色谱

色谱 ›› 2017, Vol. 35 ›› Issue (9): 941-948.DOI: 10.3724/SP.J.1123.2017.06001

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆-飞行时间质谱法快速筛查姜和葱中44种农药残留

刘永强1, 刘胜2, 许文娟1, 田国宁1, 张金玲1   

  1. 1. 潍坊出入境检验检疫局检验检疫技术中心, 山东 潍坊 261041;
    2. 淄博出入境检验检疫局检验检疫技术中心, 山东 淄博 255035
  • 收稿日期:2017-05-31 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 刘永强,Tel:(0536)8582596,E-mail:liuyongqianga@163.com.
  • 基金资助:

    山东出入境检验检疫局科研课题（SK201613）；国家质检总局科技计划项目（2016IK202）.

Rapid screening of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

LIU Yongqiang1, LIU Sheng2, XU Wenjuan1, TIAN Guoning1, ZHANG Jinling1   

  1. 1. Technical Center for Inspection & Quarantine of Weifang Entry-Exit Inspection & Quarantine Bureau, Weifang 261041, China;
    2. Technical Center for Inspection & Quarantine of Zibo Entry-Exit Inspection & Quarantine Bureau, Zibo 255035, China
  • Received:2017-05-31 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    Program of Shandong Entry-Exit Inspection & Quarantine Bureau (No. SK201613); Science and Technology Project of Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No. 2016IK202).

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94

被引次数

6

摘要：

建立了超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF/MS）快速筛查和确证姜和葱中44种农药残留的分析方法。样品采用QuEChERS技术进行前处理，用含0.1%（v/v）乙酸的乙腈溶液进行提取，N-丙基乙二胺（PSA）和十八烷基键合硅胶（C18）吸附剂净化。使用Poroshell 120 SB-C18色谱柱（100 mm×3.0 mm， 2.7 μm）分离，以0.1%（v/v）甲酸水溶液（含5 mmol/L乙酸铵）-乙腈为流动相，梯度洗脱，在电喷雾正离子模式下检测，外标法定量。采用全离子MS/MS模式，通过一次数据采集，同时完成化合物的定性筛查和确证。44种化合物在线性范围内线性关系良好，相关系数（r）均大于0.995。44种化合物的定量限（S/N=10）为2.5~5.0 μg/kg，在3个添加水平下的回收率为73.4%~113.7%，相对标准偏差（RSD）为0.7%~12.1%（n=6）。该法有效地提高了高分辨质谱进行农药多残留筛查时的检测效率，具有较强的实际应用价值。

关键词: QuEChERS, 超高效液相色谱-四极杆-飞行时间质谱, 高分辨全离子二极质谱技术, 农药残留, 筛查

Abstract:

An analytical method was established for the simultaneous determination of 44 pesticide residues in ginger and scallion by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile containing 0.1% (v/v) acetic acid aqueous solution, and cleaned-up by primary secondary amine (PSA) and octadecyl bonded silica (C18) adsorbents. The compounds were separated on a Poroshell 120 SB-C18 column (100 mm×3.0 mm, 2.7 μm) with 0.1% (v/v) formic acid aqueous solution containing 5 mmol/L ammonium acetate-acetonitrile as mobile phases under gradient elution. The eluent was determined by UPLC-Q-TOF/MS with electrospray ionization in positive mode. The quantification analysis was performed with the external standard method. In all ions MS/MS mode, the compounds were qualitatively screened and confirmed by one data acquisition. The correlation coefficients (r) were greater than 0.995 in the linear ranges of the 44 pesticides. The limits of quantification (LOQs, S/N=10) of the 44 pesticides were 2.5-5.0 μg/kg. At the three spiked levels, the recoveries were between 73.4% and 113.7% with the relative standard deviations (RSDs) ranging from 0.7% to 12.1% (n=6). The method effectively improves the determination efficiency of pesticide residues screening by high-resolution mass spectrometry.

Key words: high-resolution all ions MS/MS technology, pesticide residues, QuEChERS, screening, ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS)

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