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Separation and preparation process of high-purity typhaneoside

A technology for the preparation of typhaloside and its preparation technology, which is applied in the field of separation and preparation of high-purity typhaloside, which can solve the problems of long production cycle and high cost, achieve the effects of large preparation volume, good product purity, and overcoming cumbersome operations

Inactive Publication Date: 2011-11-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all use column chromatography repeatedly, and the production cycle is long and the cost is high

Method used

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  • Separation and preparation process of high-purity typhaneoside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 2 kg of Puhuang into the extraction kettle of the supercritical extraction device, and use supercritical CO 2 As a solvent, the supercritical extraction of Puhuang was carried out, the extraction pressure was 28MPa, the temperature was 45°C, the extraction time was 3 hours, CO 2 The flow rate is 25L / h. After the environment in the extraction tank is stable, add 65% acetone carrier (20% of the amount of medicinal material) to the carrier storage tank, adjust the temperature of the analyte to 55°C, and the pressure to be 8MPa. The extract released from the outlet. The extract was extracted with n-butanol, and concentrated under reduced pressure to obtain 244 g of extract. Take 50g of extract and add silica gel (extract: silica gel = 1:3), stir evenly, dry at low temperature, then use new silica gel to pack, mix sample silica gel to put on column, chloroform-ethanol mixed solution is 9:1, 7: 1, 4:1, 2:1, 1:1, 1:2 for gradient elution, the amount of each gradient elue...

Embodiment 2

[0021] 5kg of Puhuang is packed in the extraction still of supercritical extraction device, with supercritical CO 2 As a solvent, carry out the supercritical extraction of Puhuang, the extraction pressure is 33MPa, the temperature is 32°C, the extraction time is 1.5 hours, CO 2 The flow rate is 28L / h. After the environment in the extraction tank is stable, add 70% acetone carrier (22% of the amount of medicinal material) to the carrier storage tank, adjust the temperature of the analyte to 40°C, and the pressure to be 4MPa. The extract released from the outlet. The extract was extracted with n-butanol and concentrated under reduced pressure to obtain 595 g of extract. Take 50g of extract and add silica gel (extract: silica gel = 1:4), stir evenly, dry at low temperature, then pack with new silica gel, mix the sample silica gel onto the column, and mix the chloroform-ethanol solution in a volume ratio of 9:1, 7: 1, 4:1, 2:1, 1:1, 1:2 for gradient elution, the amount of each g...

Embodiment 3

[0024] Put 8 kg of Puhuang into the extraction kettle of the supercritical extraction device, and use supercritical CO 2 As a solvent, the supercritical extraction of Puhuang was carried out, the extraction pressure was 38 MPa, the temperature was 43 ° C, the extraction time was 2 hours, CO 2 The flow rate is 30L / h. After the environment in the extraction tank is stable, add 90% acetone carrier (23% of the amount of medicinal material) to the carrier storage tank, adjust the temperature of the analyte to 47°C, and the pressure to be 10MPa. The extract released from the outlet. The extract was extracted with n-butanol, and concentrated under reduced pressure to obtain 1 kg of extract. Take 50g of extract and add silica gel (extract: silica gel = 1:2), stir evenly, dry at low temperature, then use new silica gel to pack, mix sample silica gel to put on column, chloroform-ethanol mixed solution is 9:1, 7: 1, 4:1, 2:1, 1:1, 1:2 gradient elution, the amount of each gradient eluen...

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Abstract

The invention discloses a separation and preparation process of high-purity typhaneoside. The separation and preparation process comprises: carrying out supercritical CO2 extraction to obtain flavones, carrying out solvent extraction and silica gel column chromatography separation and enrichment to obtain crude typhaneoside, and separating and purifying the crude typhaneoside with a preparative reversed-phase high-performance liquid chromatograph to obtain a typhaneoside crystal. Through the separation and preparation method disclosed in the invention, not only can flavones be continuously extracted from Pollen typhae, but also high-purity typhaneoside monomers can be prepared.

Description

Technical field: [0001] The invention belongs to the technical field of extraction of effective components of traditional Chinese medicines, and relates to a separation and preparation process of high-purity cattail glycosides. Background technique: [0002] Cattail plants grow in ponds, watersides or shallow swamps. There are 18 species in the world, and about 10 species in my country. The resources are extremely rich. Cattail cattail, also known as cattail pollen, Typha angustifolia L., Typha orientalis Presl., or the dried pollen of plants belonging to the family Typhaceae (Typhaceae), has the functions of hemostasis, blood stasis and drenching. Function, used for hematemesis, uterine bleeding, traumatic bleeding, amenorrhea dysmenorrhea, bloody stranguria and astringent pain. Puhuang mainly contains steroids, flavonoids, long-chain aliphatic hydrocarbons, acidic components, amino acids, inorganic components, etc. Among them, flavonoids have the functions of improving m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
CPCY02P20/54
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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