超高效液相色谱-串联质谱法同时测定水产品中6 种丁香酚类物质的残留量

doi:10.7506/spkx1002-6630-20190826-280

食品科学 ›› 2020, Vol. 41 ›› Issue (16): 320-326.doi: 10.7506/spkx1002-6630-20190826-280

• 安全检测 • 上一篇

超高效液相色谱-串联质谱法同时测定水产品中6 种丁香酚类物质的残留量

吴少明，蔡小明，周鹏，蔡慧钦，梁敏，陈言凯，李燕平，冯丽凤，林浩学，黄媛

（福建省产品质量检验研究院，国家加工食品质量监督检验中心，福建福州 350002）

发布日期:2020-08-19
基金资助:
福建省产品质量检验研究院科技项目（KY201813A）

Determination of 6 Eugenol Residues in Aquatic Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WU Shaoming, CAI Xiaoming, ZHOU Peng, CAI Huiqin, LIANG Min, CHEN Yankai, LI Yanping, FENG Lifeng, LIN Haoxue, HUANG Yuan

(Fujian Inspection and Research Institute for Product Quality, China National Quality Supervision and Testing Center for Processed Food, Fuzhou 350002, China)

Published:2020-08-19

摘要/Abstract

摘要： 建立同时测定水产品中丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚、乙酸丁香酚酯、乙酰基异丁香酚的超高效液相色谱-串联质谱（ultra-high performance liquid chromatography-tandem mass spectrometry，UPLC-MS/MS）方法，并应用于实际样品的测定。样品加入无水硫酸钠进行基质分散后以乙腈振荡提取，提取液经HLB固相萃取柱净化，浓缩后，以Shim-pack GIST（2.1 mm×50 mm，2 μm）为色谱柱，甲醇-水作为流动相进行梯度洗脱分离，UPLC-MS/MS进行分析。方法学验证表明，在1.00～500 ng/mL范围内，6 种丁香酚类物质线性关系较好（R＞0.999）；检出限在0.1～0.3 μg/kg之间；定量限在0.3～1.0 μg/kg之间；以3 种不同基质进行2.00、5.00、10.0 μg/kg的加标回收实验，每种加标水平平行实验6 次。结果显示6 种丁香酚类物质平均回收率在83.9%～105.4%之间，相对标准偏差在1.8%～6.9%之间，符合痕量分析的要求。该法简便、结果准确可靠、灵敏度高、检出限低，适用于水产品中6 种丁香酚类物质的测定。

关键词: 超高效液相色谱-串联质谱；丁香酚；固相萃取；水产品?

Abstract: A new method for simultaneous determination of eugenol, isoeugenol, methyl eugenol, methyl isoeugenol, aceteugenol and lsoeugenyl acetate residues in aquatic products by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The samples were extracted with acetonitrile and purified on an HLB solid phase extraction (SPE) column. Chromatographic separation was achieved on a Shim-pack GIST column (2.1 mm × 50 mm, 2 μm) by linear gradient elution using methanol/water as the mobile phase before analysis by UPLC-MS/MS. The method validation showed that good linearity (R > 0.999) was observed in the range of 1.00–500 ng/mL for the 6 eugenols. The limits of detection (LODs) were between 0.1 and 0.3 μg/kg, and the limits of quantification (LOQs) were between 0.3 and 1.0 μg/kg. The recoveries ranged between 83.9% and 105.4% at three spiked levels (2.00, 5.00, and 10.0 μg/kg) with relative standard deviations (n = 6) between 1.8% and 6.9%. This method proved to be simple, accurate, sensitive, and suitable for the quantitative determination of six eugenol residues in aquatic products.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry; eugenol; solid-phase extraction; aquatic products

中图分类号:

TS207.3

吴少明，蔡小明，周鹏，蔡慧钦，梁敏，陈言凯，李燕平，冯丽凤，林浩学，黄媛. 超高效液相色谱-串联质谱法同时测定水产品中6 种丁香酚类物质的残留量[J]. 食品科学, 2020, 41(16): 320-326.

WU Shaoming, CAI Xiaoming, ZHOU Peng, CAI Huiqin, LIANG Min, CHEN Yankai, LI Yanping, FENG Lifeng, LIN Haoxue, HUANG Yuan. Determination of 6 Eugenol Residues in Aquatic Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2020, 41(16): 320-326.

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超高效液相色谱-串联质谱法同时测定水产品中6 种丁香酚类物质的残留量

Determination of 6 Eugenol Residues in Aquatic Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

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