A kind of preparation method of high-purity corylides and dehydrocoylides

Abstract

The invention relates to a method for preparing high-purity costuslactone and dehydrocostus lactone through high-speed countercurrent chromatography, which comprises the following steps of: (1) preparing a proper solvent system, standing and demixing to obtain an upper phase and a lower phase; (2) selecting the upper phase as a fixed phase and the lower phase as a mobile phase, filling the fixed phase in a column of a countercurrent chromatograph, regulating the rotating speed of a main machine to be 600-1,000rpm, pumping the mobile phase into the column at a flow rate of 0.5-5.0ml / min, and sampling through a sampling valve after the whole system is dynamically balanced; and (3) receiving a target component according to an ultraviolet spectrum of a detector, concentrating, and crystallizing. The method is suitable for preparing the costuslactone and dehydrocostus lactone in various contents through various high-speed countercurrent chromatographs, and has the characteristics of large separation amount, high recovery rate, and simplicity and convenience of operation.

Description

technical field

[0001] The invention belongs to the field of preparation of lactones contained in cassia, in particular to a preparation method of high-purity cassialides and dehydrocassialides. Background technique

[0002] Muxiang is the dried root of Auckland ia lappaDecne, a plant of the family Asteraceae. It has the effects of promoting qi and relieving pain, invigorating the spleen and eliminating food. It is mainly used clinically for the treatment of ulcers, biliary colic, bronchial asthma and other diseases. . Woody incense mainly contains volatile oil, and its main components are woody hydrocarbon lactone and dehydrowoody lactone, both of which have smooth muscle relaxation and antispasmodic effects, are the main active ingredients of woody, and are also important indicators of woody quality control. Lactone components such as woody lactone and delactone volatile oil can resist the bronchoconstriction effect caused by histamine, acetylcholine and barium chloride, ...

Examples

Embodiment 1

[0032] The methyl acetate-n-propanol-ethanol-water system was selected on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 4:0.8:2:6, shaken and allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 100 mg of crude woody sample and dissolve it in a solution composed of 10 ml upper phase and 10 ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 950rpm, and pump the mobile phase in...

Embodiment 2

[0034] Select ethyl acetate-n-butanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 30°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 3:0.5:1:8, shaken and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg of crude woody sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile phase into the column at a flow rate of 3.0m...

Embodiment 3

[0036]Select butyl acetate-n-propanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 22°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 4:1:1:6, shaken and allowed to stand to separate into layers. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg of crude woody sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 750rpm, and pump the mobile phase into the column at a flow rate of 4.0ml / min; The u...

technical field

[0001] The invention belongs to the field of preparation of lactones contained in cassia, in particular to a preparation method of high-purity cassialides and dehydrocassialides. Background technique

[0002] Muxiang is the dried root of Auckland ia lappaDecne, a plant of the family Asteraceae. It has the effects of promoting qi and relieving pain, invigorating the spleen and eliminating food. It is mainly used clinically for the treatment of ulcers, biliary colic, bronchial asthma and other diseases. . Woody incense mainly contains volatile oil, and its main components are woody hydrocarbon lactone and dehydrowoody lactone, both of which have smooth muscle relaxation and antispasmodic effects, are the main active ingredients of woody, and are also important indicators of woody quality control. Lactone components such as woody lactone and delactone volatile oil can resist the bronchoconstriction effect caused by histamine, acetylcholine and barium chloride, ...

Examples

Embodiment 1

[0032] The methyl acetate-n-propanol-ethanol-water system was selected on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 4:0.8:2:6, shaken and allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 100 mg of crude woody sample and dissolve it in a solution composed of 10 ml upper phase and 10 ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 950rpm, and pump the mobile phase in...

Embodiment 2

[0034] Select ethyl acetate-n-butanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 30°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 3:0.5:1:8, shaken and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg of crude woody sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile phase into the column at a flow rate of 3.0m...

Embodiment 3

[0036]Select butyl acetate-n-propanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify corylides. The suitable temperature for the experiment is 22°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 4:1:1:6, shaken and allowed to stand to separate into layers. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg of crude woody sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 750rpm, and pump the mobile phase into the column at a flow rate of 4.0ml / min; The u...

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