Quality Evaluation of Branches of <italic style="font-style: italic">Juglans mandshurica</italic> by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents

Hong LIU; Xiao-chang JU; Feng-shuo SHI; Xue DI; Hong-he XIAO; Hui ZHANG; Yan-jun ZHAI; Tian-min WANG

doi:10.13422/j.cnki.syfjx.20202448

您当前的位置：

首页 >

文章列表页 >

Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents

Pharmacy Fundamentals | 更新时间：2021-04-02

- Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 27, Issue 9, Pages: 137-146(2021)
- 作者机构：
  
  辽宁中医药大学药学院，辽宁大连 116600
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20202448
  CLC： R22;R931;R28;O657
- Received：05 August 2020，
  
  Published Online：20 October 2020，
  
  Published：05 May 2021
- 稿件说明：
移动端阅览
刘宏,鞠晓畅,石丰硕等.HPLC-DAD指纹图谱结合HPLC-Q-TOF-MS/MS成分表征评价胡桃楸枝的质量[J].中国实验方剂学杂志,2021,27(09):137-146.

LIU Hong,JU Xiao-chang,SHI Feng-shuo,et al.Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents[J].Chinese Journal of Experimental Traditional Medical Formulae,2021,27(09):137-146.
刘宏,鞠晓畅,石丰硕等.HPLC-DAD指纹图谱结合HPLC-Q-TOF-MS/MS成分表征评价胡桃楸枝的质量[J].中国实验方剂学杂志,2021,27(09):137-146. DOI： 10.13422/j.cnki.syfjx.20202448.

LIU Hong,JU Xiao-chang,SHI Feng-shuo,et al.Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents[J].Chinese Journal of Experimental Traditional Medical Formulae,2021,27(09):137-146. DOI： 10.13422/j.cnki.syfjx.20202448.

摘要

目的

建立胡桃楸枝的高效液相色谱法（HPLC）指纹图谱，并对不同产地、不同采收期的胡桃楸枝样品进行质量分析。

方法

采用Agilent Poroshell 120 SB-C

色谱柱（2.1 mm×100 mm，2.7 μm），流动相0.2%甲酸水溶液（A）-0.2%甲酸乙腈溶液（B）梯度洗脱（0~5 min，5%~10%B；5~25 min，10%~16%B；25~40 min，16%~22%B；40~45 min，22%~45%B；45~50 min，45%~65%B；50~52 min，65%~100%B；52~55 min，100%B），流速0.3 mL·min

-1

，柱温30 ℃，检测波长270 nm。采用相似度评价、聚类分析、主成分分析和偏最小二乘法-判别分析对指纹图谱数据进行统计分析。采用HPLC串联四极杆飞行时间质谱法（HPLC-Q-TOF-MS/MS）表征胡桃楸枝中的化学成分，选择电喷雾离子源（ESI），在负离子检测模式下进行质谱采集，MS扫描范围

100~1 700，MS/MS扫描范围

50~1 700。

结果

40批胡桃楸枝样品中确定了19个共有峰，其相似度处于0.430~0.995，其中春冬季节（4月，5月，12月）采收样品相似度均>0.90，大部分夏季（7~9月）采收样品相似度较低。多元统计分析后发现样品根据采收季节分为两类，而不同产地样品无明显分类规律，说明采收期是影响胡桃楸枝样品质量的主要因素之一。春冬季节采收样品中大部分化学成分的含量高于夏季采收的样品，与夏季采收样品相比，春冬季采收样品质量较好。22个色谱峰是造成不同季节采收样品差异性的主要成分。通过HPLC-Q-TOF-MS/MS表征了胡桃楸枝中的83个化学成分，其中鞣质类成分49个，有机酸类成分7个，萘衍生物14个，黄酮类成分1个，蒽衍生物6个，木脂素类成分2个，二芳基庚烷类成分3个，糖类成分1个。鉴别了13个共有峰和19个不同季节采收样品的差异峰，多为鞣质类化合物。

结论

建立的HPLC指纹图谱可用于胡桃楸枝的质量分析，鞣质是胡桃楸枝中的主要成分。采收期对胡桃楸枝质量影响较大。

Abstract

Objective

To establish a high performance liquid chromatography （HPLC） fingerprint of branches of

Juglans mandshurica

and to evaluate the quality of the samples from different producing areas and in different harvest periods.

