杜仲的核磁共振指纹图谱研究

doi:10.11938/cjmr20172580

波谱学杂志 ›› 2017, Vol. 34 ›› Issue (4): 453-464.doi: 10.11938/cjmr20172580

杜仲的核磁共振指纹图谱研究

姜阳明^1,2, 邹云云^1,2, 黄滔^1,2, 陈艳^1,2, 潘卫东^1,2, 豪富华³, 张建新^1,2

1. 贵州医科大学, 省部共建药用植物功效与利用国家重点实验室, 贵州贵阳 550014;
2. 贵州省中国科学院天然产物化学重点实验室, 贵州贵阳 550014;
3. 中国科学院武汉物理与数学研究所, 湖北武汉 430071

收稿日期:2017-05-12 修回日期:2017-11-01 出版日期:2017-12-05 在线发表日期:2017-11-29
通讯作者: 张建新,Tel:0851-83876937,E-mail:zjx620@126.com E-mail:zjx620@126.com
基金资助:
贵州省中药现代化科技产业研究开发专项资助项目（黔科合SY字[2014]3081-1号）.

NMR Fingerprints of Eucommia ulmoides Oliver

JIANG Yang-ming^1,2, ZOU Yun-yun^1,2, HUANG Tao^1,2, CHEN Yan^1,2, PAN Wei-dong^1,2, HAO Fu-hua³, Zhang Jian-xin^1,2

1. State Key Laboratory of Functions and Applications of Medicinal Plants, Guizhou Medical University, Guiyang 550014, China;
2. The Key Laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guiyang 550014, China;
3. Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, China

Received:2017-05-12 Revised:2017-11-01 Published:2017-12-05 Online:2017-11-29

摘要/Abstract

摘要： 核磁共振氢谱（Proton Nuclear Magnetic Resonance，¹H NMR）是中药指纹图谱中一种鉴定和控制植物中药质量的新方法．本文采用CPMG（Carr-Purcell-Meiboom-Gill）脉冲序列采集了杜仲提取物的¹H NMR谱，通过完整还原振幅频率表（Complete Reduction to Amplitude-Frequency Table，CRAFT）分析技术对杜仲指纹图谱进行特征指纹分析，将待目标合物的信号从混合物图谱中剥离出来，实现了不分离样品而分析目标化合物信息的目的，从而对杜仲的特征化合物——松脂醇二葡萄糖苷（Pinoresinol Glucoside，PDG）进行了定性和定量分析．结果显示贵阳药用植物园所得杜仲的PDG含量为0.275 6%，相对标准偏差（Relative Standard Deviation，RSD）为1.69%，与高效液相色谱（High Performance Liquid Chromatography，HPLC）定量分析结果（含量为0.269 6%，RSD为0.65%）基本一致．另外，通过NMR检测与多变量数据建模相结合分析了杜仲提取物的全指纹图谱，结果显示同一采收期不同产地的杜仲药材有显著差异，这表明该方法可用于鉴定不同产地的药材，具有一定的实用意义．

关键词: 核磁共振指纹图谱, 完整还原振幅频率表(CRAFT), 杜仲, 定性/定量分析, 松脂醇二葡萄糖苷(PDG)

Abstract: The ¹H NMR fingerprint of Eucommia ulmoides acquired with a CPMG pulse sequence was analyzed with the complete reduction to amplitude-frequency table (CRAFT) approach. The signals of target compounds were extracted without chemical separation and purification. Quantitative analysis showed that the average concentration of pinoresinol glucoside (PDG) in Eucommia ulmoides got from Guiyang medical plant garden was 0.275 6% with a relative standard deviation (RSD) of 1.69%. The results were consistent with those obtained by high performance liquid chromatography (average content of 0.269 6% and RSD of 0.65%). NMR fingerprint and multivariate statistical analysis also revealed that there existed significant differences between Hunan and Guizhou Eucommia ulmoides Oliver.

Key words: NMR fingerprint, complete reduction to amplitude-frequency table (CRAFT), Eucommia ulmoides Oliver, quantitative/quanlitative analysis, pinoresinol glucoside (PDG)

中图分类号:

O482.53

姜阳明, 邹云云, 黄滔, 陈艳, 潘卫东, 豪富华, 张建新. 杜仲的核磁共振指纹图谱研究[J]. 波谱学杂志, 2017, 34(4): 453-464.

