Method for separating and purifying impurities in sodium tanshinone IIA sulfonate crude drug

Abstract

The invention relates to the technical field of medicines and discloses a method for separating and purifying impurities in a sodium tanshinone IIA sulfonate crude drug. Sodium tanshinone IIA sulfonate is widely used for treating cardiovascular and cerebrovascular diseases and other systemic disease at present. 1, 2-dehydrogenation sodium tanshinone IIA sulfonate, sodium tanshinone IIB sulfonate and 1-hydroxy sodium tanshinone IIA sulfonate are three major impurities in the sodium tanshinone IIA sulfonate crude drug. The method for separating and purifying the impurities in the sodium tanshinone IIA sulfonate crude drug is that a high-speed counter-current chromatography method is used for separating and purifying the three major impurities in the sodium tanshinone IIA sulfonate crude drug. The method has the advantages of being simple, fast, high in recovery rate, large in preparation quantity, high in separation efficiency, good in product purity, convenient and suitable for studying comparison products, and defects of cumbersome operations and long separation periods of traditional preparation methods are overcome.

Description

technical field

[0001] The invention relates to the technical field of medicine, in particular to a method for separating and purifying three main impurities from tanshinone IIA sodium sulfonate crude drug. Background technique

[0002] Sodium Tanshinone II A Sulfonate (Sodium Tanshinone II A Sulfonate, Phenanthro[1,2-b]furan-2-sulfonicacid,6,7,8,9,10,11-hexahydro-1,6,6-trimethyl-10, 11-dioxo-, sodium salt) has the effects of promoting blood circulation, removing blood stasis, inhibiting platelet aggregation, reducing blood viscosity, expanding arterioles, improving systemic microcirculation, scavenging oxygen free radicals, improving tissue hypoxia, and anti-inflammation. It has been widely used at present For the treatment of cardiovascular and cerebrovascular diseases and other systemic diseases. Sodium 1,2-dehydrotanshinone IIA sulfonate, sodium tanshinone IIB sulfonate and sodium 1-hydroxytanshinone IIA sulfonate are the three main impurities in the bulk drug of sodium...

Examples

Embodiment 1

[0022] High-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) was used to separate and purify three main impurities from tanshinone IIA sodium sulfonate raw material drug: the solvent system that constitutes the high-speed countercurrent chromatography stationary phase and mobile phase is chloroform: n-butanol: Methanol: 0.5% saturated ammonium acetate aqueous solution = 17: 0.3: 14: 9 (volume ratio). After fully shaking in the separatory funnel, the layers were statically separated, the upper phase was the stationary phase, and the lower phase was the mobile phase. First make the countercurrent chromatographic column full of stationary phase, then make the host rotate, then pump the mobile phase, the volume of the countercurrent chromatographic column is 300ml, the retention rate of the stationary phase is 75%, the flow rate is 2.0ml / min, the rotating speed is 950rpm, and the detection wavelength is 280nm. Dissolve 100mg of tanshinone IIA sodium su...

Embodiment 2

[0026]According to the high-speed countercurrent chromatography operation steps of Example 1, three main impurities are separated and purified from the tanshinone IIA sodium sulfonate bulk drug: the solvent system that constitutes the high-speed countercurrent chromatography stationary phase and mobile phase is chloroform: n-butanol: methanol ︰0.5% saturated ammonium acetate aqueous solution=18︰0.2︰15︰8. The methods and steps of separation and purification, purity detection and structural identification of the three impurities are the same as in Example 1. The yield of 1,2-dehydrotanshinone IIA sodium sulfonate is 24.8%, and the purity is 95.07%; the yield of tanshinone IIB sodium sulfonate The yield was 17.46%, and the purity was 96.14%; the yield of sodium 1-hydroxytanshinone IIA sulfonate was 29.45%, and the purity was 97.57%.

technical field

[0001] The invention relates to the technical field of medicine, in particular to a method for separating and purifying three main impurities from tanshinone IIA sodium sulfonate crude drug. Background technique

[0002] Sodium Tanshinone II A Sulfonate (Sodium Tanshinone II A Sulfonate, Phenanthro[1,2-b]furan-2-sulfonicacid,6,7,8,9,10,11-hexahydro-1,6,6-trimethyl-10, 11-dioxo-, sodium salt) has the effects of promoting blood circulation, removing blood stasis, inhibiting platelet aggregation, reducing blood viscosity, expanding arterioles, improving systemic microcirculation, scavenging oxygen free radicals, improving tissue hypoxia, and anti-inflammation. It has been widely used at present For the treatment of cardiovascular and cerebrovascular diseases and other systemic diseases. Sodium 1,2-dehydrotanshinone IIA sulfonate, sodium tanshinone IIB sulfonate and sodium 1-hydroxytanshinone IIA sulfonate are the three main impurities in the bulk drug of sodium...

Examples

Embodiment 1

[0022] High-speed countercurrent chromatography (Shenzhen Tongtian Biochemical Co., Ltd.) was used to separate and purify three main impurities from tanshinone IIA sodium sulfonate raw material drug: the solvent system that constitutes the high-speed countercurrent chromatography stationary phase and mobile phase is chloroform: n-butanol: Methanol: 0.5% saturated ammonium acetate aqueous solution = 17: 0.3: 14: 9 (volume ratio). After fully shaking in the separatory funnel, the layers were statically separated, the upper phase was the stationary phase, and the lower phase was the mobile phase. First make the countercurrent chromatographic column full of stationary phase, then make the host rotate, then pump the mobile phase, the volume of the countercurrent chromatographic column is 300ml, the retention rate of the stationary phase is 75%, the flow rate is 2.0ml / min, the rotating speed is 950rpm, and the detection wavelength is 280nm. Dissolve 100mg of tanshinone IIA sodium su...

Embodiment 2

[0026]According to the high-speed countercurrent chromatography operation steps of Example 1, three main impurities are separated and purified from the tanshinone IIA sodium sulfonate bulk drug: the solvent system that constitutes the high-speed countercurrent chromatography stationary phase and mobile phase is chloroform: n-butanol: methanol ︰0.5% saturated ammonium acetate aqueous solution=18︰0.2︰15︰8. The methods and steps of separation and purification, purity detection and structural identification of the three impurities are the same as in Example 1. The yield of 1,2-dehydrotanshinone IIA sodium sulfonate is 24.8%, and the purity is 95.07%; the yield of tanshinone IIB sodium sulfonate The yield was 17.46%, and the purity was 96.14%; the yield of sodium 1-hydroxytanshinone IIA sulfonate was 29.45%, and the purity was 97.57%.

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