CN1324044C - Ursolic acid extracting method from privet leaf - Google Patents

Ursolic acid extracting method from privet leaf Download PDF

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Publication number
CN1324044C
CN1324044C CNB2003101114798A CN200310111479A CN1324044C CN 1324044 C CN1324044 C CN 1324044C CN B2003101114798 A CNB2003101114798 A CN B2003101114798A CN 200310111479 A CN200310111479 A CN 200310111479A CN 1324044 C CN1324044 C CN 1324044C
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China
Prior art keywords
ethanol
reflux
glossy privet
ursolic acid
weight
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Expired - Fee Related
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CNB2003101114798A
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Chinese (zh)
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CN1544455A (en
Inventor
袁晓
袁萍
周东斌
谢志坚
陈友丽
何志祥
吴建辉
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Sanjiu huangshi pharmaceutical factory
Wuhan Botanical Garden of CAS
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Sanjiu huangshi pharmaceutical factory
Wuhan Institute of Botany of CAS
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Priority to CNB2003101114798A priority Critical patent/CN1324044C/en
Publication of CN1544455A publication Critical patent/CN1544455A/en
Application granted granted Critical
Publication of CN1324044C publication Critical patent/CN1324044C/en
Anticipated expiration legal-status Critical
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Abstract

The present invention discloses a method for extracting ursolic acid from ligustrum leaves. The method comprises the following procedures: ligustrum leaves and water are heated and boiled in an extracting tank, and the water solution is filtered off; ethanol with low solubility is added to ligustrum leaves and heated for reflux for some time, and the liquid in the extracting tank is filtered under reduced pressure into a concentration tank; the ethanol is recovered; ethanol with high solubility is added to ligustrum leaves and heated for reflux; the liquid in the extracting tank is filtered under reduced pressure into the concentration tank; the ethanol is recovered so that ethanol extract with high solubility is obtained; ethanol with identical high solubility is added and mixed with the ethanol extract with high solubility; appropriate amount of active carbon is added and heated for reflux; filter liquor is obtained after filtration under reduced pressure; water is added to adjust the concentration of ethanol in the filter liquor; filter liquor after adjustment is treated by heating, reflux, cooling, filtration, drying and residue filtration to obtain a product of ursolic acid. The present invention has the advantages of convenient technology and convenient operation; obtained ursolic acid is a pharmaceutical raw material for reducing blood lipid and treating cardiovascular disease; the present invention is suitable for large-scale industrial production.

