色谱 ›› 2019, Vol. 37 ›› Issue (6): 612-618.DOI: 10.3724/SP.J.1123.2018.12026

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定贝类中22种农药残留

范广宇1, 唐秀1, 张云青1, 孟祥龙1, 梁振纲2   

  1. 1. 连云港海关, 江苏 连云港 222042;
    2. 海南出入境检验检疫局技术中心, 海南 海口 570311
  • 收稿日期:2018-12-17 出版日期:2019-06-08 发布日期:2015-04-17
  • 通讯作者: 范广宇,Tel:(0518)82320513,E-mail:gyfan@foxmail.com.
  • 基金资助:

    南京海关科技计划项目(2017KJ12);海关总署应急保障计划(2018IK048).

Determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry

FAN Guangyu1, TANG Xiu1, ZHANG Yunqing1, MENG Xianglong1, LIANG Zhengang2   

  1. 1. Lianyungang Customs, Lianyungang 222042, China;
    2. Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau, Haikou 570311, China
  • Received:2018-12-17 Online:2019-06-08 Published:2015-04-17
  • Supported by:

    Science and Technology Plan Project of Nanjing Customs (No. 2017KJ12); Emergency Support Plan of General Administration of Customs (No. 2018IK048).

摘要:

建立了高效液相色谱-三重四极杆质谱(HPLC-MS/MS)同时测定贝类中22种农药残留的分析方法。样品经含0.1%(v/v)甲酸的乙腈提取,N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,然后采用ACE UltraCore 2.5 SuperC18柱(100 mm×2.1 mm,2.5 μm)分离,以甲醇-0.1%(v/v)甲酸水溶液为流动相梯度洗脱,流速为0.4 mL/min,柱温为35 ℃,然后以电喷雾电离(ESI)源,在多反应监测(MRM)、正离子模式下,采用三重四极杆质谱检测。22种农药在各自的线性范围内线性关系良好,相关系数均大于0.997,检出限为0.1~0.3 μg/kg,定量限为0.3~1.0 μg/kg。在3个添加水平下,22种农药的平均回收率为65.2%~109.4%,相对标准偏差为1.3%~15.2%(n=6)。该方法操作简单,快速,准确度高,灵敏度高,可用于贝类中22种农药残留的同时检测。

关键词: 贝类, 高效液相色谱, 农药残留, 三重四极杆质谱

Abstract:

A method for the simultaneous determination of 22 pesticide residues in shellfish by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The pesticides in the samples were extracted with 0.1% (v/v) formic acid in acetonitrile, cleaned up with primary secondary amine (PSA) and graphitized carbon black (GCB), and then separated on an ACE UltraCore 2.5 Super C18 column (100 mm×2.1 mm, 2.5 μm) by elution with a methanol-0.1% (v/v) formic acid solution at a flow rate of 0.4 mL/min. The analytes were detected by electrospray ionization in the positive ion mode and the multiple reaction monitoring mode. Good linear relationships were obtained, and the correlation coefficients (r2) of the 22 pesticides were all higher than 0.997. The limits of detection and limits of quantification were 0.1-0.3 μg/kg and 0.3-1.0 μg/kg, respectively. The mean recoveries varied from 65.2% to 109.4% at three spiked levels, and the relative standard deviations ranged from 1.3% to 15.2% (n=6). The proposed method is simple, accurate, and sensitive, and is effective for the simultaneous determination of 22 pesticide residues detected in shellfish.

Key words: high-performance liquid chromatography (HPLC), pesticide residues, shellfish, triple quadrupole mass spectrometry (MS/MS)

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