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Selfheal quality control method

A quality control method and technology of Prunella vulgaris, applied in the field of traditional Chinese medicine, can solve the problems that it cannot be used as a characteristic component, the main pharmacological activity has not been reported, and the quality of the finished product of Prunella vulgaris preparation cannot be guaranteed.

Active Publication Date: 2010-06-23
GUANGZHOU XINGQUN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because ursolic acid exists not only in the fruit ears, but also in the roots, stems, leaves and other parts, unscrupulous manufacturers use the roots, stems and leaves of Prunella vulgaris as medicine for the parts of the fruit ears, resulting in the failure of the finished product of Prunella vulgaris quality not guaranteed
[Research on the content determination method of caffeic acid and rosmarinic acid in different parts of Prunella vulgaris, Zhang Lanzhen et al., Journal of Beijing University of Traditional Chinese Medicine, 30(5), 343-345] Using caffeic acid and rosmarinic acid as quality control indicators; These components also exist in different parts of Prunella vulgaris, such as roots, stems, leaves, and fruit ears, and cannot be used as the characteristic components of the medicinal part of Prunella vulgaris - the fruit ears specified in the "Chinese Pharmacopoeia"
[0005]The compound salviaflaside is extremely water-soluble, and it is a light yellow amorphous powder. The color development of ferric chloride-potassium ferricyanide and bromophenol blue is positive. Ranal is pink in color and is a caffeoyl depsipside compound. Its main pharmacological activity has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The component analysis of the different parts of Prunella vulgaris of embodiment 1

[0052] 1. Preparation of the test sample: Weigh 1g of the powder of Prunella vulgaris spicules, leaves, stems and roots respectively, weigh it accurately, add 10mL of methanol, ultrasonicate for 30min (power 250W, frequency 40kHz), take it out, let it stand, and let it cool , 0.22μm microporous membrane filtration for HPLC analysis.

[0053] 2. Chromatographic conditions: Chromatographic column: Agilent Eclipse XDB-C18 (4.6mm×250mm, 5μm); flow rate: 1.0mL.min -1 ; Detection wavelength: 290nm; Column temperature: 30° C.; Injection volume: 10 μL;

[0054] Table 1 Mobile phase system gradient

[0055]

[0056] 3. Results: figure 1 The results showed that the compound salviaflaside in the chromatographic peak (I) only exists in the fruit ears of Prunella vulgaris, and does not exist in the parts of roots, stems and leaves, and is a characteristic component of the medicinal material (f...

Embodiment 2

[0057] The separation example 1 of characteristic compound (I) salviaflaside in embodiment 2 Prunella vulgaris

[0058] 1. Extraction: Prunella vulgaris medicinal material, reflux extraction with 5 times the amount of 60% ethanol twice, each time for 1 hour, filter out the medicinal liquid after cooling, and recover to dryness;

[0059] 2. Separation: Knead and dissolve the recovered dry sample with water, extract with petroleum ether, and discard the extract; continue to extract the water part with chloroform, and then discard the extract. Then concentrate the water part to dryness, mix the sample with 60-100 mesh silica gel, put it on the silica gel column, and use chloroform, chloroform:methanol (9:1), chloroform:methanol:water (65:35:10), chloroform:methanol: Wash the column with water (60:40:10) to obtain Part1, Part2, Part3, and Part4; 3. Purification: dissolve the sample of Part4 with methanol water, put it on the ODS column, and elute with methanol:water (50:50) , to ...

Embodiment 3

[0060] Example 3 Separation example of characteristic compound (I) salviaflaside in Prunella vulgaris 21. Extraction: Get Prunella vulgaris medicinal material, use 5 times the amount of 60% ethanol to reflux extract twice, each time for 1h, filter the medicinal solution after cooling, and recycle to dryness ;

[0061] 2. Separation: Knead and dissolve the recovered dry sample with water, extract with petroleum ether, and discard the extract; continue to extract the water part with chloroform, and then discard the extract. Then concentrate the water part to dryness, mix the sample with 60-200 mesh silica gel, put it on the silica gel column, and use the solutions of chloroform, chloroform:methanol (9:1), chloroform:methanol:water (65:35) from low to high polarity respectively : 10), chloroform: methanol: water (60: 40: 10) was washed into the column to obtain Part1, Part2, Part3, and Part4;

[0062] 3. Purification: Dissolve the sample in Part4 with methanol water, put it on t...

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Abstract

The invention discloses a selfheal quality control method which is a high performance liquid chromatography and a thin layer chromatography the marker components of which contain compound salviaflaside. The high performance liquid chromatography comprises the following steps: preparation of comparison products: carbinol is used to dissolve the salviaflaside compound so as to prepare the comparison product solution of the salviaflaside compound; preparation of test product solution : selfheal medicinal material powder is taken to be precisely weighed, added with carbinol, and filtered by a microfiltration membrane to be used as the test product solution; and injection to a liquid chromatograph, determination and mobile phase: elution by acetonitrile acetic acid liquid. The thin layer chromatography comprises the following steps: rosmarinic acid of the comparison product solution and salviaflaside solution and the test product solution are respectively absorbed to be sampled on the same thin board, chloroform:carbinol:formic acid or chloroform: water are taken as developers, developing, taking and drying are carried out, vanillin concentrated sulphuric acid is used for developing, and heating is carried out until spots are clear. The method is simple and effective, and thereby preventing illegal producers from using roots, stems, leaves and other non-medical parts to substitute the cluster parts of the selfheal to be used for the medical purpose.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicines, in particular to a quality control method for Prunella vulgaris. Background technique [0002] Prunella vulgaris is the dried fruit ear of Prunella vulgaris L., a plant of Lamiaceae. It has the effects of clearing fire, improving eyesight, dispelling stagnation, and reducing swelling. It is used for conjunctival congestion and swelling, eye pain at night, headache and dizziness, scrofula, goiter, mastitis swelling and pain; goiter, lymph node tuberculosis, breast hyperplasia ,hypertension. [0003] Ursolic acid, oleanolic acid, rosmarinic acid, and caffeic acid are the main components of Prunella vulgaris, and there are certain contents in different parts of Prunella vulgaris, such as roots, stems, leaves, and fruit ears. [0004] The 2005 edition of "Chinese Pharmacopoeia" stipulates that the medicinal part of Prunella vulgaris is fruit ears, and the quality control index adopted i...

Claims

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Application Information

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IPC IPC(8): A61K36/536A61P27/02A61P35/00A61P15/14A61P9/12A61P25/00A61P29/00A61P1/08A61P5/14A61P31/06G01N30/02G01N30/90A61K131/00
Inventor 林丽美许招懂蒋莉娟方铁铮谭新花汝凤
Owner GUANGZHOU XINGQUN PHARMA
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