Description

A kind of method of from Leaf of Glossy Privet, extracting ursolic acid
Technical field
The present invention relates to the extraction of Leaf of Glossy Privet ursolic acid, more specifically relate to a kind of method of from Leaf of Glossy Privet, extracting ursolic acid.
Background technology
Ursolic acid (ursolic acid) has another name called ursonic acid, and urson belongs to triterpene compound.It is very wide in distributed in nature, as is present in the leaf, fruit of Du Juan flower section plant black bearberry, and in the leaf of goatweed royal paulownia, and the leaf of oleaceae plant glossy privet is medium.Ursolic acid has biological effect widely, and it has significantly stable and cooling effect to central nervous system; External all have anti-microbial activity to G+ and G-bacterium and yeast.In addition, it also has the effect of anti-diabetic, antiulcer agent and blood fat reducing.In recent years the Shu Faxian ursolic acid not only has resistant function to multiple carcinogenic, short cancer thing, and for example P388 and L1210 leukemia cell, A549 human lung adenocarcinoma cell have the growth of inhibition effect to multiple malignant cell.In addition, ursolic acid also can induce the F9 teratocarcinoma cell to become endoderm cell and angiogenesis inhibitor.Huangshi 999 Pharmaceutical Co., Ltd. is that raw material is researched and developed into national Chinese medicine two kind new medicines with the Leaf of Glossy Privet extract, this product is used for the treatment of hyperlipidemia, has comprehensive comprehensive adjustment human body lipid function, through clinical study, can reduce TC, TG, TC-HDL-C/HDL-C, rising HDL, and can reduce the level of LDL-C, can improve simultaneously the hepatic and renal YIN deficiency, tinnitus, dry that hyperlipemia causes, sleep less, diseases such as irritated irritability, limb fiber crops are afraid of cold, constipation, blood fat curative effect total effective rate is 95%.From the structure bone is the research that raw material extracts ursolic acid technology, modern chemical industries such as Sun Laijiu, 2000,20 (9) 47-48.Present chemosynthesis ursolic acid complex process, the cost height.
Summary of the invention
The objective of the invention is to be to provide a kind of method of extracting ursolic acid from Leaf of Glossy Privet, this method is easy, and is easy to operate, and cost is low, extracts ursolic acid from Leaf of Glossy Privet, is used for Medicines and Health Product, the treatment cardiovascular disease.
In order to achieve the above object, the present invention adopts following technical scheme, the steps include:
1, add dry Leaf of Glossy Privet in extractor, add dry Leaf of Glossy Privet weight 15-20 water doubly again, boiled 40-60 minute, the elimination aqueous solution repeats this step 2-3 time;
2, add dry Leaf of Glossy Privet weight 3-6 30-45% ethanol doubly again in extractor, reflux 1-2 hour, the liquid filtration under diminished pressure in the extractor in concentration tank, is repeated this step 2-3 time, it is stand-by to reclaim ethanol;
3, add dry Leaf of Glossy Privet weight 3-6 70-88% ethanol doubly again in extractor, reflux 1-2 hour, the liquid filtration under diminished pressure in the extractor to concentration tank, is repeated this step 2-3 time, get ethanol extract behind the concentrated filtrate, it is stand-by to reclaim ethanol;
4, add dry Leaf of Glossy Privet weight 0.25-0.5 78-88% ethanol doubly, add ethanol extract weight 0.5-1 activated carbon doubly in the concentration tank of ethanol extract, reflux 1-2 hour, 45-55 ℃ of filtration under diminished pressure gets filtrate, repeating this step adds the above-mentioned filtrate 1 time except that " add dry Leaf of Glossy Privet weight 0.25-0.5 doubly 78-88% ethanol " changes into, filtrate enters in the hold-up vessel, adds water the alcohol concn of filtrate in the hold-up vessel is transferred to 50-75% by 78-88%, gets the 50-75% ethanolic soln;
5, with 50-75% ethanolic soln reflux 10-25 minute, be cooled to 20-25 ℃, cooled liquid was placed below 0 ℃ 10-14 hour, and filtration under diminished pressure gets filter residue, dry filter residue, the ursolic acid product.
The present invention compared with prior art has the following advantages and effect: this method is easy, and is easy to operate, and cost is low, and technological method is grasped easily, is particularly suitable for scale operation.Content of ursolic acid just can reach more than 40% by above step.The annual people who suffers from cardiovascular diseases of China becomes the trend of rapid increase, and ursolic acid has unique curative effect of reducing blood-fat, is treatment cardiovascular diseases medical material, and not only technology is simple, obtains from natural plants extensive again.In addition, extract the used plant Leaf of Glossy Privet of ursolic acid and distribution widely, aboundresources are arranged in China.
Embodiment
1, add the dry Leaf of Glossy Privet of 1kg in extractor, add 20kg water again, boiled 45 minutes, the elimination aqueous solution repeats this step and removes " adding in the 1kg drying Leaf of Glossy Privet extractor " 3 times;
2, add 6kg30% ethanol again in extractor, reflux 2 hours in concentration tank, repeats this step 2 time with the liquid filtration under diminished pressure in the extractor, and it is stand-by to reclaim ethanol;
3, add 6kg85% ethanol again in extractor, reflux 1 hour to concentration tank, repeats this step 2 time with the liquid filtration under diminished pressure in the extractor, behind the concentrated filtrate ethanol extract, it is stand-by to reclaim ethanol;
4, add 0.5kg85% ethanol, add the 0.03kg activated carbon in the concentration tank of ethanol extract, reflux 1 hour, 55 ℃ of filtration under diminished pressure get filtrate, repeating this step adds the above-mentioned filtrate 1 time except that " adding 0.5kg85% ethanol " changes into, filtrate enters in the hold-up vessel, adds water the alcohol concn of filtrate in the hold-up vessel is transferred to 70% by 85%, gets 70% ethanolic soln;
5, with 70% ethanolic soln reflux 15 minutes, be cooled to 20 ℃, cooled liquid was placed below 0 ℃ 12 hours, and filtration under diminished pressure gets filter residue, and dry filter residue promptly gets ursolic acid product 0.014kg, and yield is 1.4%, and content of ursolic acid is greater than 40%.

