Extraction and purification method of incanone

A purification method, the technology of orchid vanilla, applied in the separation/purification of carbonyl compounds, organic chemistry, etc., to achieve the effect of increasing extraction rate, shortening extraction time and high efficiency

Inactive Publication Date: 2014-10-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Through literature search, there is no report on the extraction of vanillone by enzymatic hydrolysis and negative pressure cavitation suspension solid-liquid extraction in China.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Crush orchid vanilla through a 20-mesh sieve, weigh 3kg, add 3 times V / W amylase solution for enzymolysis for 18 hours, the concentration of the biological enzyme solution is 2g / L, to obtain enzymolysis raw materials, add 15L of 75% ethanol solution After mixing, negative pressure cavitation suspension solid-liquid extraction is carried out to obtain an extract, which is concentrated to obtain an extract;

[0020] 2) Suspend the extract in saturated brine to make the concentration reach 1g / ml, extract twice with ethyl acetate at 70°C, the amount of ethyl acetate is 2 / 3, 1 / 3 of the volume of saturated brine solution , combined the ethyl acetate extracts and washed with anhydrous Na 2 SO 4 After dehydration, it was concentrated under reduced pressure to near dryness to obtain ethyl acetate extract;

[0021] 3) The extract was purified by silica gel column chromatography, eluted with a mixed solvent of petroleum ether-ethyl acetate at a ratio of 5:5, 5:8, and 5:10, an...

Embodiment 2

[0023] 1) Crush orchid vanilla through a 20-mesh sieve, weigh 3kg, add 4 times V / W cellulose enzyme solution for enzymolysis for 12 hours, the concentration of the biological enzyme solution is 2g / L, to obtain the raw material for enzymolysis, add 30L of 85% ethanol After the solutions are mixed, negative-pressure cavitation suspension solid-liquid extraction is carried out to obtain an extract, which is then concentrated to obtain an extract;

[0024] 2) Suspend the extract in saturated brine to make the concentration up to 1.5g / ml, and extract with ethyl acetate three times at 50°C, the amount of ethyl acetate is 2 / 3, 1 / 3 of the volume of saturated brine solution 2, 1 / 3, combined ethyl acetate extract, with anhydrous Na 2 SO 4 After dehydration, it was concentrated under reduced pressure to near dryness to obtain ethyl acetate extract;

[0025] 3) The extract was purified by silica gel column chromatography, eluted with a mixed solvent of petroleum ether-ethyl acetate at a...

Embodiment 3

[0027] 1) Crush orchid vanilla through a 20-mesh sieve, weigh 3kg, add 4 times of V / W pectin enzyme solution for enzymolysis for 24 hours, the concentration of the biological enzyme solution is 2g / L, to obtain the raw material for enzymolysis, add 21L of 80% ethanol After the solutions are mixed, negative-pressure cavitation suspension solid-liquid extraction is carried out to obtain an extract, which is then concentrated to obtain an extract;

[0028] 2) Suspend the extract in saturated brine to make the concentration up to 1.5g / ml, and extract it three times with ethyl acetate at 60°C, the amount of ethyl acetate is 2 / 3, 1 / 3 of the volume of saturated brine solution 2, 1 / 3, combined ethyl acetate extract, with anhydrous Na 2 SO 4 After dehydration, it was concentrated under reduced pressure to near dryness to obtain ethyl acetate extract;

[0029] 3) The extract was purified by silica gel column chromatography, eluted with a mixed solvent of petroleum ether-ethyl acetate a...

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PUM

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Abstract

The invention discloses an extraction and purification method of incanone. The method comprises the steps of (1) smashing caryopteris incana, adding a biological enzyme solution to carry out enzymolysis to obtain an enzymolysis raw material, after adding 5-10 times of 75-85% ethanol solution to mix, carrying out negative-pressure cavitation hybrid suspension solid-liquid extraction to obtain an extracting solution, and concentrating to obtain an extract; (2) suspending the extract in saturated salt water, extracting 2-3 times by using ethyl acetate, merging ethyl acetate extracting solutions, and carrying out vacuum concentration to be approximately dry after dehydrating by using anhydrous Na2SO4 to obtain an ethyl acetate extract; (3) purifying the extract by using silica column chromatography, carrying out gradient elution by using a petroleum ether-ethyl acetate mixed solvent, eluting by using ethyl acetate and ethanol, collecting the fraction, recovering a reagent, and drying to obtain incanone. When being used for extracting and purifying incanone, the method disclosed by the invention is simple in operation, high in efficiency, high in product purity and suitable for industrial preparation.

Description

technical field [0001] The invention belongs to the technical field of extraction of natural substances, and relates to an extraction and purification method of orchid vanillone. Background technique [0002] Incanone, CAS No. 180282-91-1, molecular formula C 20 h 28 o 5 , molecular weight 348.46, structural formula is [0003] [0004] Orchid vanilla is the whole plant of Verbenaceae (Verbenaceae) orchid vanilla Caryopteris incana (Thunb.) Miq., 4.7% of orchid vanillone in orchid vanilla. The functions of orchid vanilla are mainly to relieve wind and relieve exterior syndrome, eliminate phlegm and relieve cough, dissipate stasis and relieve pain. Clinically, it is mainly used for upper respiratory tract infection, whooping cough, bronchitis, rheumatic joint pain, gastroenteritis, bruises, swelling and pain, postpartum congestion and abdominal pain; external use for snake bites, eczema, and itchy skin. Studies have shown that blue vanillone has cytotoxic activity, sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/747C07C45/79
CPCC07C45/78C07C2603/22
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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