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Method for purifying kerriin A from Pittosporum kerrii craib velamen by column chromatography-high speed countercurrent chromatography

A technology of high-speed countercurrent chromatography and column chromatography, which is applied in the field of purifying sheep brittle lignin A, and can solve the problems of less research on the preparation methods of sheep brittle lignin A

Inactive Publication Date: 2020-01-14
南京乐扬医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few studies on the preparation methods of sheep brittle lignin A

Method used

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  • Method for purifying kerriin A from Pittosporum kerrii craib velamen by column chromatography-high speed countercurrent chromatography
  • Method for purifying kerriin A from Pittosporum kerrii craib velamen by column chromatography-high speed countercurrent chromatography
  • Method for purifying kerriin A from Pittosporum kerrii craib velamen by column chromatography-high speed countercurrent chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Preparation of sheep brittle lignin A

[0029] 1. Experimental materials

[0030] The dry sheep crispy root bark was purchased from the Chinese herbal medicine market, crushed through a 40-mesh sieve, and stored in a cool place for later use.

[0031] Ethanol is industrial anhydrous ethanol, and water is added as needed to make ethanol aqueous solution with different volume percentage concentration.

[0032] Dichloromethane and ethyl acetate were chemically pure products from Nanjing Chemical Reagent Co., Ltd.

[0033] Sheep brittle lignin A reference substance was donated by Yunnan University for Nationalities, with a purity of ≥98%.

[0034] The C18 chromatographic column is a product of Agilent Company, the model is Agilent TC-C18, and the specification is 250mm×4.6mm, 5μm.

[0035] Chromatographically pure acetonitrile and trifluoroacetic acid are products of TEDIA.

[0036] Water is used for chromatography, which is self-made by a water maker.

[00...

Embodiment 2

[0047] Example 2: Preparation of sheep brittle lignin A

[0048] 1. Experimental materials

[0049] The dry sheep crispy root bark was purchased from the Chinese herbal medicine market, crushed through a 40-mesh sieve, and stored in a cool place for later use.

[0050] Ethanol is industrial anhydrous ethanol, and water is added as needed to make ethanol aqueous solution with different volume percentage concentration.

[0051] Dichloromethane and ethyl acetate were chemically pure products from Nanjing Chemical Reagent Co., Ltd.

[0052] Sheep brittle lignin A reference substance was donated by Yunnan University for Nationalities, with a purity of ≥98%.

[0053] The C18 chromatographic column is a product of Agilent Company, the model is Agilent TC-C18, and the specification is 250mm×4.6mm, 5μm.

[0054] Chromatographically pure acetonitrile and trifluoroacetic acid are products of TEDIA.

[0055] Water is used for chromatography, which is self-made by a water maker.

[0056...

Embodiment 3

[0065] Example 3: Preparation of sheep brittle lignin A

[0066] 1. Experimental materials

[0067] The dry sheep crispy root bark was purchased from the Chinese herbal medicine market, crushed through a 40-mesh sieve, and stored in a cool place for later use.

[0068] Ethanol is industrial anhydrous ethanol, and water is added as needed to make ethanol aqueous solution with different volume percentage concentration.

[0069] Dichloromethane and ethyl acetate were chemically pure products from Nanjing Chemical Reagent Co., Ltd.

[0070] Sheep brittle lignin A reference substance was donated by Yunnan University for Nationalities, with a purity of ≥98%.

[0071] The C18 chromatographic column is a product of Agilent Company, the model is Agilent TC-C18, and the specification is 250mm×4.6mm, 5μm.

[0072] Chromatographically pure acetonitrile and trifluoroacetic acid are products of TEDIA.

[0073] Water is used for chromatography, which is self-made by a water maker.

[00...

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Abstract

The invention discloses a method for purifying kerriin A from Pittosporum kerrii craib velamen by column chromatography-high speed countercurrent chromatography. The method comprises the following steps: step A, taking a proper amount of Pittosporum kerrii craib velamen powder, carrying out heat reflux extraction with an ethanol aqueous solution, filtering and concentrating an extracted solution until no alcohol smell exists, carrying out isopyknic extraction with ethyl acetate, and concentrating an obtained ethyl acetate fraction under reduced pressure to obtain an ethyl acetate extract; stepB, dissolving the ethyl acetate extract in a proper amount of an ethanol aqueous solution; filtering with absorbent cotton, loading a sample to a D101 macroporous adsorption resin column, eluting with 10 column volume times of an ethanol aqueous solution with the volume percentage concentration of 30% to remove impurities, eluting with an ethanol aqueous solution with the volume percentage concentration of 65%, collecting a sixth column volume eluent, recovering ethanol under reduced pressure, and carrying out freeze drying to obtain a kerriin A enriched product; and step C, purifying the kerriin A by high speed countercurrent chromatography. The method provided by the invention does not depend on silica gel column chromatography or gel column chromatography, and is easy to operate and industrially apply.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a preparation method of natural compounds, in particular to a column chromatography-high-speed countercurrent chromatography method for purifying sheep crisp lignin A from the root bark of sheep crisp. Background technique [0002] Pittosporum kerrii Craib is a plant of the genus Pittosporum Bank. Its root, stem and bark have been used as folk herbal medicine for thousands of years. It has been reported that a variety of chemical components have been isolated from the extracts of the roots, stems, and bark of the sheep brittle tree. According to the structure type, there are mainly compounds such as triterpenes and their glycosides, sesquiterpenes, carotenoids, and sterols. These chemical components have a variety of biological activities, such as pharmacological activities such as anti-tumor, anti-inflammatory and analgesic, anti-viral and anti-microbial. [0003] Sheep brittlenin A is a...

Claims

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Application Information

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IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 周天北
Owner 南京乐扬医药科技有限公司
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