Claims (1)

1, a kind of method of extracting ursolic acid from Leaf of Glossy Privet comprises the following steps:
A, add dry Leaf of Glossy Privet in extractor, add dry Leaf of Glossy Privet weight 15-20 water doubly again, boiled 40-60 minute, the elimination aqueous solution repeats this step 2-3 time;
B, add in the dry Leaf of Glossy Privet weight 3-6 30-45% extraction using alcohol jar doubly again, reflux 1-2 hour, the liquid filtration under diminished pressure in the extractor in concentration tank, is repeated this step 2-3 time, recovery ethanol is stand-by;
C, add dry Leaf of Glossy Privet weight 3-6 70-88% ethanol doubly in extractor again, reflux 1-2 hour, the liquid filtration under diminished pressure in the extractor in concentration tank, is repeated this step 2-3 time, behind the concentrated filtrate ethanol extract, recovery ethanol is stand-by;
D, add dry Leaf of Glossy Privet weight 0.25-0.5 78-88% ethanol doubly, add ethanol extract weight 0.5-1 activated carbon doubly in the concentration tank of ethanol extract, reflux 1-2 hour, 45-55 ℃ of filtration under diminished pressure gets filtrate, repeating this step adds the above-mentioned filtrate 1 time except that " add dry Leaf of Glossy Privet weight 0.25-0.5 doubly 78-88% ethanol " changes into, filtrate enters in the hold-up vessel, adds water the alcohol concn of filtrate in the hold-up vessel is transferred to 50-75% by 78-88%;
E, with the ethanolic soln reflux of 50-75% 10-25 minute, cooling, cooled solution was placed below 0 ℃ 10-14 hour, filtration under diminished pressure gets filter residue, dry filter residue promptly gets the ursolic acid product.
CNB2003101114798A 2003-11-28 2003-11-28 Ursolic acid extracting method from privet leaf Expired - Fee Related CN1324044C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CNB2003101114798A CN1324044C (en) 2003-11-28 2003-11-28 Ursolic acid extracting method from privet leaf

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CN1324044C true CN1324044C (en) 2007-07-04

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102028698B (en) * 2009-12-02 2012-05-23 山东省中医药研究院 Medicine for treating colon cancer and preparation method thereof
CN102512426A (en) * 2011-12-26 2012-06-27 哈尔滨医科大学 Application of ursolic acid in preparation of health care product with effects of weight loss and fatty liver improvement
CN107325150B (en) * 2017-07-24 2020-05-12 广东药科大学 Method for extracting ligustrum lucidum ursolic acid by supercritical carbon dioxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1358733A (en) * 2001-12-20 2002-07-17 武汉大学 Process for extracting ursolic acid from fructus ligustri lucidi leaf
CN1453289A (en) * 2003-05-19 2003-11-05 西安交通大学 Process of extracting and separating ursolic acid from plant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1358733A (en) * 2001-12-20 2002-07-17 武汉大学 Process for extracting ursolic acid from fructus ligustri lucidi leaf
CN1453289A (en) * 2003-05-19 2003-11-05 西安交通大学 Process of extracting and separating ursolic acid from plant

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
从毛泡桐叶中提取分离熊果酸的新工艺研究 韩晶等人,西北大学学报(自然科学版),第33卷第3期 2003 *
从毛泡桐叶中提取分离熊果酸的新工艺研究 韩晶等人,西北大学学报(自然科学版),第33卷第3期 2003;以陆英为原料提取乌索酸的工艺研究 李开泉等人,中成药,第25卷第5期 2003 *
以陆英为原料提取乌索酸的工艺研究 李开泉等人,中成药,第25卷第5期 2003 *

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