Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by <sup>1</sup>H-NMR Combined with Multivariate Statistical Analysis

WEI Xianwen; CHEN Lanying; MENG Xiaowei; ZHU Qing; YU Honghua; ZHENG Qiwan; REN Jiahui; LIN Lihua; LIU Ronghua

doi:10.13422/j.cnki.syfjx.20230149

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Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by ¹H-NMR Combined with Multivariate Statistical Analysis

更新时间：2023-06-02

- Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by ¹H-NMR Combined with Multivariate Statistical Analysis
  增强出版
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 29, Issue 13, Pages: 173-179(2023)
- 作者机构：
  
  1.江西中医药大学药学院，南昌 330004
  2.江西中医药大学中药固体制剂制造技术国家工程研究中心，南昌 330006
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20230149
  CLC： R22;R28;R931;O657
- Received：08 October 2022，
  
  Published Online：23 November 2022，
  
  Published：05 July 2023
- 稿件说明：
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危先文,陈兰英,孟晓伟等.¹H-NMR技术结合多元统计分析鉴别降香及其伪品[J].中国实验方剂学杂志,2023,29(13):173-179.

WEI Xianwen,CHEN Lanying,MENG Xiaowei,et al.Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by ¹H-NMR Combined with Multivariate Statistical Analysis[J].Chinese Journal of Experimental Traditional Medical Formulae,2023,29(13):173-179.
危先文,陈兰英,孟晓伟等.¹H-NMR技术结合多元统计分析鉴别降香及其伪品[J].中国实验方剂学杂志,2023,29(13):173-179. DOI： 10.13422/j.cnki.syfjx.20230149.

WEI Xianwen,CHEN Lanying,MENG Xiaowei,et al.Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by ¹H-NMR Combined with Multivariate Statistical Analysis[J].Chinese Journal of Experimental Traditional Medical Formulae,2023,29(13):173-179. DOI： 10.13422/j.cnki.syfjx.20230149.

摘要

目的

采用核磁共振氢谱（

H-NMR）技术结合多元统计分析建立降香及其伪品的鉴别方法。

方法

获得降香及其伪品的

H-NMR图谱，建立全成分信息并转化为数据矩阵，检测条件为以含0.03%四甲基硅烷（TMS）的氘代二甲基亚砜（DMSO-d

）为溶剂，恒温298 K（1 K=-272.15 ℃），脉冲间隔1.00 s，谱宽12 019.23 Hz，扫描数16次，采样时间1.08 s。对降香及其伪品数据矩阵进行相似度考察和层次聚类分析（HCA），采用正交偏最小二乘法-判别分析（OPLS-DA）对数据矩阵进行分析，找出降香与其伪品之间的差异性成分；建立OPLS-DA类别变量值模型，设定降香类别变量值为1，降香伪品类别变量值为0，阈值±0.3，用于市售降香的真伪鉴别；以OPLS-DA得分图确定市售降香中伪品的种类，并通过薄层色谱法（TLC）进行验证。

结果

相似度分析与HCA结果表明，降香与其伪品之间差异明显；OPLS-DA发现降香与其伪品显著性差异成分为反式-橙花叔醇；建立的类别变量值模型可成功对市售降香进行真伪鉴别；OPLS-DA得分图结果显示，市售降香中存在交趾黄檀心材和斜叶黄檀心材，并与TLC验证结果相吻合。

结论

市场上存在以交趾黄檀心材和斜叶黄檀心材代替降香出售的现象，

H-NMR图谱结合多元统计分析能有效区分降香及其伪品，可为降香及其伪品的鉴别提供参考。

Abstract

Objective

To establish the identification method of Dalbergiae Odoriferae Lignum（DOL） and its counterfeits by nuclear magnetic resonance hydrogen spectrum（

H-NMR） combined with multivariate statistical analysis.

Method

H-NMR spectra of DOL and its counterfeits were obtained by NMR， and the full composition information was established and transformed into a data matrix， and the detection conditions were as follows：taking dimethyl sulfoxide-d

（DMSO-d

） containing 0.03% tetramethylsilane（TMS） as the solvent， the constant temperature at 298 K（1 K=-272.15 ℃）， pulse interval of 1.00 s， spectrum width of 12 019.23 Hz， the scanning number of 16 times， and the sampling time of 1.08 s. Similarity examination and hierarchical cluster analysis（HCA） were performed on the data matrix of DOL and its counterfeits， and orthogonal partial least squares-discriminant analysis（OPLS-DA） was used to analyze the data matrix and identify the differential components between them. In the established OPLS-DA category variable value model， the category variable value of DOL was set as 1， and the category variable value of the counterfeits was set as 0， and the threshold was set as ±0.3， in order to identify the commercially available DOL. The OPLS-DA score plot was used to determine the types of counterfeits in commercially available DOL， and it was verified by thin layer chromatography（TLC）.

Result

The results of similarity analysis and HCA showed that there was a significant difference between DOL and its counterfeits. OPLS-DA found that the differential component between DOL and its counterfeits was

trans

-nerolidol. The established category variable value model could successfully identify the authenticity of the commercially available DOL. The results of the OPLS-DA score plot showed that there were heartwood of

Dalbergia pinnata

and

D. cochinchinensis

in the commercially available DOL， and were consistent with the TLC verification results.

Conclusion

There is a phenomenon that heartwood of

D. pinnata

and

D. cochinchinensis

are sold as DOL in the market.

H-NMR combined with multivariate statistical analysis can effectively distinguish DOL and its counterfeits， which can provide a reference for the identification of them.

关键词

Keywords

references

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Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by 1H-NMR Combined with Multivariate Statistical Analysis

DOI：10.13422/j.cnki.syfjx.20230149

摘要

Abstract

关键词

Keywords

references

Identification of Dalbergiae Odoriferae Lignum and Its Counterfeits by ¹H-NMR Combined with Multivariate Statistical Analysis