食品科学 ›› 2021, Vol. 42 ›› Issue (12): 275-280.doi: 10.7506/spkx1002-6630-20200428-378

• 安全检测 • 上一篇    下一篇

液相色谱-串联质谱法测定畜禽表皮中松香酸和脱氢松香酸

沈金灿,黄昌雄,肖陈贵,吴章杰,赵凤娟,康海宁,岳振峰   

  1. (1.深圳海关食品检验检疫技术中心,广东 深圳 518045;2.深圳市食品安全检测技术研发重点实验室,广东 深圳 518045)
  • 出版日期:2021-06-25 发布日期:2021-06-29
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2017YFC1601603)

Simultaneous Determination of Abietic Acid and Dehydrogenated Abietic Acid in Livestock and Poultry Skin by Liquid Chromatography-Tandem Mass Spectrometry

SHEN Jincan, HUANG Changxiong, XIAO Chengui, WU Zhangjie, ZHAO Fengjuan, KANG Haining, YUE Zhenfeng   

  1. (1. Food Inspection & Quarantine Center, Shenzhen Customs District, Shenzhen 518045, China; 2. Shenzhen Key Laboratory of Detection Technology R&D on Food Safety, Shenzhen 518045, China)
  • Online:2021-06-25 Published:2021-06-29

摘要: 采用液相色谱-串联质谱法对畜禽表皮组织中的松香酸和脱氢松香酸含量进行检测。样品中的松香酸和脱氢松香酸用乙腈提取,经HLB固相萃取柱净化,采用液相色谱-串联质谱进行检测。色谱柱:反相C18柱(100 mm×2.1 mm,2 μm);流动相:0.1%甲酸溶液和0.1%甲酸-甲醇溶液(10∶90,V/V);流速:0.3 mL/min;质谱分析采用电喷雾电离正离子模式检测,扫描方式为多反应监测。结果表明:松香酸线性范围为2.0~100 μg/L,检出限为1.1 μg/kg,定量限为3.6 μg/kg;脱氢松香酸线性范围为5.0~250 μg/L,检出限为3.9 μg/kg,定量限为13 μg/kg。在5.0~200 μg/kg添加量范围内松香酸和脱氢松香酸的回收率为81.7%~93.7%,相对标准偏差均在12%以内。方法用于实际样品分析,多个畜禽表皮样品中检出松香酸及脱氢松香酸,采用松香甘油酯进行脱毛的鸭皮中也检出了一定含量的松香酸及脱氢松香酸。本实验建立的分析方法简便快捷,具有较好的灵敏度和可靠性,可用于畜禽表皮组织中松香酸和脱氢松香酸的定量确证分析。

关键词: 液相色谱-串联质谱;畜禽;松香酸;脱氢松香酸

Abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established to determine abietic acid and dehydrogenated abietic acid in livestock and poultry skin. Samples were extracted with acetonitrile, and the extract was purified with an HLB solid-phase extraction (SPE) cartridge before analysis by LC-MS/MS. The chromatographic separation was accomplished on a C18 column (100 mm × 2.1 mm, 2 μm) with a mobile phase consisting of 0.1% formic acid solution and 0.1% formic acid-methanol solution (10:90, V/V) at a flow rate of 0.3 mL/min. The analysis was achieved by using an electrospray ionization (ESI) source in the positive ion mode with multiple reaction monitoring. The linear range, detection limit and quantification limit were 2.0–100 μg/L, 1.1 μg/kg, and 3.6 μg/kg for abietic acid; and 5.0–250 μg/L, 3.9 μg/kg, and 13 μg/kg for dehydrogenated abietic acid, respectively. The recovery rates of spiked samples at three different concentration levels of 5.0, 10 and 50 μg/kg for abietic acid and of 20, 40 and 200 μg/kg for dehydrogenated abietic acid were in the range of 81.7%–93.7%, with relative standard deviations (RSDs) within 12%. The developed method was successfully applied for the analysis of several real samples. Both abietic acid and dehydrogenated abietic acid were detected in some samples including duck skin dehaired with rosin glyceride. This analytical method proved to be simple, fast, sensitive and reliable, and could be used for confirmatory and quantitative analysis of abietic acid and dehydrogenated abietic acid in livestock and poultry skin.

Key words: liquid chromatography-tandem mass spectrometry; livestock; abietic acid; dehydrogenated abietic acid

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