色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1097-1103.DOI: 10.3724/SP.J.1123.2015.03021

• 技术与应用 • 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15种碱性合成色素

黄鹂, 戴意飞, 王萍亚, 周勇, 赵巧灵, 蒋玲波, 罗海军   

  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:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 赵巧灵
  • 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 screen of 15 basic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

HUANG Li, DAI Yifei, WANG Pingya, ZHOU Yong, ZHAO Qiaoling, JIANG Lingbo, LUO Haijun   

  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:2015-10-08 Published:2012-05-09

PDF

80

被引次数

10

摘要：

建立了超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF MS)快速检测水产品中15种碱性合成色素的方法。水产样品经乙腈(含10%(v/v)乙酸)提取,采用C18复合硅胶基质分散管进行样品净化处理。目标物采用C18色谱柱分离,以乙腈和0.1%(v/v)甲酸-5 mmol/L乙酸铵溶液为流动相,梯度洗脱,四极杆飞行时间串联质谱电喷雾正离子模式检测。结果表明:15种碱性色素的定量限(LOQs, S/N=10)为0.1~100 μg/kg,并在各自的线性范围内线性关系良好,相关系数(r)≥0.993。在3个加标水平下的平均回收率为80.60%~107.37%,测定结果的相对标准偏差为3.33%~6.69%(n=6)。该方法快速、简便、灵敏度高,适用于日常水产品中15种碱性合成色素的快速筛查。

关键词: C18复合硅胶基质萃取管, 超高效液相色谱-四极杆飞行时间质谱, 碱性合成色素, 快速筛查, 水产品

Abstract:

A new method was established for the simultaneous determination of 15 basic 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 acetonitrile containing 10% (v/v) acetic acid, then purified by dispersive solid phase extraction with C18-silicone adsorbent. The compounds were separated by a 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 positive mode. As a result, the limits of quantification (LOQs, S/N=10) of the 15 target compounds were 0.1-100 μg/kg in fishery products. The 15 analytes behaved linearly in their respective ranges with the correlation coefficients no less than 0.993. The average recoveries of the 15 analytes spiked at three levels were ranged from 80.60% to 107.37% with the RSDs of 3.33%-6.69% (n=6). This method is suitable for routine qualitative and quantitative analyses of the 15 basic artificial dyes in fishery products due to its fastness, simplicity and relatively high sensitivity.

Key words: basic artificial dyes, C18-silicone solid phase extraction column, fishery products, rapid screening, ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF MS)

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