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作 者:余黄鹏[1,2] 李志峰[1,2] 孟月华[2] 何明珍[1] 苏丹[1,2] 冯育林[1,2] 杨世林[1,2]
机构地区:[1]中药固体制剂制造技术国家工程研究中心,南昌330006 [2]江西中医学院,南昌330006
出 处:《中国实验方剂学杂志》2013年第16期66-69,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家"重大新药创制"科技重大专项(2012ZX09103201-008);江西省科技支撑计划项目(20111BBG70005-2;20121BBG70019);江西省自然科学基金项目(20114BAB215046)
摘 要:目的:建立不同产地预知子药材的HPLC-ELSD指纹图谱分析方法,并与不同产地预知子药材指纹特征相比较,为科学评价与有效控制预知子药材质量提供新方法。方法:采用HPLC-ELSD法测定了10个不同产地的预知子药材样品。使用Cosmosil-C18色谱柱(4.6 mm×250 mm,5μm),ELSD检测器,流动相乙腈-0.2%甲酸水,梯度洗脱,流速1.0 mL.min-1,ELSD检测器,漂移管温度110℃,气流流速3.0 L.min-1。采用直观分析和相似度软件评价不同产地预知子药材指纹图谱的相似度。结果:建立了不同产地预知子的HPLC-ELSD指纹图谱,检测了10个产地的预知子药材,标定了14个共有峰,各色谱峰分离度较好,相似度较高,达到了中药指纹图谱研究的技术要求。对其中的常春藤皂苷元3-O-β-D-吡喃葡萄糖基-(1→3)-α-L-吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖苷(皂苷X,saponins X),常春藤皂苷元3-O-β-D-吡喃木糖基-(1→2)-α-L-吡喃阿拉伯糖苷(皂苷B,saponins B),常春藤皂苷元3-O-α-L-吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖苷(皂苷PD,saponins PD),常春藤皂苷元3-O-α-L-吡喃阿拉伯糖苷(皂苷A,saponins A)进行了首次归属。结论:该法具有良好的重复性和稳定性,数据准确可靠,建立的HPLC-ELSD指纹图谱可为预知子药材的质量控制提供科学准确的依据。Objective: To establish a fingerprint analysis method for identification of Akebiae Fructus by HPLC-ELSD, get the control chromatogram and compare the fingerprints of Akebiae Fructus collected from different producing areas so as to establish a sensitive and specific method for controlling the quality of Akebiae Fructus. Method: The HPLC-ELSD fingerprints of Akebiae Fructus from 10 different places were obtained. The HPLC separation was performed on a Cosmosil-C18scolumn (4. 6 mm × 250 mm, 5 p.m) in gradient elute mode with a mixture consisting of acetonitrile and 0.2% formic acid water at the flow rate of 1.0 mL ·min ^- 1. The ELSD detector is used and the drift tube temperature of ELSD was set at 110 ℃ with the flow rate of 3.0 L ·min^-1. The data were analyzed by Fingerprint Similarity Evaluation Software to compare the similarity of the samples from different habitats. Result: Fingerprint spectrum of Akebiae Fructus was established. 10 samples were detected and 14 peaks in the chromatogram were common. There was a high similarity and each chromatographic peak was obtainedwith good separation. And the correlation could meet the technical requirements of fingerprint of Chinese traditional medicine. And four peaks in HPLC-ELSD chromatogram were firstly assigned as 3-O-β-D-glucopyranosyl (1→3) - α-L-rhamnopyranosyl- (1→2) -α-L-arabinopyranosyl hederagenin ( saponins X), 3-O-β-D-xylopyranosyl- ( 1→ 2) -α-L-arabinopyranosyl hederagenin ( saponins B) , 3-O-α-L-rhamnopyranosyl- (1→2) -α-L-arabinopyranosyl hederagenin (saponins PD), 3-O-α-L-arabinopyranoside hederagenin (saponins A). Conclusion: This method shows high precision and reliability and the fingerprint spectrum provides a scientific basis for controlling the quality of Akebiae Fructus.
关 键 词:预知子 指纹图谱 高效液相色谱-蒸发光检测
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