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Method for extracting and purifying oleanolic acid and Ligustrum lucidum Ait

A technology of oleanolic acid and privetin, applied in chemical instruments and methods, organic chemistry, steroidal compounds, etc., can solve the problems of cumbersome process, difficult treatment and filtration, high cost, etc., and achieve easy operation, simple process, The effect of low production cost

Inactive Publication Date: 2010-09-01
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Acid-base water treatment Filtration is difficult Column chromatography can separate oleanolic acid and similar impurities well, but this method has a small amount of sample and is not suitable for large-scale industrial production
For example, patent 200710020063.3 "A Method for Separating and Purifying Oleanolic Acid and Ursolic Acid", which uses membrane separation, chromatographic column and acid-base treatment. The process is cumbersome and the yield is low and the cost is high.
There are very few studies on the separation methods of privetin, and most of them are in the laboratory
[0008] At the same time, the method of extracting and purifying oleanolic acid and privet glycosides from Ligustrum lucidum has not been reported, and most of them are laboratory research projects, which are not suitable for industrial production. (I)", expounding the separation process of the active ingredients of Ligustrum lucidum, but this process is difficult to scale up production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Get 10kg of dry Ligustrum lucidum (oleanolic acid content 1.2%, privetin content 2.4%), pulverize, use 60L70% ethanol 50 ℃ of dynamic extraction for 1 hour, filter, add 60L70% ethanol to extract again, combine two Add 1000 g of activated carbon for injections to the secondary liquid, decolorize it under stirring and reflux for 2 hours, filter the activated carbon, concentrate under reduced pressure until the alcohol content is 30%, and stand to crystallize. Separate crystals and mother liquor to obtain 260g crystals, stir and dissolve with 1820ml times 90% (containing 1% sodium hydroxide) ethanol, filter, add hydrochloric acid to the solution to adjust pH neutrality, filter out the precipitate, and use 90% ethanol for the precipitate Reflux to dissolve and place to crystallize twice, and dry to obtain 87 g of oleanolic acid with a content of 98.1%.

[0026] Continue to recover ethanol from the above mother liquor, let it cool and filter, add HZ816 resin column for adsor...

Embodiment 2

[0028] Get 10kg of dry Ligustrum lucidum (oleanolic acid content 1.2%, privetin content 2.4%), pulverize, use 40L80% ethanol 70 ℃ of dynamic extractions for 1 hour, extract three times, add 1500g activated carbon for injections into the combined liquid, Decolorize under stirring and reflux for 1 hour, filter activated carbon, concentrate under reduced pressure until the alcohol content is 40%, and stand to crystallize. Separate crystals and mother liquor to obtain 255g crystals, stir and dissolve with 2000ml times 80% (containing 0.5% sodium hydroxide) ethanol, filter, add hydrochloric acid to the solution to adjust pH neutrality, filter out precipitates, and dissolve precipitates with 95% ethanol Reflux to dissolve and place to crystallize twice, and dry to obtain 85 g of oleanolic acid with a content of 98.2%.

[0029] Continue to recover ethanol from the above mother liquor, let it cool and filter, add HZ816 resin column for adsorption, first wash the resin column with 6BV ...

Embodiment 3

[0031] Get 10kg of dry Ligustrum lucidum (oleanolic acid content 1.2%, privetin content 2.4%), pulverize, use 50L70% ethanol 60 ℃ of dynamic extractions for 1.5 hours, extract three times, add 1500g active carbon for injections into the combined liquid, Decolorize under stirring and reflux for 2 hours, filter activated carbon, concentrate under reduced pressure until the alcohol content is 50%, and stand to crystallize. Separate crystals and mother liquor to obtain 245g crystals, stir and dissolve with 2200ml times 90% (containing 0.5% sodium hydroxide) ethanol, filter, add hydrochloric acid to the solution to adjust pH neutrality, filter out the precipitate, and use 99% ethanol for the precipitate Reflux to dissolve and place to crystallize twice, and dry to obtain 83 g of oleanolic acid with a content of 98.3%.

[0032] The above mother liquor continues to recover ethanol, let it cool and filter, add SPD-100 resin column for adsorption, first wash the resin column with 7BV o...

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PUM

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Abstract

The invention relates to a method for separating and purifying oleanolic acid and Ligustrum lucidum Ait, which easily realizes industrialization. The method comprises the following process steps: ethanol extraction, separation of the oleanolic acid and the Ligustrum lucidum Ait in low alcohol, alkali alcohol treatment, ethanol dissolution, crystallization and purification of the oleanolic acid, macroporous resin chromatography and extraction, crystallization and purification of Ligustrum lucidum Ait. The method for producing the oleanolic acid and the Ligustrum lucidum Ait has the advantages of simple process, high utilization rate of raw materials and low cost.

Description

Technical field: [0001] The invention relates to a process for extracting and purifying oleanolic acid and privetin, in particular to a process for simultaneously extracting and purifying oleanolic acid and privetin from Ligustrum lucidum. Background technique: [0002] Ligustrum lucidum is the dried and mature fruit of Ligustrum lucidum Ait., a plant of Oleaceae, which is a commonly used Chinese medicinal material. Its function is to strengthen the body, nourish the liver and kidney, improve eyesight and black hair. Clinically, it is mainly used to strengthen the waist and knees, strengthen the muscles and bones, black beard and hair, and treat internal heat due to yin deficiency, dizziness, and tinnitus. The highly fat-soluble oleanolic acid is considered to be the main active ingredient of Ligustrum lucidum for its antioxidant effect, and the water-soluble split ring iridoid glycosides are also important antioxidant active ingredients in Ligustrum lucidum. Strong physiol...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H17/04C07H1/08
Inventor 李法庆张翼刘东锋
Owner 苏州宝泽堂医药科技有限公司
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