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乳业科学与技术 ›› 2019, Vol. 42 ›› Issue (3): 24-28.DOI: 10.15922/j.cnki.jdst.2019.03.005

• 分析检测 • 上一篇    下一篇

QuEChERS-分散固相萃取-气相色谱-质谱法测定牛乳中喹氧灵残留

齐晓茹, 苏运聪, 李飞, 李兴佳, 张耀广, 柴艳兵   

  1. 石家庄君乐宝乳业有限公司, 农业农村部乳品质量安全控制重点实验室, 河北 石家庄 050021
  • 出版日期:2019-05-01 发布日期:2021-11-09
  • 基金资助:
    “十三五”国家重点研发计划重点专项（2018YFC1604304）

Determination of Quinoxyfen in Milk by QuEChERS Dispersive Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

QI Xiaoru, SU Yuncong, LI Fei, LI Xingjia, ZHANG Yaoguang, CHAI Yanbing   

  1. (Key Laboratory of Dairy Quality and Safety Control, Ministry of Agriculture and Villages, Shijiazhuang Junlebao Dairy Co. Ltd., Shijiazhuang 050021, China)
  • Online:2019-05-01 Published:2021-11-09

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摘要： 建立气相色谱-质谱联用技术测定牛乳中喹氧灵残留量的检测方法。以乙腈作为提取剂，借助分散固相萃 取（填料为C18和N-丙基乙二胺）作为净化手段，经Agilent HP-5MS色谱柱分离，通过基质匹配外标法校正定量。结果 表明：目标物在0.00～1.00 μg/mL范围内线性关系良好，R2＞0.998 7，样品基质在3 个添加水平（5、10、20 μg/kg）下的 回收率为83.2%～100.8%，相对标准偏差为2.1%～4.3%，定量限为5 μg/kg；该方法步骤简单、可靠、稳定，可以推广应 用于牛乳中喹氧灵含量的测定；采用该方法对75 个奶户牛乳中喹氧灵含量进行测定，结果均小于国家限量值。

关键词: 牛乳；喹氧灵；气相色谱-质谱测定

Abstract: A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of quinoxyfen in milk. The sample was extracted with acetronitrile, and then the extract was cleaned up by dispersive solid-phase extraction (dSPE) with C18 and N-propyl ethylenediamine (PSA) as sorbent materials. The analyte was separate on an Agilent HP- 5MS column, detected by GC-MS, and quantified by matrix-matched external standard method. The results showed that good linearity was obtained within the concentration range of 0.00–1.00 μg/mL with a correlation coefficients (R2) > 0.998 7. The average recoveries at three spiked levels (5, 10 and 20 μg/kg) ranged from 83.2% to 100.8% with relative standard deviations (RSDs) of 2.1%–4.3%. The limit of quantitation was 5 μg/kg. The proposed method was simple, sensitive and reliable, and could be applied to the determination of quinoxyfen in milk. The content of quinoxyfen in milk samples from 75 dairy households was detected to be less than the national limit value by this method.

Key words: milk; quinoxyfen; gas chromatography-mass spectrometric determination

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