Triptophenolide preparation method

Abstract

The invention relates to a triptophenolide preparation method, in particular to a method for extracting and purifying triptophenolide by means of the supercritical CO2 extraction technology. The method includes: using triperygium hypoglaucum as raw materials, extracting by means of supercritical CO2, using 90% ethanol as entrainer, collecting extract liquor, using ethyl acetate for extracting after ethanol is recovered, subjecting ethyl acetate extractum obtained by condensing ethyl acetate extract liquor to magnesium oxide short-range column chromatography, using n-hexane-acetone for gradient elution, and crystallizing. The triptophenolide preparation method is mild in condition, reasonable in process, capable of realizing quick extraction and separative purification, and easy for industrialization.

Description

technical field

[0001] The invention belongs to the technical field of extraction and separation of effective parts of traditional Chinese medicines, and in particular relates to a method for extracting and preparing rafenolactone from Kunming mountain crabapple. Background technique

[0002] Kunming mountain crabapple, also known as hexagonal rattan, has its roots used as medicine, mainly containing alkaloids, diterpene lactones, etc. It has the effects of expelling wind and dehumidification, relaxing meridians and activating collaterals, clearing heat and detoxifying, and is widely used in the treatment of rheumatoid arthritis, systemic lupus erythematosus and chronic nephritis.

[0003] Triptophenolide is a diterpenoid compound with the molecular formula C 20 h 24 o 3 , molecular weight 312.41, colorless needle crystal, mp.232-233°C, CAS number: 74285-86-2. It mainly exists in Euonymus family plants, such as Kunming mountain crabapple Tripterygium hypoglaucum (Levl.)...

Examples

Embodiment 1

[0017] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 37°C, the extraction pressure is 16MPa, CO 2 The flow rate is 4ml / g crude drug / min, the pressure and temperature of the kettle are kept constant, 90% ethanol is introduced as an entrainer, the extraction time is 2h, the temperature of the separation kettle is 32°C, and the pressure is 4MPa. The extract is collected and analyzed, and recovered under reduced pressure. Ethanol, extracted 4 times with ethyl acetate equivalent to 3 times the amount of ethanol extract, collected and combined ethyl acetate extracts, concentrated under reduced pressure to obtain ethyl acetate extract; ethyl acetate extract and magnesium oxide were mixed in a mass ratio of 1 :1 mixed and dried, then take new magnesia column, put the mixed magnesia on it, and use n-hexane-acetone mixed solvent in sequence according to the volume ratio of 10:1, 5:1, 3:1, 1:1 Carr...

Embodiment 2

[0019] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 48°C, the extraction pressure is 23MPa, CO 2 The flow rate is 3ml / g crude drug / min, keep the kettle pressure and temperature constant, feed 90% ethanol as entrainer, extract time is 1.5h, the temperature of the separation kettle is 40°C, the pressure is 6MPa, collect and analyze the extract, depressurize Recover ethanol, extract twice with ethyl acetate equivalent to 2 times the amount of ethanol extract, collect and combine ethyl acetate extracts, concentrate under reduced pressure to obtain ethyl acetate extract; mix ethyl acetate extract and magnesium oxide by mass ratio Mix and dry at 1:1.5, then take new magnesia and pack it into a column, put the mixed magnesia on it, use n-hexane-acetone mixed solvent in sequence according to volume ratio 10:1, 5:1, 3:1, 1: 1 for elution, collect the refenolactone eluent, recover the reagent, co...

Embodiment 3

[0021] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 45°C, the extraction pressure is 36MPa, CO 2 The flow rate is 4ml / g crude drug / min, the pressure and temperature of the kettle are kept constant, 90% ethanol is introduced as an entrainer, the extraction time is 3h, the temperature of the separation kettle is 33°C, and the pressure is 8MPa. The extract is collected and analyzed, and recovered under reduced pressure. Ethanol, extracted 3 times with ethyl acetate equivalent to 4 times the amount of ethanol extract, collected and combined ethyl acetate extracts, concentrated under reduced pressure to obtain ethyl acetate extract; ethyl acetate extract and magnesium oxide were mixed in a mass ratio of 1 : 2.5 Mix and dry, then take new magnesia column, put the mixed magnesia on it, use n-hexane-acetone mixed solvent in sequence according to volume ratio 10:1, 5:1, 3:1, 1:1 Carry out elutio...

