Preparation process for separating and purifying strychnine from total alkali of nux vomica

Abstract

The invention discloses a preparation process for separating and purifying strychnine from total alkali of nux vomica. Pure strychnine with the content exceeding 94% is prepared by taking total alkali of nux vomica as the raw material through a column chromatography and organic solvent extraction purification and separation method. The pure strychnine can be used as a chemical standard substance and a reference substance of nux vomica or an extract of the nux vomica or used as a raw material of a preparation. The preparation process is not only low in cost, simple and easy in process, but also applicable to the preparation of a larger amount of pure strychnine, and has wide social and economic effects.

Description

technical field

[0001] The invention relates to the field of preparation of traditional Chinese medicine components, in particular to a preparation process for separating and purifying strychnine from total strychnine. Background technique

[0002] Strychnos nux-vomica L., a traditional Chinese medicine, is the dry mature seed of Strychnos nux-vomica L., which has the effects of dredging collaterals, relieving pain, dispelling stagnation and reducing swelling. Modern studies have shown that its main active ingredients are alkaloids, with a content of about 1.5% to 5% of crude drugs, mainly strychnine, brucine and nitrogen oxides, among which strychnine Strychnine content tops the list, accounting for 1.2% to 2.2%; strychnine accounts for about 0.8%, which is a weakly alkaline indole alkaloid with a molecular formula of C 23 h 26 N 2 o 4 , relative molecular weight 394, white crystalline powder, extremely bitter taste; slightly soluble in water, soluble in organic solvent...

Examples

Embodiment 1

[0030] (1) Weigh 10 g of total alkaloids of Strychnis chinensis, dissolve with an appropriate amount of chloroform, mix evenly with 8 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0031] (2) Weigh 180 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 15 cm, which is a silica gel column for separation.

[0032] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0033] (4) eluting with 95% ethanol, collecting the eluent in sections, each section of the eluent is 2 times of column volume, and is identified as containing a single strychnine component by thin-layer chromatography of Strychnis in the Chinese Pharmacopoeia, Combine the eluents of each section of the single strychnine component and concentrate ...

Embodiment 2

[0036] (1) Take by weighing 10 g of total alkaloids of Nuxebra chinensis, after dissolving with an appropriate amount of chloroform, mix evenly with 10 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0037] (2) Weigh 400 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 25 cm, which is a silica gel column for separation.

[0038] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0039] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 1% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as conta...

Embodiment 3

[0042] (1) Weigh 10 g of total alkaloids of strychnium, dissolve with an appropriate amount of chloroform, mix evenly with 20 g of silica gel (80-100 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0043](2) Weigh 900g of silica gel (200-300 mesh), plug it into a glass column with a diameter of 5cm at the bottom, fill the column with anhydrous ethanol wet method, tap it, and the column bed height is about 30cm, which is a silica gel column for separation.

[0044] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0045] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 2% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as containing a single strychnine co...

technical field

[0001] The invention relates to the field of preparation of traditional Chinese medicine components, in particular to a preparation process for separating and purifying strychnine from total strychnine. Background technique

[0002] Strychnos nux-vomica L., a traditional Chinese medicine, is the dry mature seed of Strychnos nux-vomica L., which has the effects of dredging collaterals, relieving pain, dispelling stagnation and reducing swelling. Modern studies have shown that its main active ingredients are alkaloids, with a content of about 1.5% to 5% of crude drugs, mainly strychnine, brucine and nitrogen oxides, among which strychnine Strychnine content tops the list, accounting for 1.2% to 2.2%; strychnine accounts for about 0.8%, which is a weakly alkaline indole alkaloid with a molecular formula of C 23 h 26 N 2 o 4 , relative molecular weight 394, white crystalline powder, extremely bitter taste; slightly soluble in water, soluble in organic solvent...

Examples

Embodiment 1

[0030] (1) Weigh 10 g of total alkaloids of Strychnis chinensis, dissolve with an appropriate amount of chloroform, mix evenly with 8 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0031] (2) Weigh 180 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 15 cm, which is a silica gel column for separation.

[0032] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0033] (4) eluting with 95% ethanol, collecting the eluent in sections, each section of the eluent is 2 times of column volume, and is identified as containing a single strychnine component by thin-layer chromatography of Strychnis in the Chinese Pharmacopoeia, Combine the eluents of each section of the single strychnine component and concentrate ...

Embodiment 2

[0036] (1) Take by weighing 10 g of total alkaloids of Nuxebra chinensis, after dissolving with an appropriate amount of chloroform, mix evenly with 10 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0037] (2) Weigh 400 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 25 cm, which is a silica gel column for separation.

[0038] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0039] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 1% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as conta...

Embodiment 3

[0042] (1) Weigh 10 g of total alkaloids of strychnium, dissolve with an appropriate amount of chloroform, mix evenly with 20 g of silica gel (80-100 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0043](2) Weigh 900g of silica gel (200-300 mesh), plug it into a glass column with a diameter of 5cm at the bottom, fill the column with anhydrous ethanol wet method, tap it, and the column bed height is about 30cm, which is a silica gel column for separation.

[0044] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0045] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 2% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as containing a single strychnine co...

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