A kind of preparation method of salvinolone chemical reference substance in Sage Kangding

A technology of Kangding sage and reference substance, applied in the field of preparation of Salvinolone chemical reference substance, can solve problems such as no reports, and achieve the effects of low price, cheap and easy-to-obtain filler, and high recovery rate

Inactive Publication Date: 2017-08-15
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the large-scale and rapid preparation of the compound Salvinolone from the Sage sage plant

Method used

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  • A kind of preparation method of salvinolone chemical reference substance in Sage Kangding
  • A kind of preparation method of salvinolone chemical reference substance in Sage Kangding
  • A kind of preparation method of salvinolone chemical reference substance in Sage Kangding

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Experimental program
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Effect test

Embodiment 1

[0028] A kind of preparation method of Salvinolone chemical reference substance in Sage Kangding in embodiment 1 comprises the following steps:

[0029] ⑴ Silica gel column enrichment:

[0030] The ethanol extract 2.0Kg in the brownish-red extract-like Sage Kangding prepared by a conventional method is separated through silica gel column chromatography: the mixed solvent of chloroform-methanol-water is used for elution by 5 times the column volume, and Fractions were collected in 500 mL portions, and the fractions with an Rf value of 0.7 to 0.9 were collected by thin-layer chromatography. The fractions were dried under reduced pressure to obtain 19.6 g of red powdery crude samples of components rich in Salvinolone.

[0031] in:

[0032] The conditions of decompression drying refer to a vacuum degree of 0.09MPa and a temperature of 50°C;

[0033] The mixed solvent of chloroform-methanol-water refers to the mixture of chloroform, methanol and water in a volume ratio of 9:1:0.1...

Embodiment 2

[0047] A preparation method of Salvinolone chemical reference substance in Sage Kangding, comprising the following steps:

[0048] ⑴ Silica gel column enrichment:

[0049] The ethanol extract 1.0Kg in the brown-red extract-like Sage Kangding prepared by conventional methods is separated by silica gel column chromatography: the mixed solvent of chloroform-methanol-water is used for elution by 10 times the column volume, and Fractions were collected in 500 mL portions, and the fractions with an Rf value of 0.7 to 0.9 were collected by thin-layer chromatography. The fractions were dried under reduced pressure to obtain 10.2 g of crude red powdery components rich in Salvinolone.

[0050] in:

[0051] The conditions of decompression drying refer to a vacuum degree of 0.06MPa and a temperature of 70°C;

[0052] The mixed solvent of chloroform-methanol-water refers to the mixture of chloroform, methanol and water in a volume ratio of 9:1:0.1.

[0053] The conditions for thin-layer c...

Embodiment 3

[0066] A preparation method of Salvinolone chemical reference substance in Sage Kangding, comprising the following steps:

[0067] ⑴ Silica gel column enrichment:

[0068] The ethanol extract 0.5Kg in the reddish-brown sage extract of Kangding prepared by conventional method is separated by silica gel column chromatography: the mixed solvent of chloroform-methanol-water is used for elution by 8 times of column volume, and Fractions were collected in 500 mL portions, and the fractions with an Rf value of 0.7 to 0.9 were collected by thin-layer chromatography. The fractions were dried under reduced pressure to obtain 4.9 g of crude red powdery components rich in Salvinolone.

[0069] in:

[0070] The conditions of decompression drying refer to a vacuum degree of 0.08MPa and a temperature of 60°C;

[0071] The mixed solvent of chloroform-methanol-water refers to the mixture of chloroform, methanol and water in a volume ratio of 9:1:0.1.

[0072] The conditions for thin-layer c...

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Abstract

The invention relates to a preparation method of a salvinolone chemical reference substance in Salvia prattii, which comprises the following steps: silica gel column enrichment, impurity removal by solid-phase extraction, and refinement by reversed-phase liquid-phase preparative chromatography. The silica gel column enrichment adopted in the first step can perform high-efficiency enrichment on salvinolone in the sample; the impurity removal by solid-phase extraction adopted in the second step can obtain the salvinolone refined component with the purity of about 70%; and the reversed-phase liquid-phase preparative chromatography is adopted in the third step to obtain the salvinolone chemical reference substance. The method can obtain the high-purity salvinolone reference substance, has higher yield (greater than 80%), is very suitable for large-scale production, has low requirements for the raw material (common wild or planted Salvia prattii alcohol extract), and can easily implement mass material preparation. The filler is cheap and accessible. A solid-phase extraction column is adopted for impurity removal; and the solid-phase extraction column is recyclable, is low in average price, and can easily implement large-scale treatment. In the refinement, the reversed-phase liquid-phase preparative chromatography, which is a quick isocratic process, is adopted.

Description

technical field [0001] The invention relates to a preparation method of a Salvinolone chemical reference substance, in particular to a preparation method of a Salvinolone chemical reference substance in Sage Kangding. Background technique [0002] Kangding sage (Salvia prattii) is a plant belonging to the genus Salvia (Salvia L.) and the Labiatae family. Modern studies have shown that the chemical constituents in sage plants mainly include phenolic acids and terpenes. In 1989, Long-Ze Lin et al. isolated Salvinolone from Sage (Phytochemistry, 1989, 28(1): 177-181). Salvinolone is a tanshinone compound with a relatively high content in Kangding sage. Modern pharmacological studies have shown that the compound Salvinolone has various pharmacological activities such as antibacterial, anticancer, lowering blood cholesterol levels and inhibiting HIV protease. In order to speed up the production and sales of Kangding Sage and the pace of research and development of related new d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/79C07C49/747
CPCC07C45/79C07C49/747
Inventor 党军邵赟陶燕铎梅丽娟王启兰张莉赵建强
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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