LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin

Miao-kai LYU; Zhi-peng HUO; Yuan-xue LIU; Yu-ting TIAN; Yu WANG; Chun-yong WU; Yi HE

doi:10.13422/j.cnki.syfjx.20200847

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LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin

Pharmacy Fundamentals | 更新时间：2020-09-09

- LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 26, Issue 14, Pages: 152-163(2020)
- 作者机构：
  
  1.中国药科大学药学院，南京 210009
  2.天士力控股集团有限公司研究院现代中药开发中心，天津 300410
  3.天士力医药集团股份有限公司创新中药关键技术国家重点实验室，天津 300410
  4.天津中医药大学中药学院，天津 301617
  5.天津大学药物科学与技术学院，天津 300072
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20200847
  CLC： R22;R914;R28;C37;O657
- Published Online：31 December 2019，
  
  Published：20 July 2020
- 稿件说明：
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吕苗凯,霍志鹏,刘元雪等.地榆成分在D101型大孔树脂和聚酰胺树脂上保留行为的LCMS-IT-TOF分析[J].中国实验方剂学杂志,2020,26(14):152-163.

LYU Miao-kai,HUO Zhi-peng,LIU Yuan-xue,et al.LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(14):152-163.
吕苗凯,霍志鹏,刘元雪等.地榆成分在D101型大孔树脂和聚酰胺树脂上保留行为的LCMS-IT-TOF分析[J].中国实验方剂学杂志,2020,26(14):152-163. DOI： 10.13422/j.cnki.syfjx.20200847.

LYU Miao-kai,HUO Zhi-peng,LIU Yuan-xue,et al.LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(14):152-163. DOI： 10.13422/j.cnki.syfjx.20200847.

摘要

目的

基于柱色谱技术和液相色谱-离子阱-飞行时间质谱（LCMS-IT-TOF）技术展开地榆的物质基础研究，分析地榆水提液中不同成分在D101型大孔树脂和聚酰胺树脂上的分布规律。

方法

通过D101型大孔树脂和聚酰胺树脂分离地榆水提液，使用LCMS-IT-TOF检测，使用ACQUITY UPLC HSS T3色谱柱（2.1 mm×100 mm，1.8 μm），流动相水-乙腈梯度洗脱，流速0.3 mL·min

-1

，柱温30 ℃，采用电喷雾离子源（ESI），正、负离子模式采集数据，质谱扫描范围

100~1 200，根据精确相对分子质量及质谱碎片等信息并结合文献研究，鉴定地榆水提液的上样流出液和洗脱液中化学成分。提取各样品中质谱峰强度数据，绘制成分在各流分中分布热图，直观比较各成分的洗脱规律。

结果

D101型大孔树脂和聚酰胺树脂的富集和分离作用明显，鞣质类成分主要集中于大孔树脂上样流出液及其水洗脱液中，三萜类成分主要分布在大孔树脂90%乙醇洗脱液中。在地榆水提液的流出液和洗脱液中，共鉴定出63个化合物，其中6-

-galloylnorbergerin，3-

-galloylnorbergerin，2

6-乙酰氧基-5

7-二羟基-8-甲氧基色原酮，鞣花酸-4-吡喃阿拉伯糖苷或其异构体，2-甲基-3-乙酰氧基-苯并呋喃-5

-硫酸酯6个成分在地榆中为首次发现。

结论

该方法能够快速准确地鉴定地榆水提液经过柱色谱分离后的成分分布，为探索地榆药效成分及其作用机制提供了实验依据。

Abstract

Objective

To study on the material basis of Sanguisorbae Radix by column chromatography and liquid chromatography-ion trap-time-of-flight mass spectrometry (LCMS-IT-TOF)

and analyze the distribution of different components in

Sanguisorbae Radix water extract on D101 macroporous resin and polyamide resin.

Method

Sanguisorbae Radix water extract was separated by D101 macroporous resin and polyamide resin

and LCMS-IT-TOF was used for detection

chromatography separation was achieved on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm

1.8 μm) with the mobile phase consisted of water (A) and acetonitrile (B) for gradient elution (0-10 min

5%-20%B; 10-18 min

20%-35%B; 18-23 min

35%-50%B; 23-28 min

50%-90%B; 28-30 min

90%B; 30-33 min

90%-5%B; 33-35 min

5%B)

the flow rate was 0.3 mL·min

-1

the column temperature was 30 ℃. Data acquisition was carried out in electrospray ionization (ESI) under the positive and negative ion modes

the scanning range was

100-1 200. According to mass spectrometry data such as accurate molecular mass and fragment information

combined with literature

different chemical components in loading effluents and ethanol eluents of Sanguisorbae Radix water extract were identified. A heat map of the distribution of components in each fraction was drawn by extracting mass spectrum peak intensity data of each sample. The elution rules of various components were compared visually.

Result

The enrichment and separation of D101 macroporous resin and polyamide resin were obvious. Tannins in Sanguisorbae Radix water extract was mainly concentrated in loading effluent of macroporous resin and its water eluent

triterpenoids were mainly distributed in the 90% ethanol eluent of macroporous resin. In the above effluents and eluents

a total of 63 compounds (including isomers) were identified. Among them

6 compounds

ellagic acid-4-pyranoarabinoside or its isomer

-galloylnorbergerin

(6-acetyloxy-5

7-dihydroxy-8-methoxy-4-oxochromen-2-yl) acetate

ethyl 2-methyl-5

6-bis (sulfooxy) benzofuran-3- carboxylate were first discovered in Sanguisorbae Radix.

Conclusion

The method can quickly and accurately identify the distribution of components in aqueous extract of Sanguisorbae Radix after column chromatography

providing experimental basis for exploring the pharmacodynamic components and mechanism of Sanguisorbae Radix.

关键词

Keywords

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