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Preparation method of polyphyllin II and polyphyllin VII

A technology of Chonglou saponin and Yunnan Chonglou, applied in steroids, organic chemistry, etc., can solve the problems of separation and purification of Chonglou steroidal saponin monomer compounds, difficulty in purification, and limitation of new drug research and development potential.

Inactive Publication Date: 2017-11-03
KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difficulty in the separation and purification of the monomeric compounds of papaya steroidal saponins, it is one of the bottlenecks that limit the potential of new drug development.
So far, there is no new drug with a single steroidal saponin as the main component on the market

Method used

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  • Preparation method of polyphyllin II and polyphyllin VII
  • Preparation method of polyphyllin II and polyphyllin VII
  • Preparation method of polyphyllin II and polyphyllin VII

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The extraction method of papaya saponin II and VII of the present invention:

[0028] After the dry peel (0.50 g) of Paprika dianthus is crushed, it is extracted with water, 90% ethanol or absolute ethanol, and ultrasonically extracted. The extraction time is 30-120 minutes, and the extraction temperature is 25°C-60°C. Under different extraction conditions, the detected contents of papaya saponin II and papaya saponin VII are shown in Table 1. After filtering the extract, evaporate to dryness below 60°C to obtain the crude extract (0.14-0.27 g) of the pericarp of Papaya dianthus.

[0029] Table 1. Content comparison of papaya saponin II and papaya saponin VII in different extraction methods

[0030]

[0031] Note: The content of papaya saponin II and papaya saponin VII is calculated according to the dry matter of the extracted raw materials

Embodiment 2

[0033] The enrichment method of papaya saponin II and VII of the present invention:

[0034] Method 1: Take 6.85g of the crude extract of the pericarp of Parisia diangi, add 100mL of water to make a suspension, and extract it with 100mL of ethyl acetate and n-butanol for 5 times respectively. After the extract was concentrated, an ethyl acetate extract (0.41 g) and an n-butanol extract (3.22 g) were obtained, respectively. The fraction extracted with n-butanol was chromatographed on a Sephadex LH-20 gel column and eluted with methanol to obtain fractions (1.50 g) rich in saponins II and VII.

[0035] Method 2: take 500 g of the crude extract of the pericarp of Pachyphyllum yunnanensis, go through D101 macroporous resin chromatography, and elute with water, 80% ethanol, 95% ethanol and acetone, respectively. Among them, 80% ethanol eluted part was concentrated to obtain 150 g of eluate. Take 10 g of 80% ethanol eluent, add 100 mL of water to make a suspension, and sequentiall...

Embodiment 3

[0037] Separation and purification method of papaya saponin II and VII of the present invention:

[0038] Method 1: Take 1.50 g of the part rich in papaya saponin II and VII in method 1 of Example 2, and pass it through preparative HPLC (YMC-Pack, ODS-A chromatographic column, diameter 250×20mm, 5μm; flow rate v=8.0mL / min; eluent: 0~15min, methanol-water, 87:13; 15~30min, methanol-water, 90:10) to prepare the compound papaya saponin VII (156.0mg, t R =12.943min) and papaya saponin II (145.8mg, t R = 24.010 min).

[0039] Method 2: Take 164.6 mg of the part rich in papaya saponin II and VII in method 2 of Example 2, and pass through preparative HPLC (YMC-Pack, ODS-A chromatographic column, diameter 250×20mm, 5μm; flow rate v=8.0mL / min; the eluent is methanol-water, 90:10) to prepare compound saponin VII (24.4mg, t R =11.520min) and papaya saponin II (27.1mg, t R = 21.320 min).

[0040] Method 3: Take 150.3 mg of the part rich in papaya saponin II and VII in method 2 of Exa...

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Abstract

The invention provides a preparation method of polyphyllin II and polyphyllin VII, and in particular provides a method for preparing the polyphyllin II and the polyphyllin VII from peel of paris polyphylla var. yunnanensis. The method comprises the steps of crushing the peel of the paris polyphylla var. Yunnanensis, extracting by a solvent to obtain a crude extract, enriching the polyphyllin II and the polyphyllin VII from the crude extract so as to obtain parts which are rich in the polyphyllin II and the polyphyllin VII, performing further separation and purification to obtain the polyphyllin II and the polyphyllin VII. Through the method provided by the invention, the purpose of preparing the polyphyllin II and the polyphyllin VII in large scale can be realized.

Description

Technical field: [0001] The invention belongs to the technical field of extraction and separation of natural products, and in particular relates to preparation methods of papaya saponin II and papaya saponin VII. Background technique: [0002] Steroidal saponins of Chonglou are the main active ingredients of Chonglou plants, which have pharmacological activities such as anti-cancer, hemostasis, and anti-gastric mucosa damage [Wang Yuehu, Niu Hongmei, Zhang Zhaoyun, Hu Xiangyang, Li Heng. Medicinal value and Its chemical substance basis. Chinese Journal of Traditional Chinese Medicine, 2015, 40(5), 833-839]. However, due to the difficulty in the separation and purification of the monomeric compound of steroidal saponins, it is one of the bottlenecks that limit the potential of its new drug research and development. So far, there is no new drug with a single steroidal saponin as the main component on the market. Therefore, the large-scale preparation of papaya steroidal sapo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 王跃虎李晓艳杨珺夏梦媛罗吉凤杨永平李恒
Owner KUNMING INST OF BOTANY - CHINESE ACAD OF SCI
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