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.
The

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 1:

[0025] Take 10kg dried Ligustrum lucidum (Oleanolic acid content 1.2%, Ligustrum lucidum content 2.4%), pulverize, and dynamically extract with 60L 70% ethanol at 50°C for 1 hour, filter, add 60L 70% ethanol to extract once, combine the two Add 1000 g of activated carbon for injections to the secondary liquid, decolorize for 2 hours under stirring and reflux, filter through activated carbon, concentrate under reduced pressure to 30% alcohol content, and place for crystallization. Separate the crystals and mother liquor to obtain 260g of crystals, dissolve them with 1820ml times 90% (containing 1% sodium hydroxide) ethanol, filter, add hydrochloric acid to the solution to adjust the pH neutrality, filter the precipitates, and use 90% ethanol for the precipitates After refluxing, dissolving and standing for crystallization twice, 87 g of oleanolic acid content was 98.1% after drying.

[0026] The above-mentioned mother liquor continues to recover ethanol, cool an...

Example Embodiment

[0027] Example 2:

[0028] Take 10kg of dried Ligustrum lucidum (Oleanolic acid content 1.2%, Ligustrum lucidum content 2.4%), crush it, and use 40L 80% ethanol at 70°C for dynamic extraction for 1 hour, extract three times, combine the liquid and add 1500g of activated carbon for injections. Stir and decolorize under reflux for 1 hour, filter through activated carbon, concentrate under reduced pressure to an alcohol content of 40%, and leave to crystallize. Separate the crystals and mother liquor to obtain 255g crystals, dissolve them with 2000ml times 80% (containing 0.5% sodium hydroxide) ethanol, and filter, add hydrochloric acid to the solution to adjust the pH neutrality, filter the precipitates, and use 95% ethanol for the precipitates After refluxing to dissolve and standing for crystallization twice, 85 g of oleanolic acid content was 98.2% after drying.

[0029] The above-mentioned mother liquor continues to recover ethanol, cool and filter, add to the HZ816 resin column...

Example Embodiment

[0030] Example 3:

[0031] Take 10kg of dried Ligustrum lucidum (Oleanolic acid content 1.2%, Ligustrum lucidum content 2.4%), pulverize, and dynamically extract with 50L 70% ethanol at 60°C for 1.5 hours, extract three times, combine the liquid and add 1500g activated carbon for injections. Stir and decolorize under reflux for 2 hours, filter through activated carbon, concentrate under reduced pressure to 50% alcohol content, and place to crystallize. Separate the crystals and mother liquor to obtain 245g crystals, dissolve them with 2200ml times 90% (containing 0.5% sodium hydroxide) ethanol, filter, add hydrochloric acid to the solution to adjust the pH neutrality, filter the precipitates, and use 99% ethanol for the precipitates After refluxing, dissolving and standing for crystallization twice, it was dried to obtain 83 g of oleanolic acid with 98.3% content.

[0032] Continue to recover ethanol from the above mother liquor, let it cool and filter, add it to the SPD-100 resin...

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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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