Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS<sup>E</sup> Technology

Hao-zhou HUANG; Min QIU; Jin-fa TANG; Meng-Qi LI; Hai-yan LIU; San-hu FAN; Peng TAN; Li HAN; Jun-zhi LIN; Ding-kun ZHANG

doi:10.13422/j.cnki.syfjx.20200848

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Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology

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

- Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 26, Issue 14, Pages: 143-151(2020)
- 作者机构：
  
  1.成都中医药大学药学院，西南特色中药资源国家重点实验室，成都 611137
  2.河南中医药大学第一附属医院，郑州 450000
  3.四川护理职业学院，成都 610100
  4.成都市三勒浆药业集团，成都 610000
  5.四川省中医药科学院国家中医药管理局中药质量生物评价重点研究室，成都 610041
  6.成都中医药大学附属医院，成都 610072
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20200848
  CLC： R22;R914;R28;R94;O657
- Published Online：31 December 2019，
  
  Published：20 July 2020
- 稿件说明：
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黄浩洲,仇敏,唐进法等.基于UPLC-Q-TOF-MS^E技术的三勒浆口服液上清液及沉淀部分化学成分分析[J].中国实验方剂学杂志,2020,26(14):143-151.

HUANG Hao-zhou,QIU Min,TANG Jin-fa,et al.Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(14):143-151.
黄浩洲,仇敏,唐进法等.基于UPLC-Q-TOF-MS^E技术的三勒浆口服液上清液及沉淀部分化学成分分析[J].中国实验方剂学杂志,2020,26(14):143-151. DOI： 10.13422/j.cnki.syfjx.20200848.

HUANG Hao-zhou,QIU Min,TANG Jin-fa,et al.Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(14):143-151. DOI： 10.13422/j.cnki.syfjx.20200848.

摘要

目的

分析三勒浆口服液上清液和沉淀部分的主要化学成分，为建立其质量标准与沉淀控制技术提供依据。

方法

使用UPLC-Q-TOF-MS

技术分别对分离后的上清液及沉淀部分化学成分进行定性分析，采用Waters ACQUITY UPLC BEH C

色谱柱（2.1 mm×100 mm，1.7 μm），流动相选择0.1%甲酸水溶液（A）-乙腈（B）梯度洗脱（0~1 min，2%B；1~2 min，2%~5%B；2~4 min，5%~7%B；4~6 min，7%~24%B；6~10 min，24%~42%B；10~12 min，42%~54%B；12~15 min，54%~76%B；15~18 min，76%~100%B），流速0.3 mL·min

-1

，柱温30 ℃，进样量2 μL。质谱分析采用电喷雾离子源（ESI），负离子模式下使用时间依赖型MS

方式采集样品质谱数据，采集范围

50~1 200（上清液）和

50~3 000（沉淀），通过对采集数据的保留时间、精确相对分子质量和二级质谱裂解碎片进行比对后鉴定化学成分。

结果

在三勒浆口服液上清液中共鉴定了61个化合物，包括鞣质类、酚酸类、黄酮类、氨基酸类、有机酸类、脂肪酸类等；沉淀中共鉴定了15个化合物，包括鞣质类、酚酸类、黄酮类、脂肪酸类等。

结论

三勒浆口服液的水解鞣质可能是该制剂潜在的沉淀物质基础，其沉淀物很可能是以鞣花酸和鞣红为主构成的复杂沉淀。建立的UPLC-Q-TOF-MS

可快速、全面地分析三勒浆口服液的化学成分，可为其物质基础、沉淀机制及质量控制等研究提供科学依据。

Abstract

Objective

To analyze the main chemical components in the supernatant and precipitate of Sanajon oral liquid

so as to provide basis for establishing its quality standard and precipitation control technology.

Method

UPLC-Q-TOF-MS

was used to analyze the chemical components in the supernatant and precipitate of this oral liquid. The analysis was performed on Waters ACQUITY UPLC BEH C

column (2.1 mm×100 mm

1.7 μm) with the mobile phase of 0.1% formic acid solution (A) and acetonitrile (B) for gradient elution (0-1 min

2%B; 1-2 min

2%-5%B; 2-4 min

5%-7%B; 4-6 min

7%-24%B; 6-10 min

24%-42%B; 10-12 min

42%-54%B; 12-15 min

54%-76%B; 15-18 min

76%-100%B)

the flow rate was set to 0.3 mL·min

-1

the column temperature was 30 ℃

the injection volume was 2 µL. The mass spectrographic analysis was used with electrospray ionization (ESI)

sample MS data was acquired by time-dependent MS

in negative ion mode

the collection range was

50-1 200 (supernatant) and

50-3 000 (precipitate). Then the chemical constituents were identified by the information of retention time

accurate relative molecular mass and secondary mass spectrum fragment.

Result

Totally 61 compounds were identified in the supernatant

including tannins

phenolic acids

flavonoids

amino acids

organic acids

fatty acids

etc. Totally 15 compounds were identified in the precipitate

including tannins

phenolic acids

flavonoids

fatty acids

etc.

Conclusion

The hydrolyzed tannin of Sanajon oral liquid may be the potential material basis of its precipitate

and its precipitate is likely to be a complex precipitate mainly composed of ellagic acid and tanned red. The established UPLC-Q-TOF-MS

can quickly and comprehensively analyze the chemical composition of Sanajon oral liquid

which can provide a scientific basis for the researches of its material basis

precipitation mechanism and quality control.

关键词

Keywords

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Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MSE Technology

DOI：10.13422/j.cnki.syfjx.20200848

摘要

Abstract

关键词

Keywords

references

Analysis of Chemical Components in Supernatant and Precipitate of Sanajon Oral Liquid Based on UPLC-Q-TOF-MS^E Technology