JIANG Yang-ming, ZOU Yun-yun, HUANG Tao, CHEN Yan, PAN Wei-dong, HAO Fu-hua, Zhang Jian-xin. NMR Fingerprints of Eucommia ulmoides Oliver[J]. Chinese Journal of Magnetic Resonance, 2017, 34(4): 453-464.

参考文献

[1]FANG D M.Research and application of fingerprint technology of traditional Chinese medicine[J].Chinese Traditional and Herbal Drugs.2005,36(4):632-634.房德敏.中药指纹图谱技术的研究与应用[J].中草药,2005,36(4):632-634. [2]姚丽娜.杜仲的化学成分研究[D].天津:天津大学,2010. [3]吴贵辉.黔产道地药材杜仲核磁共振指纹图谱研究[D].贵阳:贵州大学,2015. [4]黄重阳.喹赛多毒理性质的代谢组学研究[D].武汉:中国科学院武汉物理与数学研究所,2013. [5]李钊.基于核磁共振的统计全相关谱的应用[D].武汉:中国科学院武汉物理与数学研究所,2007. [6]YANG Y W,WANG Y L,SA R N,et al.Chemical fingerprinting of angilica sinensis at different growth stages by 1H NMR[J].Chinese J Magn Reson,2013,30(1):69-79.杨应文,王亚丽,萨日娜,等.不同生长期当归1H NMR指纹图谱的研究[J].波谱学杂志,2013,30(1):69-79. [7]LUO G A,WANG Y M.Classification and development of TCM fingerprint[J].Chinese Journal of New Drugs,2002,11(1):46-51.罗国安,王义明.中药指纹图谱的分类和发展[J].中国新药杂志,2002,11(1):46-51. [8]ZHAO T Z,LIANG X T.Identification of Chinese medicine by 1H-NMR fingerprint[J].Chinese Traditional and Herbal Drugs.2000,31(11):868-870.赵天增,梁晓天.1H-NMR指纹法鉴定植物中药[J].中草药,2000,31(11):868-870. [9]QING H L,ZHAO T Z,DOU H Q,et al.Identification of gastrodia and it's counterfeits by nuclear magnetic resonance spectroscopy[J].Jorunal of Chinese Medicinal Materials,1994,17(6):23-24.秦海林,赵天增,都恒青,等.核磁共振波谱法鉴别天麻及其伪品[J].中药材,1994,17(6):23-24. [10]QING H L,SHANG Y J,ZHAO W,et al.Study on identification of coptischinensis franch by nuclear magnetic resonance spectroscopy[J].Chinese Traditional and Herbal Drugs,2000,31(1):48-50.秦海林,尚玉俊,赵伟,等.核磁共振氢谱法鉴别黄连的研究[J].中草药,2000,31(1):48-50. [11]KRISHNAMURTHY K.CRAFT (complete reduction to amplitude frequency table)-robust and time-efficient bayesian approach for quantitative mixture analysis by NMR[J].Magn Reson Chem,2013,51(12):821-829. [12]BRADLEY S A,SMITKA T A,RUSSELL D J,et al.Quantitative NMR analysis of complex mixtures using craft (complete reduction to amplitude frequency table) method[J].Current Metabolomics,2015,3(1):21-31. [13]YU S,GUO Q S,WANG H L,et al.Simultaneous determination of resveratrol and polydatin in polygonum cuspidatum by quantitative nuclear magnetic resonance spectroscopy[J].Chinese Journal of Analytical Chemistry,2015(1):69-74.禹珊,郭强胜,王会琳,等.定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量[J].分析化学,2015(1):69-74. [14]PETER P,ADEK Z A,WILL G.NMR-assignments of n-acylaporphlne alkaloids from Tinospora crispa[J].Planta Med,1992,58(2):184-187. [15]LE GALL G,COLQUHOUN I J,DAVIS A L,et al.Metabolite profiling of tomato (lycopersiconesculentum) using 1H NMR spectroscopy as a tool to detect potential unintended effects following a genetic modification[J].J Agric Food Chem,2003,51(9):2447-2456. [16]KOJIMA H,TOMINAGA H,SATO S,et al.Pentacyclic triterpenoids from Prunella Yulgaris[J].Phytochemistry,1987,26(4):1107-1111. [17]JUNG Y,LEE J,KWON J,et al.Discrimination of the geographical origin of beef by 1H NMR based metabolomics[J].J Agric Food Chem,2010,58(19):10458-10466. [18]贾伟.医学代谢组学[M].上海:上海科学技术出版社,2011,193-221. [19]OKADA T,AFENDI F M,ALTAF-UI-AMIN M,et al.Metabolomics of medicinal plants:the importance of multivariate analysis of analytical chemistry data[J].Curr Comput Aided Drug Des,2010,6(3):179-196. [20]SACCENTI E,TIMMERMAN E.Approaches to sample size determination for multivariate data:applications to PCA and PLS-DA of omics data[J].J Proteome Res.2016,15(8):2379-2393. [21]STEWART S,IVY M A,ANSLYN E V.The use of principal component analysis and discriminant analysis in differential sensing routines[J].Chem Soc Rev,2014,43(1):70-84.