Method

Chromatographic separation was performed on an Agilent Poroshell 120 SB-C

column （2.1 mm×100 mm， 2.7 μm） for gradient elution with mobile phase of 0.2% formic acid solution （A）-0.2% formic acid acetonitrile solution （B）（0-5 min， 5%-10%B； 5-25 min， 10%-16%B； 25-40 min， 16%-22%B； 40-45 min， 22%-45%B； 45-50 min， 45%-65%B； 50-52 min， 65%-100%B； 52-55 min， 100%B） at a flow rate of 0.3 mL·min

-1

. The column temperature was 30 ℃ and the detection wavelength was 270 nm. The quality of branches of

Juylans mandshurica

was evaluated by similarity evaluation， cluster analysis， principal component analysis and partial least squares-discriminant analysis. The chemical constituents of the samples were identified by HPLC coupled with quadrupole time-of-flight mass spectrometry （HPLC-Q-TOF-MS/MS）. The mass spectrometry was conducted in negative ion mode with electrospray ionization（ESI）. Data were acquired over a range of

100-1 700 for MS and

50-1 700 for MS/MS.

Result

A total of 19 common peaks were confirmed in 40 batches of samples， and the similarity ranged from 0.430 to 0.995， of which the similarity of samples collected in spring and winter seasons （April， May and December） was greater than 0.90， while the similarity of most samples collected in summer （July to September） was low. Multivariate statistical analysis showed that the samples were divided into two groups according to the harvest time， but there was no obvious classification rule for the samples from different producing areas. The contents of most constituents in the samples collected in spring and winter were higher than those collected in summer. The result illustrated that different harvest periods had great influence on the quality of branches of

mandshurica

. Compared with the samples collected in summer， the quality of samples collected in spring and winter was better. A total of 22 peaks were proved to be the main constituents that contributed to the difference between samples collected in different seasons. A total of 83 chemical components were identified by HPLC-Q-TOF-MS/MS， including 49 tannins， 7 organic acids， 14 naphthalene derivatives， 1 flavonoid， 6 anthracene derivatives， 2 lignans， 3 diarylheptanoids and 1 saccharide. Totally 13 common peaks were identified. Of the peaks that contributed to discriminate samples collected in different season， 19 peaks were identified and most of them were tannins.

Conclusion

The established HPLC fingerprint can provide useful information for the quality evaluation of branches of

mandshurica

. Tannin is the main constituents in the samples. Harvest period has great influence on the quality of branches of

mandshurica

关键词

Keywords

references

中国科学院《中国植物志》编辑委员会 . 中国植物志［M］. 北京：科学出版社， 1982 ： 33 .

张洪娟，桑树荣 . 高奎滨用青龙衣制剂治疗肿瘤用药经验［J］. 黑龙江中医药， 2000 （ 2 ）： 62 .

朱蕴娟，钱卫星 . 东方云芝胶囊联合复方木鸡冲剂治疗Ⅱ期原发性肝癌32例临床报告［J］. 上海中医药杂志， 1994 （ 10 ）： 43 .

曹颖林，金和筠，王玉坤，等 . 复方木鸡口服液抑瘤作用的研究［J］. 中成药， 1996 ， 18 （ 8 ）： 30 - 32 .

李英春 . 核桃楸叶的化学成分及其抗肿瘤活性的研究［D］. 长春：吉林大学， 2007 .

王少东，脱朝伟 . 核桃楸青果皮抗肿瘤作用的药理研究［J］. 辽宁中医杂志， 1990 （ 11 ）： 37 - 39 .

姚大雷，姜丽君，周薇，等 . 胡桃楸根氯仿提取物对小鼠S180肉瘤抑制作用的研究［J］. 中药材， 2009 ， 32 （ 4 ）： 595 - 596 .

王添敏，俞文婕，付莹，等 . 胡桃楸茎枝含药鸡蛋对小鼠H22肝癌实体瘤的抑制作用［J］. 现代药物与临床， 2017 ， 32 （ 3 ）： 365 - 369 .

古乐，曹秀格，李岩 . 胡桃楸树皮抗肿瘤有效成分对H 22 荷瘤小鼠T细胞亚群的影响［J］. 科技导报， 2016 ， 34 （ 11 ）： 37 - 41 .

孙冬雪，郭雄飞，阿拉腾图雅，等 . 青龙衣中化学成分及其体外抗肿瘤活性研究［J］. 中国中药杂志， 2019 ， 44 （ 11 ）： 2278 - 2282 .

