食品科学 ›› 2019, Vol. 40 ›› Issue (24): 300-305.doi: 10.7506/spkx1002-6630-20190107-085

• 安全检测 • 上一篇    下一篇

固相萃取联合超高效液相色谱-串联质谱法测定畜肉中3 种儿茶酚胺类物质

任南,赵文涛,陈超,吴彦超,张颖颖,李莹莹,郭文萍,范维,王守伟   

  1. (中国肉类食品综合研究中心,北京 100068)
  • 出版日期:2019-12-25 发布日期:2019-12-24
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2017YFC1601706)

Determination of Three Catecholamines in Livestock Meat by Solid Phase Extraction Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

REN Nan, ZHAO Wentao, CHEN Chao, WU Yanchao, ZHANG Yingying, LI Yingying, GUO Wenping, FAN Wei, WANG Shouwei   

  1. (China Meat Food Research Center, Beijing 100068, China)
  • Online:2019-12-25 Published:2019-12-24

摘要: 建立超高效液相色谱-串联质谱技术同时检测畜肉中3 种儿茶酚胺类物质。畜肉样品用高氯酸溶液提取,经混合阳离子固相萃取小柱净化,HILIC Plus色谱柱(4.6 mm×100 mm,3.5 μm)分离,流动相分别为甲酸-水(1∶99,V/V)和乙腈,采用电喷雾离子源,正离子多反应监测,对儿茶酚胺类药物进行检测,外标法实现定量分析。结果表明:3 种儿茶酚胺类药物在40~1 000 ng/mL范围内线性良好,相关系数大于0.99,畜肉中检出限(RSN≥3)为10 μg/kg,定量限(RSN≥10)为40 μg/kg;添加量为40~1 000 μg/kg的3 种儿茶酚胺类物质的回收率均在75.48%~91.25%之间,方法的精密度在1.2%~4.6%之间(n=6)。该方法前处理简单、快速、准确,为畜肉中儿茶酚胺的检测提供方法。

关键词: 儿茶酚胺, 畜肉, β受体激动剂, 固相萃取技术, 超高效液相色谱-串联质谱法

Abstract: This study aimed to establish a method for simultaneous qualitative and quantitative analysis of three catecholamines (CAs) in livestock meat by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were homogenized, extracted with perchloric acid solution, and purified on a PCX solid phase extraction cartridge. The chromatographic separation was achieved on an HILIC Plus column (4.6 mm × 100 mm, 3.5 μm) using a mobile phase consisting of acetonitrile and formic acid in water (1:99, V/V). The analytes were ionized by positive electrospray (ESI+), detected in the multiple reaction monitoring mode (MRM) and quantified by the external standard method. The results indicated that a good linearity over the concentration range of 40–1 000 ng/mL was observed for all the analytes with correlation coefficients greater than 0.99. The limits of detection (LOD) and quantification (LOQ) were 10 and 40 μg/kg, respectively. The average recoveries of the CAs ranged from 75.48% to 91.25% with relative standard deviations (RSDs) of 1.2%–4.6% (n = 6). The method is sensitive, simple, rapid and accurate and can meet the requirements for practical analysis.

Key words: catecholamines, livestock meat, β adrenergic agonist, solid phase extraction, ultra-high performance liquid chromatography-tandem mass spectrometry

中图分类号: