色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 672-676.DOI: 10.3724/SP.J.1123.2012.02016

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法检测香辛料中罗丹明B

尹峰, 丁召伟, 杨志坚   

  1. 国家副食品质量监督检验中心, 北京 100070
  • 收稿日期:2012-02-13 修回日期:2012-04-17 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 尹峰,硕士,工程师,主要从事兽药残留、食品添加剂的检验工作.

Determination of rhodamine B in spices by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

YIN Feng, DING Zhaowei, YANG Zhijian   

  1. State Non-Staple Food Quality Supervision and Test Center, Beijing 100070, China
  • Received:2012-02-13 Revised:2012-04-17 Online:2012-07-28 Published:2012-07-19

PDF

574

被引次数

29

摘要： 建立了香辛料中罗丹明B的固相萃取-高效液相色谱-串联质谱分析方法。样品经乙腈提取后离心,在提取液中加入10 mL 1%三氯乙酸溶液后,用Bond Elut Plexa PCX强阳离子固相萃取柱净化、富集,Pursuit C18色谱柱(100 mm×2.0 mm, 3 μm)分离,以0.1%甲酸水和甲醇为流动相梯度洗脱,电喷雾电离正离子模式下多反应监测(MRM)模式进行定性、定量检测。结果表明,在0.6～6 μg/L范围内的线性相关系数R2＞0.99;方法的定量限为1.2 μg/kg;添加量分别为1.197、2.992及5.985 μg/L时的加标回收率为80%～121%,相对标准偏差＜15%。同时对流动相的洗脱梯度、提取溶剂、固相萃取柱等条件进行了优化。该方法的专属性较强,基质效应较小,可用于固体香辛料产品中罗丹明B的定性、定量分析。

关键词: 高效液相色谱-串联质谱法, 固相萃取, 罗丹明B, 香辛料

Abstract: Rhodamine B (RB), as an unlawful colour, is forbidden to add into foods by Chinese government. A solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS) method for the determination of RB in spices has been developed. The sample was extracted by acetonitrile and then centrifugated, purified and enriched with a strong positive ion exchange SPE column (Bond Elut Plexa PCX SPE column) after adding 10 mL 1% trichloroacetic acid solution. The HPLC separation was performed on a Pursuit C18 column (100 mm×2.0 mm, 3 μm) by gradient elution with 0.1%(v/v) formic acid solution and methanol as the mobile phase. The analyte was detected by electrospray ionization in positive ion mode-MS/MS in multiple reaction monitoring (MRM) mode. The good linearity (R2＞0.99) was obtained over the range of 0.6~6 μg/L. The limit of quantification (LOQ) for RB was 1.2 μg/kg. The average recoveries were ranged from 80% to 121% at the spiked levels of 1.197, 2.992 and 5.985 μg/L, and the relative standard deviations (RSDs) were not more than 15%. The conditions of mobile phase elution gradients, extraction solvents, and SPE columns were optimized. This method is highly selective and has weak matrix effect for qualitative and quantitative analyses of RB in spices.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) , rhodamine B, spices, solid phase extraction (SPE)