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黄芪药材提取纯化过程中黄芪皂苷Ⅳ含量变化及相关成分分析
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作者单位
陈超,吴惠勤,黄晓兰,黄芳,刘梦云 广东省科学院广东省测试分析研究所(中国广州分析测试中心)广东省中药质量安全工程技术研究中心 
中文摘要:该文建立了准确测定黄芪药材中游离黄芪皂苷Ⅳ含量的超高效液相色谱-串联质谱(UPLC-MS/MS)法,并研究了2015年版《中国药典》黄芪项下黄芪皂苷Ⅳ(黄芪甲苷)含量测定前处理操作对黄芪皂苷Ⅳ含量的影响。分别比较索氏提取后、正丁醇萃取后和氨试液除杂后黄芪皂苷Ⅳ的含量变化,并利用具有超高分辨率的傅里叶变换离子回旋共振质谱仪(FT-ICR-MS)分析其成分的差异性。结果表明,在优化条件下,黄芪药材中黄芪皂苷Ⅳ在0.387 0~24.75 mg/L范围内呈良好的线性关系,相关系数(r)为0.999 8,检出限(LOD)为1.0 mg/kg,定量下限(LOQ)为3.0 mg/kg,加标回收率为94.5%~105%,相对标准偏差(RSD,n=6)为1.4%。研究发现甲醇直接提取的黄芪皂苷Ⅰ相对含量最高,正丁醇萃取后的氨试液除杂过程会导致黄芪皂苷Ⅰ及其他黄芪皂苷Ⅳ同系物水解,黄芪皂苷Ⅰ的相对含量显著降低,而黄芪皂苷Ⅳ的含量显著升高;并发现黄芪药材中存在目前尚未报道的黄芪皂苷Ⅱ异构体,将其命名为新黄芪皂苷Ⅱ。
中文关键词:黄芪  游离黄芪皂苷Ⅳ  含量变化  新黄芪皂苷Ⅱ  超高效液相色谱-串联质谱
 
Analysis of Content Variation of Astragaloside Ⅳ and Related Chemical Components During the Extraction and Purification of Astragali Radix
Abstract:A validated analytical method was developed for the determination of free astragaloside Ⅳ in Astragali Radix by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Effects of each step of pretreatment were studied on the determination of astragaloside Ⅳ in Chinese pharmacopoeia(2015)(ChP).Furthermore,impacts of n-butanol extraction and ammonia impurity removal on the determination and content variation of astragaloside Ⅳ were investigated.The differences of components caused by pretreatment were analyzed by Fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS).Results showed that there was a good linear relationship of the proposed method for astragaloside Ⅳ in the range of 0.387 0-2475 mg/L,with a correlation coefficient(r) of 0.999 8.The limit of detection(LOD) and limit of quantitation(LOQ) were 1.0 mg/kg and 3.0 mg/kg,respectively.The recoveries at three spiked levels ranged from 94.5% to 105%,with a relative standard deviation(RSD,n=6) of 1.4%.The relative content of astragaloside Ⅰ was the highest when Astragali Radix was directly extracted with methanol.The impurity removal process with ammonia after n-butanol extraction led to the homologues turned into astragaloside Ⅳ by hydrolysis,which significantly increased the content of astragaloside Ⅳ.Moreover,it was found that there exists a new isomer of astragaloside Ⅱ,named as neoastragaloside Ⅱ in Astragali Radix.
Key Words:Astragali Radix  free astragaloside Ⅳ  content change  neoastragaloside Ⅱ  ultra high performance liquid chromatography-tandem mass spectrometry
引用本文:陈超,吴惠勤,黄晓兰,黄芳,刘梦云.黄芪药材提取纯化过程中黄芪皂苷Ⅳ含量变化及相关成分分析[J].分析测试学报,2020,39(12):1487-1493.
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