色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1216-1223.DOI: 10.3724/SP.J.1123.2017.09026

• 特别策划:“毒鸡蛋”检测专栏 • 上一篇    下一篇

固相萃取-液相色谱-四极杆飞行时间质谱法快速筛查禽蛋及蛋制品中氟虫腈及其代谢物

郭德华1, 时逸吟1, 李优1, 伊雄海1, 邓晓军1, 肖文清1, 王键1, 李霄1, 柳菡2, 沈伟健2   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 江苏出入境检验检疫局, 江苏 南京 210001
  • 收稿日期:2017-09-14 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 时逸吟,E-mail:shiyy@shciq.gov.cn
  • 基金资助:

    上海市科委2015-度科学仪器领域项目（15142201700）.

Rapid screening of fipronil and its metabolites in egg and egg products by solid phase extraction-liquid chromatography-quadrupole time-of-flight mass spectrometry

GUO Dehua1, SHI Yiyin1, LI You1, YI Xionghai1, DENG Xiaojun1, XIAO Wenqing1, WANG Jian1, LI Xiao1, LIU Han2, SHEN Weijian2   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2017-09-14 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Project of Shanghai Science and Technology Commission 2015 Annual Field of Scientific Instruments (No. 15142201700).

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187

被引次数

4

摘要：

建立了液相色谱-四极杆飞行时间质谱（LC-QTOF MS）测定禽蛋及蛋制品中氟虫腈及其代谢物的快速筛查方法。样品经酸性乙腈提取，PRiME HLB SPE柱净化，Poroshell 120 EC C18色谱柱（150 mm×3 mm，2.7 μm）分离，以水-乙腈为流动相，梯度洗脱，负离子模式下测定，以乙虫腈为内标定量。实验中建立了一级精确质量和二级碎片离子质谱数据库，并且对4种禽蛋及蛋制品的基质效应进行了考察。结果表明，氟虫腈及其代谢物在0.1~5 μg/L范围内线性关系良好，相关系数（r2）均大于0.99。方法的检出限（LOD，S/N>3）和定量限（LOQ，S/N>10）分别为0.2 μg/kg和1 μg/kg。在不同基质中，氟虫腈及其代谢物在1、2和5 μg/kg的添加水平下平均加标回收率为82.6%~98.1%，相对标准偏差为3.8%~9.9%（n=6）。该方法有效消除了液相色谱-四极杆飞行时间质谱检测过程中的离子化抑制效应，灵敏度和准确度高，适用于鸡蛋、鸡蛋面、蛋糕和蛋黄酱中氟虫腈、氟虫腈砜、氟虫腈亚砜和氟甲腈的快速筛查。

关键词: 氟虫腈及其代谢物, 固相萃取, 禽蛋及蛋制品, 筛查, 液相色谱-四极杆飞行时间质谱

Abstract:

A method for rapid screening of fipronil and its metabolites in egg and egg products was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The samples were extracted by acid-acetonitrile, cleaned up by PRiME HLB SPE. The separation was performed on a Poroshell 120 EC C18 column (150 mm×3 mm, 2.7 μm) with gradient elution using water and acetonitrile as mobile phases. The target compounds were monitored under negative ionization mode with electrospray ionization (ESI) source and two databases of accurate mass and fragment ions were created. The matrix effects in four kinds of egg and egg products were considered and the quantification was carried out by internal standard method. The results demonstrated that the linear ranges were from 0.1 to 5 μg/L with good correlation coefficients (r2>0.99). The limits of detection (LODs, S/N>3) and limits of quantitation (LOQs, S/N>10) were 0.2 μg/kg and 1 μg/kg, respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1, 2 and 5 μg/kg varied from 82.6%-98.1%, and the relative standard deviations (RSDs) were between 3.8%-9.9% (n=6). The method can effectively correct the ionization suppression. It is sensitive, accurate and suitable for the rapid screening of fipronil, fipronil sulfide, fipronil sulfone and fipronil desulfinyl in egg, egg noodle, cake and mayonnaise.

Key words: egg and egg products, fipronil and its metabolites, liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS), screening, solid phase extraction (SPE)

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