色谱

色谱

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超高效液相色谱-电喷雾串联四极杆质谱法检测果汁和葡萄酒中的27种工业染料

赵珊, 张晶, 杨奕, 邵兵*   

  1. 北京市疾病预防控制中心, 北京 100013
  • 收稿日期:2009-09-28 修回日期:2009-11-28 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 邵兵

Determination of 27 industrial dyes in juice and wine using ultra performance liquid chromatography with electrospray ionization tandem quadrupole mass spectrometry

ZHAO Shan, ZHANG Jing, YANG Yi, SHAO Bing*   

  1. Beijing Center for Disease Prevention and Control, Beijing 100013, China
  • Received:2009-09-28 Revised:2009-11-28 Online:2010-04-28 Published:1980-12-25
  • Contact: SHAO Bing

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摘要： 建立了以超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)检测果汁和葡萄酒中27种工业染料的方法。样品经乙腈振荡提取,在盐析作用下分层,目标化合物转移至乙腈层中。目标化合物在梯度洗脱条件下经C18柱分离后采用多反应监测(MRM)模式进行检测。其中24种工业染料使用正离子模式检测,流动相为乙腈和0.1%的甲酸水溶液;其余3种工业染料则采用负离子模式检测,流动相为乙腈和水。结果表明: 果汁中27种工业染料的定量限(LOQ)为0.1～50 μg/kg,回收率为57.0%～117.7%,相对标准偏差为2.4%～17.7%。葡萄酒中的LOQ为0.2～50 μg/kg,回收率为40.8%～109.4%,相对标准偏差为1.6%～17.9%。该方法操作简单,灵敏度高,实现了不同种类的工业染料的同时提取,适合于软饮料中非法添加工业染料的快速检测。

关键词: 超高效液相色谱-电喷雾串联四极杆质谱, 工业染料, 果汁, 葡萄酒

Abstract: A method for the determination of 27 industrial dyes in juice and wine has been developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Acetonitrile was used as extraction solvent, and sodium chloride was added to salt out the analytes from the samples. Chromatographic separation was performed on a C18 column with the gradient elution and the mass spectrometric acquisition was carried out under the mode of multiple reaction monitoring (MRM). Twenty-four of the 27 dyes were detected under positive ionization mode using the mobile phase of acetonitrile and water containing 0.1% formic acid. The other 3 dyes were analyzed under negative ionization mode with the mobile phase of acetonitrile and water. As a result, the average recoveries of 27 dyes spiked in juice ranged from 57.0% to 117.7% with the relative standard deviations (RSDs) of 2.4%~17.7%, and the average recoveries of 27 dyes spiked in wine ranged from 40.8% to 109.4% with the RSDs of 1.6%~17.9%. The limits of quantification (LOQs) of 27 dyes spiked in juice were in the range of 0.1~50 μg/kg, and 0.2~50 μg/kg for those spiked in wine. This method can be applied to rapid detection of illegally added dyes in soft drinks due to its simplicity and high sensitivity.

Key words: industrial dyes, juice, wine , ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry (UPLC-ESI-MS/MS)