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Purification process of geniposide

A technology of geniposide and process, applied in the field of medicine, can solve the problems of low solubility and low extraction rate of geniposide, achieve the effects of shortening the production cycle, increasing the extraction rate, and simplifying the separation and purification process

Inactive Publication Date: 2010-11-10
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

Tu Shenghui's published document "Research on the Refining of Geniposide from Gardeniae Jasminoides by Macroporous Adsorption Resin" uses ethyl acetate extraction and HPD100 macroporous resin adsorption, and the solubility of geniposide in cold ethyl acetate is not high, so the extraction rate is relatively low. Low

Method used

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  • Purification process of geniposide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 5kg of gardenia medicinal material, crush it into coarse powder, put it into an acid-resistant extraction tank; add 90L and 75L of hydrochloric acid solution of pH2.5 to soak twice, each time for 3h, after filtering the extract, add 40L55% and 30L80 of the dregs respectively % ethanol was heated and refluxed for 2 times, each time for 1h, and the extracts were combined four times after hot filtration, passed through an activated carbon column for decolorization, collected the decolorized solution, adjusted to pH 6.5, filtered, and the filtrate was concentrated under reduced pressure to 25L to obtain a concentrated solution Use 10kg of 80-mesh polyamide to separate, and carry out gradient elution with 10:1:1, 6:1:1, 2:1:1, 1:2:1 chloroform-acetone-water in sequence, and the pressure is controlled at 0.05Mpa. Collect the eluent, recover the solvent under reduced pressure to 1 / 9 of the original volume, and stand still to obtain coarse crystals. Saturate and dissolve th...

Embodiment 2

[0024] Take 10kg of gardenia medicinal material, crush it into a coarse powder, put it into an acid-resistant extraction tank; add 200L, 250LpH2 formic acid solution to soak twice, each time for 2h, after the extract is filtered, add 100L50%, 70L65%, 60L of 80% ethanol was heated and refluxed for 3 times, each time for 0.5h. After hot filtration, the extracts were combined five times, passed through an activated carbon column for decolorization, collected the decolorized solution, adjusted to pH 6, filtered, and the filtrate was concentrated under reduced pressure to 75L to obtain a concentrated solution Use 15kg of 100-mesh polyamide to separate, and carry out gradient elution with 10:1:1, 6:1:1, 2:1:1, 1:2:1 chloroform-acetone-water in sequence, and the column pressure is controlled at 0.06Mpa , collect the eluent, recover the solvent under reduced pressure to 1 / 10 of the original volume, stand still to obtain coarse crystals, dissolve the coarse crystals in saturated pyridin...

Embodiment 3

[0026] Take 50kg of gardenia medicinal material, crush it into a coarse powder, put it into an acid-resistant extraction tank; add 1200L and 750L of pH3 sulfuric acid solution to soak twice, each time for 4 hours, after the extract is filtered, add 500L of 60% and 300L of 80% of the dregs Ethanol was heated and refluxed for 2 times, each time for 2 hours. After hot filtration, the extracts were combined four times, passed through an activated carbon column for decolorization, collected the decolorized solution, adjusted to pH 7, filtered, and the filtrate was concentrated under reduced pressure to 350L. The obtained concentrated solution was used with 100kg of 120 Separation of polyamide, followed by gradient elution with 10:1:1, 6:1:1, 2:1:1, 1:2:1 chloroform-acetone-water, the column pressure was controlled at 0.04Mpa, and the eluted Liquid, the solvent was recovered under reduced pressure to 1 / 9 of the original volume, and the coarse crystals were obtained by standing still....

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Abstract

The invention discloses a purification process of geniposide. In the method, cape jasmine fruits serve as raw materials are soaked in acidic water, then ethanol refluxing extraction, decoloration and polyamide column absorption are performed, eluent is concentrated to a small volume to precipitate coarse crystals, the coarse crystals are dissolved in pyridine-hot ethyl acetate, and white crystals are obtained by recrystallization. The advancement and practical value of the method lie in that the purity of the geniposide prepared by the method is high and that the method is simple and practical.

Description

Technical field: [0001] The invention relates to a process for purifying geniposide, which belongs to the field of medicine. Background technique: [0002] Geniposide [0003] Molecular formula: C 17 h 24 o 10 ;Molecular weight: 388.366; [0004] Molecular Structure: [0005] [0006] Physical and chemical properties: white crystal. It reacts positively to α-naphthol, hydroxamic acid and ferric chloride. The melting point is 163°C to 164°C. Soluble in water, soluble in ethanol, insoluble in petroleum ether. [0007] Gardenia is the dry and mature fruit of Gardenia jasminoides Ellis, a Rubiaceae plant. Gardenia is a commonly used traditional Chinese medicine recorded in the previous editions of the Pharmacopoeia. It has the effects of purging fire and relieving restlessness, clearing away heat and diuresis, cooling blood and detoxifying. For febrile disease upset, jaundice red urine, blood stranguria astringent pain, blood heat spit at the nose, conjunctival cong...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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