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Method for preparing high-purity carnosic acid by continuous medium pressure column chromatography

A carnosic acid, high-purity technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of difficulty in expanding production and equipment conditions, and achieve the effect of facilitating continuous industrial production

Inactive Publication Date: 2010-10-06
NORTHEAST FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The rosemary antioxidant containing carnosic acid is prepared by supercritical CO2, which is still the crude extract of carnosic acid, and currently limited by equipment conditions, it is difficult to expand production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 400g of 15% carnosic acid crude product was stirred and refluxed, dissolved in 2L ethyl acetate, cooled, and the insoluble matter was filtered off, and 8kg of 100-200 mesh silica gel with a moisture content of 12% was suspended in ethyl acetate to drive out air bubbles, and evenly added to In a glass chromatography column with an effective column length of 350 cm and an inner diameter of 5 cm, the above-mentioned dissolved carnosic acid sample is put on the head of the column with a plunger solvent pump, and then pumped into ethyl acetate to elute, and the fractions are collected in sections, monitored by HPLC, and combined For the effluent with a content of more than 92%, the eluent was recovered under reduced pressure to obtain 65 g of chromatographic products, which were dissolved by adding 130 mL of petroleum ether under reflux, cooled and crystallized, and the crystals were recrystallized once with n-hexane, filtered under reduced pressure, and dried to obtain 55 g ...

Embodiment 2

[0029] 400g 18% carnosic acid crude product was stirred and refluxed, dissolved in 2L ethyl acetate, cooled, and the insoluble matter was filtered off, and 8 kg of 200-300 mesh silica gel with a moisture content of 12% was suspended in ethyl acetate, and the air bubbles were removed, and evenly added to In a glass chromatography column with an effective column length of 120 cm and an inner diameter of 10 cm, the above-mentioned dissolved carnosic acid sample is put on the head of the column with a plunger solvent pump, and then pumped into ethyl acetate to elute, and the fractions are collected in sections, monitored by HPLC, and combined For the effluent with a content of more than 92%, the eluent was recovered under reduced pressure to obtain 68 g of chromatographic products, which were dissolved by adding 130 mL of cyclohexane under reflux, cooled and crystallized, and the crystallized product was recrystallized once with n-hexane, filtered under reduced pressure, and dried. ...

Embodiment 3

[0031] 80g of 16% carnosic acid crude product was stirred and refluxed, dissolved in 2L ethyl acetate, cooled, and the insoluble matter was filtered off, and 8 kg of 300-400 mesh silica gel with a water content of 12% was suspended in ethyl acetate, and the air bubbles were removed, and evenly added to In a glass chromatography column with an effective column length of 30cm and an inner diameter of 20cm, the above-mentioned dissolved carnosic acid sample is put on the column head with a plunger solvent pump, and then pumped into ethyl acetate to elute, and the fractions are collected in sections, monitored by HPLC, and combined For the effluent with a content of more than 92%, the eluent was recovered under reduced pressure to obtain 13 g of chromatographic products, which were dissolved by adding 130 mL of n-hexane under reflux, cooled and crystallized, and the crystallized product was recrystallized once with n-hexane, filtered under reduced pressure, and dried to obtain 10.5...

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Abstract

The invention discloses a method for preparing high-purity carnosic acid by continuous medium pressure column chromatography. The method prepares the carnosic acid with the purity of over 98 percent by using a carnosic acid raw material with the content of not lower than 15 percent. The method comprises the following steps of: dissolving a coarse carnosic acid product into ethyl acetate, filtering the insoluble substances to obtain a column filling sample, and filling a column by using silica gel, namely dispersing the silica gel by using the ethyl acetate and then wetly filling the silica gel into the column; after filling, feeding liquid into the column through a plunger solvent pump by using the ethyl acetate as eluent, collecting the eluted fractions section by section, concentrating the fractions under reduced pressure till the eluent is dryly reclaimed to obtain a chromatographic product, reusing the reclaimed eluent, re-crystallizing the chromatographic product by using a hydrocarbon solvent, and drying a crystallized product under reduced pressure to obtain a pure carnosic acid product with the purity of over 98 percent, wherein after the ethyl acetate is reclaimed under reduced pressure, the mother solution serving as a column chromatography raw material can be re-purified, the used chromatographic column is regenerated by using a mixed solvent containing ethyl acetate and ethanol, the ethyl acetate is balanced by a balancing agent, and the balanced chromatographic column can be reused for over 30 times. The method has the main characteristics that the purification process has no pollution, all solvents can be recycled and the method is convenient for industrial continuous production.

Description

Technical field: [0001] The invention relates to the field of natural product chemistry, in particular to a method for preparing high-purity carnosic acid by continuous medium-pressure column chromatography. Background technique: [0002] Carnosic acid is the main fat-soluble antioxidant component in Rosemary (Rosmarinus officinalis L.) of Labiatae. Rosemary is native to countries along the Mediterranean Sea, and is now widely cultivated all over the world. In recent years, it has been planted on a large scale in Guangxi, Yunnan, Zhejiang, Guizhou, Hainan and Xinjiang in my country. As a natural fat-soluble antioxidant, carnosic acid is widely used in the fields of medicine, food processing and cosmetics. [0003] The Chinese patent with the publication number CN1441030 introduces a method for extracting natural antioxidants from rosemary, which directly uses fresh rosemary grass to obtain rosemary essential oil and antioxidant-containing raw materials through steam distill...

Claims

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Application Information

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IPC IPC(8): C07C62/32C07C51/47
Inventor 祖元刚杨磊祖柏实刘芳刘婷婷马春慧赵春建孙震王涵
Owner NORTHEAST FORESTRY UNIVERSITY
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