食品科学 ›› 2016, Vol. 37 ›› Issue (24): 252-256.doi: 10.7506/spkx1002-6630-201624040

• 安全检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法检测鱼肉和暂养水中丁香酚残留量

赵东豪,王 强,王旭峰,黎智广,柯常亮,李刘冬   

  1. 中国水产科学研究院南海水产研究所,农业部水产品加工重点实验室,农业部水产品贮藏保鲜质量安全风险评估实验室(广州),农业部渔业环境及水产品质量监督检验测试中心(广州),广东 广州 510300
  • 出版日期:2016-12-25 发布日期:2016-12-21
  • 基金资助:
    中国水产科学研究院南海水产研究所基本科研业务费项目(2014TS28);广东省水产品质量安全专项(GDSCZA2015008);国家农产品质量安全风险评估重大专项(GJFP201501003)

Determination of Eugenol in Fish and Farming Water by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHAO Donghao, WANG Qiang, WANG Xufeng, LI Zhiguang, KE Changliang, LI Liudong   

  1. Key Laboratory of Aquatic Product Processing, Ministry of Agriculture, Laboratory of Quality and Safety Risky Assessment for Aquatic Product on Storage and Preservation (Guangzhou), Ministry of Agriculture, Fishery Environment and Aquatic Products Quality Inspection and Testing Center (Guangzhou), Ministry of Agriculture, South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510300, China
  • Online:2016-12-25 Published:2016-12-21

摘要: 建立超高效液相色谱-串联质谱测定鱼肉和暂养水中丁香酚残留量的分析方法。鱼肉样品经正己烷提取,水样则直接用HLB小柱浓缩、富集与净化,以电喷雾离子源负离子模式,在多反应监测模式下测定,内标法定量。结果表明,样品在4 min内完成测定,在1~200 μg/L质量浓度范围内,相关系数(R2)大于0.996,鱼肉样品的加标回收率在88.6%~106%之间,相对标准偏差为7.82%~11.90%;水样的加标回收率在89.2%~96.5%之间,相对标准偏差为5.18%~7.83%。鱼肉和水样中丁香酚的定量限分别为2.5 μg/kg和0.05 μg/L。

关键词: 超高效液相色谱-串联质谱, 固相萃取, 丁香酚, 鱼肉, 暂养水样

Abstract: An analytical method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLCMS/ MS) was developed for the determination of eugenol in fish and farming water samples. Fish samples were extracted with n-hexane and the extract was cleaned up by solid phase extraction with a hydrophilic-lipophilic balance (HLB) cartridge. Water samples were directly concentrated and purified with HLB cartridge. Eugenol was quantitated with an internal standard method in the multiple reaction monitoring mode using negative electrospray ionization within 4 min. The calibration curve for the analyte was linear (R2 > 0.996) in the range of 1 to 200 μg/L. The recoveries of the drug from fish and farming water samples were 88.6%–106% and 89.2%–96.5%, respectively with relative standard deviations (RSDs) of 7.82%–11.90% and 5.18%–7.83%. The limits of quantity (LOQs) were 2.5 μg/kg in fish and 0.05 μg/L in water, respectively.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), solid phase extraction, eugenol, fish, farming water

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