食品科学

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UPLC-MS/MS法测定多裂翅果菊中植物甾醇的含量

侯彩婷,王瑞华,邹昀员,宋晓娜,刘海霞,李凤华,徐凌川   

  1. 1.山东中医药大学药学院,山东 济南 250355;2.山东省疾病预防控制中心,山东 济南 250014
  • 出版日期:2013-07-25 发布日期:2013-08-02

Analysis of Phytosterol Content in Pterocypsela laciniata (Houtt.) Shih by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

HOU Cai-ting,WANG Rui-hua,ZOU Yun-yuan,SONG Xiao-na,LIU Hai-xia,LI Feng-hua,XU Ling-chuan   

  1. 1. School of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355, China;
    2. Shandong Center for Disease Control and Prevention, Jinan 250014, China
  • Online:2013-07-25 Published:2013-08-02

摘要:

目的:建立超高效液相色谱与质谱联用法测定植物甾醇单体化合物含量的方法。方法:对多裂翅果菊不同采收期以及不同部位的β-谷甾醇、豆甾醇进行含量测定。试样用石油醚回流提取,ACQUITY UPLC C18超高效液相色谱柱、甲醇和1%乙睛溶液流动相进行分离,以大气压化学电离源正离子模式进行质谱分析,多反应监测(MRM)定量。结果:在0.2~25μg/mL范围内,β-谷甾醇、豆甾醇质量浓度与峰面积均有良好的线性关系,相关系数r分别为0.9990、0.9997,两种单体的加样回收率维持在93.45%~104.23%范围内,RSD不高于7%。多裂翅果菊中β-谷甾醇、豆甾醇含量由高到低依次为:基生叶、茎叶、采收初期根、采收末期根。结论:该方法灵敏度高,分析速度快,操作简便,适用于植物甾醇的含量测定分析。

关键词: 超高效液相色谱-质谱联用法, 多裂翅果菊, 植物甾醇

Abstract:

Objective: To establish a method for determining phytosterol content in Pterocypsela laciniata (Houtt.) Shih by
ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods: The contents of β-sitosterol
and stigmasterol at different harvest times and different parts of Pterocypsela laciniata (Houtt.) Shih were determined.
Samples were extracted with petroleum ether by reflux extraction, and β-sitosterol and stigmasterol in the extract were
separated by an Acquity BEH C18 UPLC column, with methanol and 1% acetonitrile as mobile phase. Atmospheric pressure
chemical ionization was applied for MS analysis in the positive ion mode, and quantification was performed under the
multiple reaction monitoring (MRM) mode. Results: Good linearity was observed for β-sitosterol and stigmasterol in the
concentration range of 0.2 to 25 μg/mL, with correlation coefficients of 0.9990 and 0.9997, respectively. The average
recovery rates were between 93.45% and 104.23%, with relative standard derivations less than 7%. Pterocypsela laciniata
(Houtt.) Shih was rich in phytosterol. Different positions of the plant harvested at different stages of growth were ranked in
decreasing order of the contents of β-sitosterol and stigmasterol as follows: basal leaves, leaves on the stem, roots at the early
stage of growth and roots at the later stage of growth. Conclusion: The method is sensitive, simple, convenient, accurate and
efficient, and it can be used for determining phytosterol.

Key words: ultra-performance liquid chromatography-tandem mass spectrometry, Pterocypsela laciniata (Houtt.) Shih, phytosterol