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Method for separating and preparing tanshinone IIA chemical reference substance

A technology of tanshinone and reference substances, which is applied in the field of preparation of tanshinone IIA chemical reference substances, can solve the problems such as difficulty in stabilizing the purity of tanshinone IIA, difficulty in obtaining large quantities of tanshinone IIA chemical reference substances, lack of online monitoring means, etc., to shorten the separation time and conditions Gentle, easy-to-use effect

Inactive Publication Date: 2008-07-02
DALIAN INST OF CHEM PHYSICS 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 lack of on-line monitoring means, the purity of tanshinone IIA is difficult to reach more than 98% stably
High-speed countercurrent chromatography does not need to use fixed fillers, so there is no irreversible adsorption, and it has the characteristics of no sample loss and no pollution. At present, high-speed countercurrent chromatography is mostly limited to the laboratory scale, and it is difficult to obtain a large amount of tanshinone IIA chemical reference substances with a purity of 98% or more.

Method used

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  • Method for separating and preparing tanshinone IIA chemical reference substance
  • Method for separating and preparing tanshinone IIA chemical reference substance

Examples

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Embodiment 1

[0024] In this embodiment, 50% tanshinone IIA extract is used as raw material, 5 μm C18 bonded phase filler is used as adsorbent, and a solution containing methanol-water (75:25, volume ratio) is used as eluting solvent. The specific process steps are as follows:

[0025] 1. Sample pretreatment

[0026] The tanshinone IIA extract was dissolved in chloroform, configured into a tanshinone IIA solution with a concentration of 60 mg / ml, and filtered through a 0.22 μm microporous membrane.

[0027] 2. Column handling

[0028] The preparative HPLC column was selected as a C18 preparative column (5 μm, 20×250 mm) produced by Sheshido Company in Japan, and the chromatographic column was equilibrated with an elution system solution of about 5 times the column volume.

[0029] 3. Sample loading

[0030] The filtered sample solution was injected through the six-way valve, and the injection volume was 1ml.

[0031] 4. Elution

[0032] The flow rate was controlled at 10ml / min, and the ...

Embodiment 2

[0038] In this example, 70% salvianic acid B extract is used as raw material, 5 μm C18 bonded phase filler is used as adsorbent, and methanol-water (60:40, volume ratio) solution is used as eluting solvent. The specific process Proceed as follows:

[0039] 1. Sample pretreatment

[0040] The tanshinone IIA extract was dissolved in methanol, configured into a tanshinone IIA solution with a concentration of 8 mg / ml, and filtered through a 0.45 μm microporous membrane.

[0041] 2. Column handling

[0042] The preparative HPLC column is a self-packed preparative column. The filler is a C18 bonded phase filler with a particle size of 5 μm. The column is packed in a wet method. Equilibrate the column with an off-system solution.

[0043] 3. Sample loading

[0044] The filtered sample solution was injected through the six-way valve, and the injection volume was 8ml.

[0045] 4. Elution

[0046] The flow rate is controlled at 90ml / min, monitored at 270nm online, and the eluent c...

Embodiment 3

[0050] In this example, 60% tanshinone IIA extract is used as raw material, 10 μm of C18 bonded phase filler is used as adsorbent, and a solution containing methanol-water (75:25, volume ratio) is used as eluting solvent. The specific process steps as follows:

[0051] 1. Sample pretreatment

[0052] The tanshinone IIA extract was dissolved in ethanol, configured into a tanshinone IIA solution with a concentration of 10 mg / ml, and filtered through a 0.45 μm microporous membrane.

[0053] 2. Column handling

[0054] The preparative HPLC column is a self-packed preparative column. The filler is a C18 bonded phase filler with a particle size of 10 μm. The chromatographic column size is 75×250mm. The chromatographic column is equilibrated with an elution system solution about 10 times the column volume.

[0055] 3. Sample loading

[0056] The filtered sample solution was injected through the six-way valve, and the injection volume was 15ml.

[0057] 4. Elution

[0058] The fl...

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Abstract

The invention relates to a preparation method of chemical reference standard of tanshinone IIA, which adopts 50-97 percent of tanshinone IIA by weight as raw material, preparative high performance liquid chromatography as a separation method and a certain ratio of methanol water solution as an elution system to produce the tanshinone IIA chemical reference standard, the purity of which is more than 98 percent. The process steps of the invention comprise: sample pretreatment, chromatographic column treatment, sample injection, elution, on-line monitor, collecting eluriant containing tanshinone IIA and decompression concentration tanshinone IIA to be dried; after the steps, the chemical reference standard of the tanshinone IIA is obtained, which has been monitored by high efficiency liquid chromatography, the content of tanshinone IIA can reach more than 98 percent.

Description

technical field [0001] The invention relates to a preparation method for a chemical reference substance of tanshinone IIA with a purity greater than 98 percent obtained by separating from salvia miltiorrhiza extract. Background technique [0002] Salvia miltiorrhiza is one of the commonly used drugs in traditional pharmacy in my country. Its preparations are widely used clinically. Salvia miltiorrhiza has the effects of promoting blood circulation, regulating menstruation, removing blood stasis, relieving pain, nourishing the heart and calming the nerves. Assay ingredients specified in. Studies have shown that Tanshinone IIA has good therapeutic effects on various cardiovascular and cerebrovascular diseases and skin symptoms, and is widely used in the fields of medicine and cosmetics. [0003] At present, the separation methods of tanshinone IIA are mainly normal phase chromatography, macroporous adsorption resin method, supercritical carbon dioxide extraction method and hig...

Claims

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Application Information

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IPC IPC(8): C07J73/00B01D15/08
Inventor 肖红斌高明哲
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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