technical field

[0001] The invention belongs to the technical field of extraction and separation of effective parts of traditional Chinese medicines, and in particular relates to a method for extracting and preparing rafenolactone from Kunming mountain crabapple. Background technique

[0002] Kunming mountain crabapple, also known as hexagonal rattan, has its roots used as medicine, mainly containing alkaloids, diterpene lactones, etc. It has the effects of expelling wind and dehumidification, relaxing meridians and activating collaterals, clearing heat and detoxifying, and is widely used in the treatment of rheumatoid arthritis, systemic lupus erythematosus and chronic nephritis.

[0003] Triptophenolide is a diterpenoid compound with the molecular formula C 20 h 24 o 3 , molecular weight 312.41, colorless needle crystal, mp.232-233°C, CAS number: 74285-86-2. It mainly exists in Euonymus family plants, such as Kunming mountain crabapple Tripterygium hypoglaucum (Levl.)...

Examples

Embodiment 1

[0017] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 37°C, the extraction pressure is 16MPa, CO 2 The flow rate is 4ml / g crude drug / min, the pressure and temperature of the kettle are kept constant, 90% ethanol is introduced as an entrainer, the extraction time is 2h, the temperature of the separation kettle is 32°C, and the pressure is 4MPa. The extract is collected and analyzed, and recovered under reduced pressure. Ethanol, extracted 4 times with ethyl acetate equivalent to 3 times the amount of ethanol extract, collected and combined ethyl acetate extracts, concentrated under reduced pressure to obtain ethyl acetate extract; ethyl acetate extract and magnesium oxide were mixed in a mass ratio of 1 :1 mixed and dried, then take new magnesia column, put the mixed magnesia on it, and use n-hexane-acetone mixed solvent in sequence according to the volume ratio of 10:1, 5:1, 3:1, 1:1 Carr...

Embodiment 2

[0019] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 48°C, the extraction pressure is 23MPa, CO 2 The flow rate is 3ml / g crude drug / min, keep the kettle pressure and temperature constant, feed 90% ethanol as entrainer, extract time is 1.5h, the temperature of the separation kettle is 40°C, the pressure is 6MPa, collect and analyze the extract, depressurize Recover ethanol, extract twice with ethyl acetate equivalent to 2 times the amount of ethanol extract, collect and combine ethyl acetate extracts, concentrate under reduced pressure to obtain ethyl acetate extract; mix ethyl acetate extract and magnesium oxide by mass ratio Mix and dry at 1:1.5, then take new magnesia and pack it into a column, put the mixed magnesia on it, use n-hexane-acetone mixed solvent in sequence according to volume ratio 10:1, 5:1, 3:1, 1: 1 for elution, collect the refenolactone eluent, recover the reagent, co...

Embodiment 3

[0021] Get Kunming Mountain Begonia 20kg pulverization process, add supercritical CO 2 In the extraction kettle, the extraction temperature is 45°C, the extraction pressure is 36MPa, CO 2 The flow rate is 4ml / g crude drug / min, the pressure and temperature of the kettle are kept constant, 90% ethanol is introduced as an entrainer, the extraction time is 3h, the temperature of the separation kettle is 33°C, and the pressure is 8MPa. The extract is collected and analyzed, and recovered under reduced pressure. Ethanol, extracted 3 times with ethyl acetate equivalent to 4 times the amount of ethanol extract, collected and combined ethyl acetate extracts, concentrated under reduced pressure to obtain ethyl acetate extract; ethyl acetate extract and magnesium oxide were mixed in a mass ratio of 1 : 2.5 Mix and dry, then take new magnesia column, put the mixed magnesia on it, use n-hexane-acetone mixed solvent in sequence according to volume ratio 10:1, 5:1, 3:1, 1:1 Carry out elutio...