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Method for preparing tanshinone IIA chemical reference substance from Salvia prattii

A technology of Kangding sage and tanshinone, which is applied in the field of preparation of tanshinone IIA chemical reference substances, can solve the problems of large loss and complicated process in the crystallization process, and achieve the effects of high recovery rate, simple process and low price

Inactive Publication Date: 2015-12-23
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

[0004] At present, there is no report on the preparation of tanshinone compounds from Kangding Salvia genus. Chinese patent (CN102146114B) reports that tanshinone IIA with a purity of more than 95% can be produced by 4 to 6 steps such as extraction, extraction, silica gel column chromatography, and crystallization. , the process is cumbersome and the crystallization process loses a lot, but there is no literature report on the preparation of large-scale and rapid acquisition of tanshinone IIA from Kangding sage

Method used

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  • Method for preparing tanshinone IIA chemical reference substance from Salvia prattii
  • Method for preparing tanshinone IIA chemical reference substance from Salvia prattii
  • Method for preparing tanshinone IIA chemical reference substance from Salvia prattii

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Experimental program
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Effect test

Embodiment 1

[0028] A method for preparing tanshinone IIA chemical reference substance in Kangding sage, comprising the following steps:

[0029] ⑴ Silica gel column enrichment:

[0030] Separation of 1.0 Kg of the ethanol extract of Sage Kangding in the form of brownish red extract prepared by conventional methods through silica gel column chromatography: eluting with 5 times the column volume of chloroform solvent, collecting the chloroform eluate and drying under reduced pressure To obtain 26.4 g of crude sample rich in tanshinone IIA in red powder form;

[0031] in:

[0032] The conditions of decompression drying refer to a vacuum degree of 0.06MPa and a temperature of 70°C;

[0033] Silica gel column refers to column chromatography silica gel equipped with 100-200 mesh.

[0034] ⑵Microporous resin impurity removal:

[0035] The crude sample rich in tanshinone IIA was dissolved with 100% methanol, filtered to obtain filtrate A, separated on a microporous resin column on the filtrat...

Embodiment 2

[0046] A method for preparing tanshinone IIA chemical reference substance in Kangding sage, comprising the following steps:

[0047] ⑴ Silica gel column enrichment:

[0048] Separation of 0.5 Kg of the ethanol extract of Sage Kangding in the form of brownish red extract prepared by a conventional method through silica gel column chromatography: eluting with 10 times the column volume of chloroform solvent, collecting the chloroform eluate and drying under reduced pressure To obtain 13.5 g of crude sample rich in tanshinone IIA in red powder form;

[0049] in:

[0050] The conditions of decompression drying refer to a vacuum degree of 0.09MPa and a temperature of 50°C;

[0051] Silica gel column refers to column chromatography silica gel equipped with 100-200 mesh.

[0052] ⑵Microporous resin impurity removal:

[0053] The crude sample rich in tanshinone IIA was dissolved with 100% methanol, filtered to obtain filtrate A, separated on a microporous resin column on the filtr...

Embodiment 3

[0064] A method for preparing tanshinone IIA chemical reference substance in Kangding sage, comprising the following steps:

[0065] ⑴ Silica gel column enrichment:

[0066] Separation of 2.0 Kg of the alcohol extract of Sage Kangding in the form of brownish red extract prepared by conventional methods through silica gel column chromatography: eluting with chloroform solvent of 8 times the column volume, collecting the chloroform eluate and drying under reduced pressure To obtain 51.9 g of crude sample rich in tanshinone IIA in red powder form;

[0067] in:

[0068] The conditions of decompression drying refer to a vacuum degree of 0.07MPa and a temperature of 60°C;

[0069] Silica gel column refers to column chromatography silica gel equipped with 100-200 mesh.

[0070] ⑵Microporous resin impurity removal:

[0071] The crude sample rich in tanshinone IIA was dissolved with 95% methanol, and filtrate A was obtained by filtration. The filtrate A was separated on a microporo...

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Abstract

The invention relates to a method for preparing a tanshinone IIA chemical reference substance from Salvia prattii. The method mainly comprises the following steps: (1) silica gel column enrichment: carrying out silica gel column chromatography separation on an alcohol extract which is prepared from brown-red extractum-state Salvia prattii by virtue of a conventional method, carrying out elution by virtue of a chloroform solvent, and collecting a crude sample; (2) micropore resin edulcoration: dissolving the crude sample by virtue of methanol, filtering, separating filtrate by virtue of a micropore resin column, carrying out elution by virtue of a methanol solution, collecting eluate, and drying under reduced pressure to obtain a tanshinone IIA component A; (3) reversed-phase preparative liquid chromatography: dissolving the tanshinone IIA component A by virtue of the methanol solution, filtering by virtue of a 0.45-micron micropore filter membrane, separating the filtrate by virtue of reversed-phase preparative liquid chromatography, detecting by virtue of an ultraviolet detector with the detection wavelength of 254nm, and collecting fractions at a chromatographic peak, so as to obtain the reference substance. The method has the beneficial effects that the process is simple, and the recovery rate is high; the method is applicable to scale production.

Description

technical field [0001] The invention relates to a preparation method of a Tanshinone IIA (TanshinoneIIA) chemical reference substance, in particular to a health [0002] Method for preparing tanshinone IIA chemical reference substance from Sage sage. Background technique [0003] Kangding sage (Salviaprattii) belongs to the genus Salvia (Salvia L.), Labiatae (Labiatae). Modern studies have shown that the chemical constituents in sage plants mainly include phenolic acids and terpenes. Tanshinone IIA is a tanshinone compound with a relatively high content in Sage Kangding. Due to the similar polarity of tanshinone compounds and the subtle structural differences of the compounds, it is difficult to obtain high-purity tanshinone IIA reference substances from Sage Kangding. In order to speed up the production and sales of Kangding Sage and the research and development of related new drugs, it is particularly important to develop an efficient preparation method for high-purity t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
Inventor 党军陶燕铎邵赟梅丽娟王启兰张莉孙策
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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