中国中药杂志

2021, v.46(05) 1168-1178

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女贞子中三萜类成分的定性定量研究
Qualitative and quantitative analysis on triterpenoids in Ligustri Lucidi Fructus

纪鑫;刘晓谦;高陆;肖苏萍;梁曜华;李春;王智民;
JI Xin;LIU Xiao-qian;GAO Lu;XIAO Su-ping;LIANG Yao-hua;LI Chun;WANG Zhi-min;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Xiuzheng Pharmaceutical Group Co.,Ltd.;China National Traditional Chinese Medicine Co.,Ltd.;

摘要(Abstract):

三萜类化学成分是女贞子中的一类主要活性成分,但是前期仅有齐墩果酸得到广泛研究。近几年,有研究表明女贞子中的其他三萜类成分同样具有良好的生物活性,因此有必要对女贞子中三萜类成分的概貌进行系统研究。采用Welch UItimate?XB C_(18)色谱柱(4.6 mm×250 mm, 5μm)进行分离,流动相为甲醇(A)-乙腈(B)-0.2%甲酸水(C),梯度洗脱;流速0.5 mL·min~(-1),柱温25℃,检测波长210 nm。采用上述色谱条件对21批女贞子样品进行测定,建立了女贞子中三萜类成分的HPLC指纹图谱;利用UHPLC-ESI-Orbitrap-MS/MS技术对指纹图谱中15个共有峰进行结构推测,并经对照品比对确认了其中6个共有峰的结构,分别是委陵菜酸、坡模醇酸、山楂酸、白桦脂醇、齐墩果酸和熊果酸。采用同一色谱条件对4个主要成分坡模醇酸、山楂酸、齐墩果酸和熊果酸的含量进行了同步测定,系统适应性与方法学考察结果均符合含量测定要求。此外,以齐墩果酸(A)为内参物,建立了上述4个成分的一测多评分析方法。其中坡模醇酸(B)、山楂酸(C)和熊果酸(D)对齐墩果酸的相对校正因子分别为f_(B/A)=1.12,f_(C/A)=1.02和f_(D/A)=0.88,三者对齐墩果酸的相对保留值分别为RRV_(B/A=)0.46,RRV_(C/A)=0.70和RRV_(D/A)=1.03,含量测定结果与外标法结果相当。该文所建立方法专属性强、分离度高、色谱峰纯度高,含量测定结果可靠,为女贞子中三萜类成分的定性和定量分析奠定了基础。
Triterpenoids are one of the most active constituents in Ligustri Lucidi Fructus, but only oleanolic acid has been mostly studied. In recent years, a growing number of studies have shown that other triterpenes from Ligustri Lucidi Fructus also have various biological activities, so it is necessary to build up a detailed profile of the triterpenoids in Ligustri Lucidi Fructus. The chromatographic separation was performed on a C_(18) column(4.6 mm×250 mm, 5 μm) with mobile phase of methanol-acetonitrile-0.2% formic acid for gradient elution. The detection wavelength was set at 210 nm, with a flow rate of 0.5 mL·min~(-1), and the column temperature of 25 ℃. The HPLC fingerprint of triterpenoids in Ligustri Lucidi Fructus was built by testing 21 batches of samples from different sources. The structures of the total 15 common chromatographic peaks were elucidated with UHPLC-ESI-Orbitrap-MS/MS technique and six of them were identified as tormentic acid, pomolic acid, maslinic acid, botulin, oleanolic acid and ursolic acid by comparison to the reference substances. Under the same chromatographic condition, four main triterpenes(podocarboxylic acid, hawthorn acid, oleanolic acid and ursolic acid) were quantified and the results of system adaptability and methodology investigation all met the requirements of content determination. Meanwhile, with oleanolic acid(A) as the internal reference substance, quantitative analysis of multi-components by single marker(QAMS) method was used to analyze the above four components. The relative correction factor of oleanolic acid(B), hawthorn acid(C) and ursolic acid(D) to oleanolic acid was f_(B/A)=1.12, f_(C/A)=1.02 and f_(D/A)=0.88, respectively, and the relative retention values of these three to oleanolic acid was RRV_(B/A)=0.46, RRV_(C/A)=0.70 and RRV_(D/A)=1.03, respectively. The contents determined by two methods were similar. In conclusion, the method built in this paper is proved to be simple, reliable and specific for the simultaneous qualitative and quantitative analysis of the triterpenoids in Ligustri Lucidi Fructus, which can lay foundation for further assays of the triterpenoids in Ligustri Lucidi Fructus and the relative products.

关键词(KeyWords): 女贞子;三萜类成分;指纹图谱;含量测定;一测多评法
Ligustri Lucidi Fructus;triterpenoids;fingerprint;content determination;quantitative analysis of multi-components by single marker(QAMS)

Abstract:

Keywords:

基金项目(Foundation): 国家中药标准化项目(ZYBZH-C-JL-26);; 中央级公益性科研院所基本科研业务费专项(ZXKT17039);; 北京市科技计划课题(Z171100001717028);; 国家重点研发计划“中医药现代化研究”专项(SQ2017YFC170519)

作者(Author): 纪鑫;刘晓谦;高陆;肖苏萍;梁曜华;李春;王智民;
JI Xin;LIU Xiao-qian;GAO Lu;XIAO Su-ping;LIANG Yao-hua;LI Chun;WANG Zhi-min;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Xiuzheng Pharmaceutical Group Co.,Ltd.;China National Traditional Chinese Medicine Co.,Ltd.;

Email:

DOI: 10.19540/j.cnki.cjcmm.20200706.204

参考文献(References):

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