色谱

色谱 ›› 2012, Vol. 30 ›› Issue (08): 832-835.DOI: 10.3724/SP.J.1123.2012.03045

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定脐橙中橘红2号染料

胡莉*, 雷绍荣, 郭灵安   

  1. 四川省农业科学院分析测试中心, 四川 成都 610066
  • 收稿日期:2012-03-23 修回日期:2012-05-09 出版日期:2012-08-28 发布日期:2012-08-17
  • 通讯作者: 胡莉,硕士,助理研究员,主要研究方向为农产品质量标准与检测技术研究. Tel: (028)84504142, E-mail: huli0704@163.com.
  • 基金资助:

    四川省农业科学院青年基金项目（2011QNJJ-027）.

Determination of citrus red 2 in navelorange by ultra performance liquid chromatography-tandem mass spectrometry

HU Li*, LEI Shaorong, GUO Ling’an   

  1. Center of Analysis and Testing, Sichuan Academy of Agricultural Sciences, Chengdu 610066, China
  • Received:2012-03-23 Revised:2012-05-09 Online:2012-08-28 Published:2012-08-17

PDF

361

被引次数

23

摘要： 建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定脐橙中的橘红2号染料。样品用乙腈提取,NH2固相萃取小柱进行净化后,用超高效液相色谱-串联质谱仪进行测定,使用Waters Acquity UPLC BEH C18柱(50 mm×2.1 mm, 1.7 μm)进行分离,以水和乙腈作为流动相梯度洗脱,流速为0.3 mL/min。质谱采用电喷雾离子源、正离子采集模式(ESI+),采集方式为多反应监测(MRM)。方法的线性范围为0.1～100 μg/L (线性相关系数r2=0.9965),检出限为0.05 μg/kg,定量限为0.1 μg/kg。在空白脐橙样品中添加1.0、10.0和100.0 μg/kg的橘红2号染料,其回收率为84.2%～94.0%,相对标准偏差为2.86%～10.15%。利用该方法对市场上随机采集的18份脐橙样品进行了检测,结果显示,从2份样品中检出橘红2号染料。该方法灵敏度高,准确度好,适用于对脐橙中橘红2号染料的检测。

关键词: 超高效液相色谱-串联质谱, 橘红2号染料, 脐橙

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of citrus red 2 (CR2) in navelorange. The sample was extracted with acetonitrile, cleaned-up by an NH2 solid phase extraction cartridge. Then, the analyte was separated on a Waters Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) in gradient elution with the mobile phases of water and acetonitrile. The separated compounds were detected with a Waters Xevo TQ MS tandem quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The linearity of the method was good (r2=0.9965) over the concentration range from 0.1 to 100 μg/L for CR2. The limit of detection (LOD) was 0.05 μg/kg, and the limit of quantification (LOQ) was 0.1 μg/kg. The average recoveries of CR2 at the three levels of 1.0, 10.0 and 100.0 μg/kg were between 84.2% and 94.0% with the relative standard deviations (RSDs) between 2.86% and 10.15%. Finally, a total of 18 navelorange samples randomly collected from different markets were detected by the proposed method, and two samples contained CR2. The sensitivity, accuracy, and precision of this method can meet the requirements of the CR2 analysis.

Key words: citrus red 2 (CR2), navelorange, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)