食品科学 ›› 2019, Vol. 40 ›› Issue (12): 345-352.doi: 10.7506/spkx1002-6630-20180820-199

• 安全检测 • 上一篇    

空间位阻净化-超高效液相色谱-串联质谱技术测定动物源性食品中抗组胺类药物残留

王 京1,2,叶佳明1,王 潇1,钟世欢2,陈青俊3   

  1. 1.赞宇科技集团股份有限公司,浙江 杭州 310030;2.浙江省轻工业研究所,浙江 杭州 310009;3.浙江公正检验中心有限公司,浙江 杭州 311305
  • 出版日期:2019-06-25 发布日期:2019-06-28
  • 基金资助:
    浙江省公益技术研究计划项目(LGN18B050001)

Determination of Antihistamine Residues in Animal-Derived Foods by Steric Hindrance Purification and UPLC-MS/MS

WANG Jing1,2, YE Jiaming1, WANG Xiao1, ZHONG Shihuan2, CHEN Qingjun3   

  1. 1. Zanyu Technology Group Co. Ltd., Hangzhou 310030, China; 2. Zhejiang Institute of Light Industry, Hangzhou 310009, China; 3. Zhejiang Gongzheng Inspection Center Co. Ltd., Hangzhou 311305, China
  • Online:2019-06-25 Published:2019-06-28

摘要: 建立超高效液相色谱-串联质谱法快速测定动物源性食品中19 种抗组胺类药物及其代谢物残留的方法。样品用乙腈-乙酸乙酯溶液提取,提取液经空间位阻净化吸附剂EMR净化,再经无水硫酸镁和氯化钠盐析并浓缩后测定,以0.1%甲酸和0.1%甲酸-乙腈作为流动相进行梯度洗脱,在Poroshell 120 EC-C18色谱柱(100 mm×2.1 mm,2.7 μm)上分离,柱温35 ℃,流速0.3 mL/min,进样量10 μL,在电喷雾正离子模式下以动态多反应监测采集数据,外标法定量。结果表明,19 种抗组胺类药物及其代谢物在相应质量浓度范围内线性良好,相关系数均大于0.999,不同阴性样品基质中(牛肉、鸡肉、猪肝)在3 个质量浓度水平加标实验回收率在75.1%~89.1%之间,相对标准偏差为2.3%~7.1%,方法检出限为0.2~2.0 μg/kg,定量限为0.6~6.0 μg/kg。经方法学验证,本方法简便快速、重复性好、灵敏度高、结果可靠。适用于动物源性食品中19 种抗组胺类药物及其代谢物的快速筛查和定量测定。

关键词: 抗组胺药物, 超高效液相色谱-串联质谱, 动物源食品, EMR-Lipid吸附剂

Abstract: A rapid method for the determination of the residues of 19 anti-histamines and their metabolites in animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. Samples were extracted with acetonitrile-ethyl acetate mixture, and the extract was purified with Enhanced Matrix Removal-Lipid sorbent (EMR-Lipid), and then salted out and concentrated with MgSO4 and NaCl. The chromatographic separation was accomplished on a Poroshell 120 EC-C18 column by gradient elution using 0.1% formic acid as mobile phase A and 0.1% formic acid-acetonitrile as mobile phase B at a flow rate of 0.3 mL/min. The column temperature was set at 35 ℃, and the injection volume was 10 μL. Data were collected by dynamic multi-reaction monitoring (MRM) in electrospray positive ion mode. The analytes were quantitated by external standard method. Statistical analysis indicated that the calibration curves for all analytes had a good linearity with correlation coefficients R2 greater than 0.999 in the tested concentration ranges. The average recoveries for different negative samples (beef, chicken and porcine liver) at three spiked levels were in the range of 75.1%–89.1%, with relative standard deviations (RSDs) of 2.3%–7.1%. The limits of detection (LODs) of this method were 0.2–2.0 μg/kg and the limits of quantitation (LOQs) were 0.6–6.0 μg/kg. In a word, this method proved to be simple, rapid, highly repeatable and sensitive, and reliable, and it could be suitable for rapid screening and quantitative determination of 19 antihistamines and their metabolites in anima-derived food samples.

Key words: antihistamine, liquid chromatography-mass spectrometry (LC-MS), animal-derived foods, EMR-Lipid sorbent

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