杜仲的核磁共振指纹图谱研究

NMR Fingerprints of Eucommia ulmoides Oliver

PDF

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价

[1]	刘颖, 袁斌华, 章浩伟. 便携式磁共振多源射频脉冲发生器设计[J]. 波谱学杂志, 2025, 42(3): 285-298.
[2]	江超超, 姚守权, 徐俊成, 蒋瑜. 宽频磁共振微线圈设计[J]. 波谱学杂志, 2025, 42(3): 299-307.
[3]	舒炜. B超和MRI在胎儿骨骼异常中的诊断价值分析[J]. 波谱学杂志, 2025, 42(3): 265-274.
[4]	隋美菊, 张磊, 王瑞芳, 骆盈盈, 李莎, 丘茂松, 徐秋怡, 陈代钦, 陈世桢, 周欣. MRI示踪的纳米酶用于级联反应增强的免疫治疗[J]. 波谱学杂志, 2025, 42(3): 231-248.
[5]	寇新慧, 张玉冰. 含氨基酸单元手性脲的对映体识别性能研究[J]. 波谱学杂志, 2025, 42(3): 221-230.
[6]	马滢雪, 赵晏强, 杨晓冬, 蒋滨, 陶诚. 我国高场及超高场磁共振成像设备研制和市场化的机遇与挑战[J]. 波谱学杂志, 2025, 42(3): 334-344.
[7]	李科言, 程鑫, 陈俊飞, 曹丽, 黄臻, 刘朝阳. 用于低场NMR的低噪声前置放大器研制[J]. 波谱学杂志, 2025, 42(3): 321-333.
[8]	汤世豪, 杨谨毓, 徐雅洁, 王亚, 彭博文, 高宇昊, 杨晓冬. 一种用于低场磁共振波谱仪的圆极化线圈设计[J]. 波谱学杂志, 2025, 42(3): 308-320.
[9]	何丰丞李明道吕兴龙姚守权蒋瑜. 掌上型核磁共振谱仪控制台软件设计[J]. 波谱学杂志, 0, (): 0-0.
[10]	郑佳琪王意浓元思文尹田鹏. 4-异丙氧基-1-(三氟乙酰基)萘的结构解析和NMR数据完整归属[J]. 波谱学杂志, 0, (): 0-0.
[11]	陈博, 刘泉, 马蕾, 陈淑年, 贾亚琦, 朱斌, 郭俊旺. 基于Simulink的连续波电子顺磁共振信号处理与检测仿真研究[J]. 波谱学杂志, 2025, 42(2): 174-183.
[12]	顾佳佳, 王远军. 混合注意力和多尺度模块的阿尔茨海默病分类方法[J]. 波谱学杂志, 2025, 42(2): 103-116.
[13]	左冰玉, 石丽莉, 宋佳, 赵阳, 李倩. 雌激素、肿瘤标志物联合DCE-MRI在宫颈癌诊断及临床分期中的应用[J]. 波谱学杂志, 2025, 42(2): 164-173.
[14]	孟靖欣, 王远军. 基于扩散磁共振的大脑浅表白质纤维束研究进展[J]. 波谱学杂志, 2025, 42(2): 205-220.
[15]	陈静聪, 冉凤伟, 章浩伟, 刘颖. 基于DCGAN的脑膜瘤与听神经瘤检测模型优化方法研究[J]. 波谱学杂志, 2025, 42(2): 117-129.