色谱

• 技术与应用 • 上一篇    

超高效液相色谱-串联质谱法测定浓缩苹果汁中的熊果苷

孔祥虹1,2* , 何强2, 乐爱山2, 吴双民2, 李建华2   

  1. 1. 陕西师范大学, 陕西 西安 710062; 2. 陕西出入境检验检疫局, 陕西 西安 710068
  • 收稿日期:2010-01-05 修回日期:2010-03-05 出版日期:2010-06-28 发布日期:1980-06-25
  • 通讯作者: 孔祥虹

Determination of arbutin in apple juice concentrate by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry

KONG Xianghong1,2*, HE Qiang2, YUE Aishan2, WU Shuangmin2, LI Jianhua2   

  1. 1. Shaanxi Normal University, Xi’an 710062, China; 2. Shaanxi Entry & Exit Inspection and Quarantine Bureau, Xi’an 710068, China
  • Received:2010-01-05 Revised:2010-03-05 Online:2010-06-28 Published:1980-06-25
  • Contact: KONG Xianghong

摘要: 建立浓缩苹果汁样品中熊果苷的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)检测方法。浓缩苹果汁样品用水溶解、过滤后,用聚苯乙烯-二乙烯基苯共聚物(PS-DVB)固相萃取柱净化,外标法定量。测定时用Eclipse Plus C18色谱柱(100 mm×2.1 mm, 1.8 μm)分离,甲醇-水系统梯度洗脱;MS测定采用多反应监测(MRM)模式。熊果苷的检出限为0.02 mg/L,在0.04~2.0 mg/L的范围内标准溶液的峰面积与质量浓度呈良好的线性关系,回收率为75.2%~102.7%,相对标准偏差(RSD)低于8.9%。该方法简便、快速、灵敏,可用于浓缩苹果汁样品中熊果苷的检测和确证。

关键词: 超高效液相色谱-串联质谱, 浓缩苹果汁 , 熊果苷

Abstract: An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of arbutin in apple juice concentrate. Samples were diluted with water, then cleaned-up with a PS-DVB column. Quantitation was carried out using an external standard method. UPLC was performed on an Eclipse Plus C18 column(100 mm×2.1 mm, 1.8 μm) using a gradient solvent system (methanol-water). MS/MS was performed with multiple reaction monitoring (MRM) mode. The detection limit of arbutin was 0.02 mg/L. The method showed good linear relationship at the range of 0.04-2.0 mg/L. The recoveries ranged from 75.2% to 102.7% with relative standard deviations (RSDs) less than 8.9%. The method is simple, fast and sensitive. It’s suitable for quantitative and qualitative analysis of arbutin in apple juice concentrate.

Key words: apple juice concentrate , arbutin, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)