色谱 ›› 2015, Vol. 33 ›› Issue (8): 822-829.DOI: 10.3724/SP.J.1123.2015.03022

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆飞行时间质谱法快速筛查水产品中28种酸性合成色素

王萍亚, 周勇, 戴意飞, 黄鹂, 赵巧灵   

  1. 舟山市食品药品检验检测研究院, 舟山市质量技术监督检测研究院, 浙江 舟山 316021
  • 收稿日期:2015-03-17 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 戴意飞
  • 基金资助:

    国家科技部公益专项(201210060);舟山市公益类科技项目(2013C31050).

Rapid screening of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

WANG Pingya, ZHOU Yong, DAI Yifei, HUANG Li, ZHAO Qiaoling   

  1. Zhoushan Institute for Food and Drug Control, Zhoushan Institute of Calibration and Testing for Quality and Technology Supervision, Zhoushan 316021, China
  • Received:2015-03-17 Online:2015-08-08 Published:2015-07-27

摘要:

利用超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF MS)技术建立了水产品中28种酸性合成色素的快速检测方法。水产样品采用氨水-水-乙醇(2:1:7, v/v/v)溶液提取,经氨基化吸附剂基质分散法净化后直接用UPLC-Q-TOF MS测定。目标物经Eclipse Plus-C18柱分离,以0.1%(v/v)甲酸-5 mmol/L乙酸铵水溶液和乙腈为流动相进行梯度洗脱,采用电喷雾负离子模式下全信息串联质谱扫描模式进行检测。结果表明:水产品中28种酸性合成色素的定量限(LOQ, S/N=10)为20~100 μg/kg;并在各自的线性范围内线性关系良好(相关系数r)≥0.991,峰面积的相对标准偏差(n=6)均小于5.61%;在3个加标水平下的平均回收率为70.24%~106.47%,相对标准偏差为5.62%~9.65% (n=6)。该方法快速简单、灵敏度高,适用于水产品中28种色素的快速筛查。

关键词: 超高效液相色谱-四极杆飞行时间质谱, 快速筛查, 水产品, 酸性合成色素

Abstract:

An analytical method was established for the simultaneous determination of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF MS). The analytes in fishery products were extracted with ethyl alcohol containing 20% (v/v) ammonia water and 10% (v/v) water. Then the extract solution was purified according to amination adsorbent matrix dispersion method. The compounds were separated by an Eclipse Plus-C18 column with acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium acetate solution as the mobile phases, and measured by UPLC-Q-TOF MS with electrospray ionization in negative mode. As a result, the limits of quantification (LOQs, S/N=10) of the target compounds were 20-100 μg/kg in fishery products. The 28 analytes behaved linearly in wide-range with the correlation coefficients more than 0.991 as well as the relative standard deviations (RSDs) of the peak areas less than 5.61% (n=6). The average recoveries of the 28 analytes spiked at three levels were ranged from 70.24% to 106.47% with RSDs of 5.62%-9.65% (n=6). This method can be applied to the analysis of the 28 acidic artificial dyes in fishery products due to its fastness, simplicity and relatively high sensitivity.

Key words: acidic artificial dyes, fishery products, rapid screening, ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF MS)

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