食品科学 ›› 2022, Vol. 43 ›› Issue (14): 311-318.doi: 10.7506/spkx1002-6630-20211018-184

• 安全检测 • 上一篇    

超高效液相色谱-串联质谱法检测畜肉及内脏中苯甲酸和马尿酸残留

王娟强,刘梦瑶,张明悦,赵文涛,李莹莹,郭文萍   

  1. (中国肉类食品综合研究中心,肉类加工技术北京市重点实验室,北京 100068)
  • 发布日期:2022-07-28
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2017YFC1601706)

Determination of Benzoic Acid and Hippuric Acid Residues in Meat and Offal by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Juanqiang, LIU Mengyao, ZHANG Mingyue, ZHAO Wentao, LI Yingying, GUO Wenping   

  1. (China Meat Research Center, Beijing Key Laboratory of Meat Processing Technology, Beijing 100068, China)
  • Published:2022-07-28

摘要: 建立超高效液相色谱-串联质谱技术对畜肉及内脏中苯甲酸和马尿酸进行检测。通过加标回收优化提取溶剂和净化方式,最终选择纯甲醇提取,经PRiME HLB固相萃取小柱净化,采用多反应监测模式检测,外标法定量。结果表明:苯甲酸在20~1 000 ng/mL、马尿酸在4~200 ng/mL质量浓度范围内线性关系良好,线性相关系数均大于0.99,检出限分别为12.5 μg/kg和2.5 μg/kg,定量限分别为50 μg/kg和10 μg/kg;在3 个添加水平的回收率在70.5%~99.7%之间,精密度相对标准偏差在0.3%~7.1%之间(n=6);方法具有良好的重复性和日内、日间稳定性,相对标准偏差不大于7.2%。该方法前处理简单、准确灵敏、回收率好,可为畜肉及内脏中苯甲酸和马尿酸残留量的监管提供技术支持。

关键词: 超高效液相色谱-串联质谱法;畜肉及内脏;苯甲酸;马尿酸

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of benzoic acid and hippuric acid in meat and offal. Through spiked recovery tests, methanol was selected as the extraction solvent. The extract was purified on a PRiME HLB solid phase extraction (SPE) column, detected in the multi-reaction monitoring (MRM) mode, and quantified by an external standard method. The results showed that good linearity was observed for benzoic acid and hippuric acid within the concentration range of 20–1 000 and 4–200 ng/mL with correlation coefficients of greater than 0.99, and the detection limits 12.5 and 2.5 μg/kg, respectively. The limits of quantification for benzoic acid and hippuric acid were 50 and 10 μg/kg, respectively; the recoveries at three spiked concentration levels were between 70.5% and 99.7%, and the relative standard deviations (RSDs) of precision were 0.3%–7.1% (n = 6). The proposed method had good repeatability and intra- and inter-day stability, with RSDs equal to or less than 7.2%. Therefore, this method is simple, accurate and sensitive, and has a good recovery rate. It can provide technical support for the supervision of benzoic acid and hippuric acid residues in meat and offal.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; meat and offal; benzoic acid; hippuric acid

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