纪鑫;刘晓谦;肖苏萍;杨立新;冯伟红;李春;王智民;
JI Xin;LIU Xiao-qian;XIAO Su-ping;YANG Li-xin;FENG Wei-hong;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;China National of Traditional & Herbal Medicine Co.,Ltd.;

• 1:中国中医科学院中药研究所中药质量控制技术国家工程实验室
• 2:中国中药有限公司

摘要(Abstract)：

为了提高女贞子质量控制水平并探讨女贞子炮制后化学成分的变化,该文建立了女贞子中大极性成分的HPLC指纹图谱和多成分同步测定方法。以十八烷基硅烷键合硅胶为固定相,乙腈-0. 2%甲酸为流动相,梯度洗脱,检测波长280 nm,流速1. 0 m L·min-1,柱温25℃。女贞子药材指纹图谱中共选择出22个共有峰,酒女贞子中选出20个,采用对照品指认了二者共有的14个色谱峰。采用同一色谱条件对其中7个成分进行了同步测定,系统适应性与方法学考察结果均符合含量测定要求。与同批次女贞子相比,酒女贞子中5-羟甲基糠醛和红景天苷的含量大幅升高,而环烯醚萜苷类成分的含量普遍降低。建立的方法为女贞子药材、饮片和相关制剂的质量控制提供了依据。
In order to improve the quality control level of Ligustri Lucidi Fructus(LLF) and to explore the changes of chemical components after processing,the HPLC method for fingerprint and simultaneous determination of the major polar components in LLF were established. The octadecylsilane bonded silica gel was used as the stationary phase,with acetonitrile as the mobile phase A and0. 2% formic acid as the mobile phase B in a gradient elution procedure at a flow rate of 1. 0 m L·min-1. The detection wavelength was set at 280 nm and the column temperature was 25 ℃. There were 22 common peaks,20 of which were selected from the fingerprint of LLF and its wine-steamed product,respectively,and 14 chromatographic peaks were identified with reference substances. With the same chromatographic conditions,seven components were quantitatively analyzed and the results of system adaptability and methodology investigation all met the requirements of content determination. Compared with the crude LLF,the content of 5-hydroxymethyl furfural and salidroside significantly increased in wine-steamed LLF,while the contents of iridoid glycosides generally decreased. The method provided a basis for quality control of LLF and its processed products as well as the related preparations.

关键词(KeyWords)： 指纹图谱;含量测定;高效液相色谱;环烯醚萜苷;苯乙醇苷;女贞子
fingerprint;content determination;high-performance liquid chromatography;iridoid glycosides;phenylethanoid glycosides;Ligustri Lucidi Fructus(LLF)

Abstract:

Keywords:

基金项目(Foundation): 国家中药标准化项目(ZYBZH-C-JL-26);; 北京市科技计划课题项目(Z171100001717028);; “中医药现代化研究”重点专项(SQ2017YFC170519)

作者(Author): 纪鑫;刘晓谦;肖苏萍;杨立新;冯伟红;李春;王智民;
JI Xin;LIU Xiao-qian;XIAO Su-ping;YANG Li-xin;FENG Wei-hong;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;China National of Traditional & Herbal Medicine Co.,Ltd.;

Email:

DOI: 10.19540/j.cnki.cjcmm.20190118.001

参考文献(References)：

• [1]中国药典.一部[S]. 2015:45.
• [2]刘先芳,梁敬钰,孙建博,等.女贞子化学成分和药理活性研究进展[J].海峡药学,2018,30(1):1.
• [3]石力夫,蔡溱,吴广通,等.不同产地女贞子中水溶性活性成分及齐墩果酸的反相高效液相色谱分析[J].中国中药杂志,1998,23(2):77.
• [4]周静,刘垣升.气相色谱法测定女贞子中齐墩果酸和熊果酸的含量[J].中国新药与临床杂志,2003,22(10):596.
• [5]吴勃岩,高明,徐绍娜.女贞子有效成分齐墩果酸对S180荷瘤小鼠抑瘤作用及存活时间的影响[J].中医药信息,2010,27(1):37.
• [6]谭文广,刘伟,鲁菲菲,等.女贞子中三萜化合物的提取与含量测定[J].食品科学,2006,27(11):260.
• [7]李阳,左燕,孙基文.女贞子中2种主要裂环环烯醚萜苷成分的分离鉴定及其抗氧化活性研究[J].中药材,2007,30(5):543.
• [8]杨少青.以胰岛素抵抗肝细胞模型筛选糖尿病药物及环烯醚萜苷类化合物降糖机制研究[D].西安:西北大学,2016.
• [9]胡冬梅,陆杨,房敏峰,等.特女贞苷对四氯化碳致小鼠急性肝损伤的保护作用[J].中国药理学通报,2016,32(9):1260.
• [10]蔡溱,石力夫,胡晋红,等.特女贞甙体外对小鼠脾淋巴细胞转化和自然杀伤细胞活性的影响[J].第二军医大学学报,1998,19(1):76.
• [11]何文君,方泰惠,屠鹏飞.松果菊苷的药理研究进展[J].中国中药杂志,2009,34(4):476.
• [12]姜秋,蒋海强,李慧芬,等.女贞子酒蒸过程中5种苯乙醇类成分的变化规律[J].中国实验方剂学杂志,2014,20(16):60.
• [13]张明发,沈雅琴.红景天苷心脏保护药理作用的研究进展[J].药物评价研究,2017,4(1):125.
• [14]陶益,张畅,李伟东,等.对照提取物法测定女贞子饮片中4种成分的含量[J].中国药房,2015,26(33):4685.
• [15]许浚,游飞祥,袁雪海,等.女贞子HPLC指纹图谱及多指标成分测定[J].中草药,2017,48(20):4198.
• [16]吴修红,孙泽,杨恩龙,等.酒女贞子HPLC指纹图谱的建立及多成分含量的测定[J].药物分析杂志,2016,36(2):273.
• [17]任爽,李铮,王京辉,等.中药女贞子饮片中8个成分的含量比较研究[J].药物分析杂志,2015,35(8):1393.
• [18]梁晓,吴鹏,张学兰,等.女贞子不同炮制品HPLC指纹图谱色谱峰的归属与比较[J].中药材,2015,38(11):2288.
• [19]崔蕴慧,樊化,利弈成,等.女贞子指纹图谱研究及红景天苷、特女贞苷的含量测定[J].时珍国医国药,2014,25(12):2854.
• [20]何盼,孙迎娜,白关亚,等.基于1H-NMR代谢组学技术的青翘抗炎活性部位筛选及作用机制研究[J].中国中药杂志,2016,41(18):3443.
• [21]王芳焕.生物色谱及其在中药活性成分筛选中的应用研究[D].银川:宁夏大学,2010.
• [22]李翠芹,贺浪冲.白细胞膜色谱模型建立与白术中TLT4受体拮抗活性成分筛选研究[J].中国科学,2005,35(6):545.
• [23]邵峰,谷丽菲,钟丹丹,等.山楂体外降三酰甘油主要活性组分谱效关系研究[J].中草药,2017,48(2):339.