张宇驰，葛鹏玲，陈家红，等 . 青龙衣萘醌类化学成分及其抗癌活性研究进展［J］. 中草药， 2019 ， 50 （ 9 ）： 2251 - 2256 .

孙国东，霍金海，程团，等 . 基于UPLC-Q-TOF/MS技术的胡桃楸叶化学成分分析［J］. 中药材， 2017 ， 40 （ 5 ）： 1123 - 1129 .

刘国如，徐康平，申健，等 . 胡桃楸根化学成分研究［J］. 中南药学， 2009 ， 7 （ 9 ）： 644 - 646 .

辽宁省食品药品监督管理局 . 辽宁省中药材标准：第1册［M］. 沈阳：辽宁科学技术出版社， 2009 ： 144 .

王添敏，孙晓丽，彭雪，等 . 胡桃楸的根、茎枝、叶和果皮中总鞣质的含量测定［J］. 中国中药杂志， 2011 ， 36 （ 1 ）： 32 - 36 .

王添敏，翟延君，徐士钊，等 . 胡桃楸茎枝中胡桃醌含量的动态变化［J］. 中国医院药学杂志， 2012 ， 32 （ 15 ）： 1166 - 1168 .

WANG T M ， LIU J ， YI T ， et al . Multiconstituent identification in root，branch，and leaf extracts of Juglans mandshurica using ultra high performance liquid chromatography with quadrupole time of flight mass spectrometry ［J］. J Sep Sci ， 2017 ， 40 （ 17 ）： 3440 - 3452 .

王琼珺，谢伟容，邰艳妮，等 . 基于Q-Marker成分定性与定量的双黄连制剂质量评价［J］. 中国实验方剂学杂志， 2017 ， 23 （ 18 ）： 36 - 46 .

WANG T M ， FU Y ， YU W J ， et al . Identification of polar constituents in the decoction of Juglans mandshurica and in the medicated egg prepared with the decoction by HPLC-Q-TOF MS 2 ［J］. Molecules ， 2017 ， 22 （ 9 ）： 1452 .

Views

下载量

CSCD

Alert me when the article has been cited

提交

Tools

Publicity Resources

Examination of Quality Characteristics of Rehmannia glutinosa Leaves by Different Fixation Methods Based on Fingerprint and Antioxidant Activity

Spectrum-effect Relationship Analysis Between HPLC Fingerprint and Immunomodulatory Activity of Zhenqi Fuzheng Granules

Quality Evaluation of Lycii Cortex and Roasted Lycii Cortex Based on Fingerprint and Content Determination

Quality Evaluation of Wine-processed Scutellariae Radix from Different Origins Based on Thermal Analysis Technology， Fingerprint and Content Determination

Research on Material Basis of Homologous and Heterogeneous Effect of Aurantii Fructus Immaturus and Aurantii Fructus Based on Total Statistical Moment Analysis and Molecular Connectivity Index

Related Author

CUI Jinpeng

GENG Xiaotong

CHENG Mengjuan

LI Weifeng

ZHANG Juan

LIU Qingpu

LEI Jingwei

XIE Caixia

Related Institution

Henan Provincial Engineering Technology Research Center for Quality Control and Evaluation of Traditional Chinese Medicine， Henan University of Chinese Medicine

Xinyang Agriculture and Forestry University

The Sixth Affiliated Hospital of Guangzhou Medical University， Qingyuan People′s Hospital

Jilin Modern Chinese Medicine Engineering and Research Center Co. Ltd.

Institute of Chinese Materia Medica，China Academy of Chinese Medical Sciences

AI问答

Postal code：100700
Tel：010-84076882 Email：syfjx_2010@188.com
Technical support is provided by Beijing Founder electronics co., LTD 京ICP备11006657号-10 京公网安备11010802024621
It is recommended to read the content of this site in Chrome&IE9+. Please switch to extreme mode in browser 360.
Cookies We use cookies to help provide and enhance our service and tailor content. By continuing, you agree to the use of cookies.

⁰

Quality Evaluation of Branches of Juglans mandshurica by HPLC-DAD Fingerprint Combined with HPLC-Q-TOF-MS/MS Characterization of Constituents

DOI：10.13422/j.cnki.syfjx.20202448

摘要

Abstract

关键词

Keywords

references