • Received:2018-01-07 Online:2018-06-08 Published:2014-04-24
  • Supported by:

    Central Public-interest Scientific Institution Basal Research Fund,Chinese Academy of Fishery Sciences (CAFS)(No.2018HY-ZD0606);the Second Project of China Agriculture Research System in Hubei Pro-vince (No.HBHZD-ZB-2017-004).

摘要:

建立了高效液相色谱-三重四极杆质谱(HPLC-MS/MS)测定克氏原螯虾中二甲戊灵残留的分析方法。用含0.1%(v/v)乙酸的乙酸乙酯溶液提取克氏原螯虾中的二甲戊灵,于35℃旋蒸至干,经含0.1%(v/v)乙酸的甲醇-水(8∶2,v/v)溶解残渣后,用酸性氧化铝柱、石墨化炭黑(GCB)进行净化。采用Symmetry C18色谱柱(100 mm×2.1 mm,3.5 μm)进行分离,用加热大气压电喷雾电离(HESI)源、正离子模式进行扫描,在多反应监测模式(MRM)下检测。结果表明,二甲戊灵在1.0~20.0 μg/L范围内线性良好,相关系数为0.9960,检出限为0.2 μg/kg;二甲戊灵的加标回收率为63.3%~104.7%,精密度为6.9%~14.5%(n=7)。该方法简单、快速、灵敏度高,能够满足克氏原螯虾中二甲戊灵药物残留检测的需求。

关键词: 残留, 二甲戊灵, 高效液相色谱-三重四极杆质谱, 克氏原螯虾

Abstract:

A novel method was developed for the determination of pendimethalin in Procambarus clarkii by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were extracted with ethyl acetate containing 0.1%(v/v) acetic acid, and the extracts were dried at 35℃. The final extracts were redissolved with methanol-water (8:2, v/v) containing 0.1%(v/v) acetic acid and cleaned up by acidic alumina column and graphitized carbon black (GCB). The prepared samples were separated on a Symmetry C18 column (100 mm×2.1 mm, 3.5 μm) and characterized using a heated electrospray ionization (HESI) source in the positive ion multiple reaction monitoring mode. Under optimum experimental conditions, the standard curve was linear in the range of 1.0-20.0 μg/L with the correlation coefficient of 0.9960. The limit of detection was 0.5 μg/kg. The spiked recoveries of the pendimethalin in the Procambarus clarkii samples ranged from 63.3% to 104.7% with RSDs of 6.9%-14.5% (n=7). The proposed method is quick, simple and sensitive, and suitable for the rapid determination and analysis of pendimethalin in Procambarus clarkii samples.

Key words: Procambarus clarkia, high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), pendimethalin, residues

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