乌梅的1H-NMR指纹图谱研究
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篇名: 乌梅的1H-NMR指纹图谱研究
TITLE:
摘要: 目的:为乌梅的质量控制以及功效物质的全面检测和开发利用提供参考。方法:以氘代甲醇-重水(1 ∶ 0.3,V/V)为提取溶剂,在25 ℃下采用标准的预饱和脉冲序列(ZGPR)压制水峰建立10批不同来源乌梅药材的氢核磁共振(1H-NMR)指纹图谱,通过“加标准品定性”试验、数据库比对和相关文献比对进行信号归属,采用相关系数法计算10批不同来源乌梅药材1H-NMR指纹图谱的相似度,并采用主成分分析(PCA)法进行药材的质量评价。结果:从乌梅药材中同时检测出19种化合物,包括绿原酸、柠檬酸、丁二酸、乙酸、丙氨酸、缬氨酸、γ-氨基丁酸等。其中,乙酸、γ-氨基丁酸和丁二酸为首次从乌梅药材中检测到。10批乌梅药材指纹图谱的相似度均>0.9,平均为0.974。 PCA结果显示,前两个主成分的累积贡献率为90.3%,与相似度评价结果基本一致。结论:建立的1H-NMR方法具有整体性和分析快等优点,可为乌梅的质量控制和功效物质的全面检测提供参考。
ABSTRACT: OBJECTIVE: To provide reference for the quality control of Prunus mume, comprehensive detection, development and utilization of active ingredients. METHODS: Using deuterated methanol and deuterium oxide (1 ∶ 0.3, V/V) as extracting solvent, 1H-NMR fingerprints of 10 batches of P. mume from different sources were established by standard presaturated pulse sequence (ZGPR) at 25 ℃. The signal was assigned through “adding standard substance qualitation” trial, database comparison and related literature comparison. The similarity of 1H-NMR fingerprints was calculated for 10 batches of P. mume from different sources by using correlation coefficient method. The quality of medicinal material was evaluated by principal component analysis (PCA). RESULTS: A total of 19 compounds were detected in P. mume, among which chlorogenic acid, citric acid, succinic acid, acetic acid, alanine, valine, γ-aminobutyric acid, etc. Among them, acetic acid, γ-aminobutyric acid and succinic acid were detected for the first time. Moreover, the similarity of 1H-NMR fingerprinting of 10 samples was higher than 0.9, being 0.974 in average. The results of PCA showed that accumulative contribution rate of former 2 main components was 90.3%, which was consistent with the similarity evaluation. CONCLUSIONS: The established 1H-NMR method has the advantages of embodying integrity and rapid analysis, and can provide reference for the quality control of P. mume, and comprehensive testing of active ingredients.
期刊: 2018年第29卷第19期
作者: 唐荣伟,田玫瑰,唐玲,杜欢,范刚,潘正
AUTHORS: TANG Rongwei,TIAN Meigui,TANG Ling,DU Huan,FAN Gang,PAN Zheng
关键字: 乌梅;氢核磁共振;指纹图谱;主成分分析;质量控制
KEYWORDS: Prunus mume; 1H-NMR; Fingerprint; Principal component analysis; Quality control
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