Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

胡巧茹; 丛中笑; 沙美兰; 曹鹏; 梁君妮; 李晓玉; 关丽丽; 谢爽

doi:doi：10.3969/j.issn.1004-4957.2019.04.004

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Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

- Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
- Vol. 38, Issue 4, Pages: 396-402(2019)
- 作者机构：
  
  烟台出入境检验检疫局检验检疫技术中心
- 作者简介：
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- DOI：doi：10.3969/j.issn.1004-4957.2019.04.004
  CLC：
- Published：2019
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胡巧茹, 丛中笑, 沙美兰, 曹鹏, 梁君妮, 李晓玉, 关丽丽, 谢爽. Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. 2019, 38(4): 396-402.
DOI：

胡巧茹, 丛中笑, 沙美兰, 曹鹏, 梁君妮, 李晓玉, 关丽丽, 谢爽. Determination of 4 Aflatoxins and 11 Pesticide Residues in Peanut by Ultrahigh Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. 2019, 38(4): 396-402. DOI： doi：10.3969/j.issn.1004-4957.2019.04.004.

摘要

建立了花生样品中4种黄曲霉毒素（黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2）和11种农药残留（啶虫脒、乙草胺、多菌灵、克百威、毒死蜱、苯醚甲环唑、烯酰吗啉、吡虫啉、嘧霉胺、戊唑醇、噻虫嗪）的超高效液相色谱－四极杆/静电场轨道阱高分辨质谱法（UPLC-HRMS）。样品经乙腈-水-乙酸提取液（84∶15∶1，体积比）提取，1.0 g硫酸镁、100 mg PSA与400 mg C18硅胶混合体系净化后进行检测。采用Hypersil Gold C18柱（100 mm×2.1 mm，1.9 μm）分离，用UPLC-HRMS进行检测。结果显示，4种黄曲霉毒素和11种农药残留在各自的质量浓度范围内线性关系良好，相关系数（r2）均大于0.996，方法定量下限为0.25~1.0 μg/kg，样品的加标回收率为79.4%~120%，相对标准偏差（RSD，n=6）为4.2%~10%。该方法的灵敏度高、结果准确、可靠，能够实现对花生样品中4种黄曲霉毒素和11种农药残留含量的同时检测。

Abstract

A method was developed for the determination of 4 aflatoxins and 11 pesticide residues in peanut by ultrahigh performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry（UPLC-HRMS）.The samples were extracted with acetonitrile-water-acetic acid（84∶15∶1，by volume）

and the extracts were cleaned up with 1.0 g MgSO4

100 mg PSA and 400 mg C18.The analytes were separated on a Hypersil Gold C18 column（100 mm×2.1 mm，1.9 μm）

and quantified by UPLC-HRMS.Results showed that 4 aflatoxins and 11 pesticide residues had good linear relationships in their respective mass concentration ranges with their correlation coefficients（r2）more than 0.996.The limits of quantitation（LOQs）of the method ranged from 0.25 μg/kg to 1.0 μg/kg.The spiked recoveries for 4 aflatoxins and 11 pesticide residues at three spiked levels ranged from 79.4%to 120%with relative standard deviations（RSD

n=6） of 4.2%-10%.With the advantages of high sensitivity and reliability

the method was suitable for the simultaneous determination of 4 aflatoxins and 11 pesticide residues in peanut.

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