Method for preparing magnoflorine from Chinese medicinal Chelidonium majus L.

Abstract

The invention belongs to the field of Chinese medicines, and provides a method for preparing magnoflorine from Chinese medicinal Chelidonium majus L.. The method comprises the following steps of: (1) extracting: extracting Chinese medicinal Chelidonium majus L. with 70 percent ethanol, filtering, concentrating a filtrate, adding ethanol till the ethanol content is 80 percent, filtering, recovering a filtrate till ethanol smell disappears, adding water for diluting, filtering, removing undissolved substances, and adjusting the pH of a filtrate to 1-3 to obtain a standby liquid I; (2) performing primary resin purification: making the standby liquid I flow through a macroporous resin chromatographic column, eluting with water, eluting with 10 percent ethanol, collecting an eluent, filtering, and adjusting the pH of a filtrate to 8-10 to obtain a standby liquid II; (3) performing secondary resin purification: making the standby liquid II flow through a macroporous resin chromatographic column, eluting with water till a color becomes light, eluting with 40 percent ethanol, collecting an eluent, concentrating and drying to obtain a crude product; and (4) refining: dissolving the crude product with water, making the dissolved crude product flow through a C-18 filler chromatographic column, eluting with water, eliminating a fluid, eluting with 5 percent ethanol, collecting an eluent, concentrating and drying to obtain magnoflorine.

Description

Technical field:

[0001] The invention belongs to the field of traditional Chinese medicine, and relates to a method for preparing magnolialine from the traditional Chinese medicine celandine. Background technique:

[0002] Celandine is the whole herb of Celandine majus L. Bitter in the mouth, cool in nature. poisonous. Have heat-clearing and toxic substances removing, pain relieving, the merit of relieving cough. Celandine contains a variety of chemical components, which can be divided into two categories: non-alkaloid and alkaloid. Magnoline, also known as magnoflorine, is one of the main active ingredients, which is an aporphylloid alkaloid with anti-inflammatory, anti-microbial and cytotoxic effects.

[0003] In the existing technology, the extraction methods of celandine mainly include Soxhlet extraction, stirring extraction, ultrasonic extraction, supercritical extraction, microwave radiation technology extraction and alcohol extraction, etc. These methods are mainl...

Examples

Embodiment 1

[0070] (1) Extraction: get celandine, cut off, add 12 times, 10 times, 8 times of 70% ethanol to reflux and extract 3 times, combine the extracts, filter, and the filtrate is concentrated under reduced pressure to 1: 1 (the concentration of the medicinal solution is 1 gram medicinal material / ml, the same below), stir and add ethanol until the ethanol content is 80%, stand still, filter, the filtrate is recovered under reduced pressure until there is no alcohol smell, add water to dilute the medicinal liquid concentration to contain 2 gram medicinal material / ml, let stand , filter, discard the insoluble matter, adjust the pH of the filtrate to 1-3, add water to dilute to 1:1, and obtain the standby solution I;

[0071] (2) Resin purification for the first time: take the spare solution I, pass it through the D-101 macroporous resin chromatographic column, and appropriate amount of water (the amount of water is based on not eluting magnolialine, that is, the Molish reaction of the...

Embodiment 2

[0075] (1) Extraction: get celandine, cut off, add 6 times of 60% ethanol to reflux extraction, filter the extract, concentrate the filtrate under reduced pressure to 1:1 (the concentration of the medicinal solution is 1 gram of medicinal material / ml), stir and add ethanol to The ethanol content is 70%, stand still, filter, and the filtrate is recovered under reduced pressure until there is no alcohol smell, and the concentration of the medicinal solution is diluted with water to contain 2 grams of medicinal materials / ml, stand still, filter, discard insolubles, and adjust the pH of the filtrate to 1 to 3, dilute to 1:1 with water to obtain stock solution Ⅰ;

[0076] (2) Resin purification for the first time: take the spare solution I, pass it through the D-101B macroporous resin chromatographic column, water (the amount of water is subject to the eluting of magnolialine, that is, the Molish reaction of the eluent is negative, or Paper spot reaction or thin-layer chromatograph...

Embodiment 3

[0080] (1) Extraction: get celandine, cut off, 10 times of 70% ethanol reflux extraction 3 times, combine the extracts, filter, and the filtrate is concentrated under reduced pressure to 1:1 (the concentration of the medicinal solution is 1 gram of medicinal material / ml, the same below ), stir and add ethanol until the ethanol content is 80%, leave standstill, filter, and the filtrate is recovered under reduced pressure until there is no alcohol smell, and the concentration of the medicinal solution is diluted with water to contain 2 grams of medicinal materials / ml, leave standstill, filter, discard the insoluble substance, the filtrate was adjusted to pH 1-3, and diluted with water to 1:1 to obtain stock solution Ⅰ;

[0081] (2) The first resin purification: take the spare solution I, pass it through the XDA-1 macroporous resin chromatographic column, and appropriate amount of water (the amount of water is subject to the eluting of magnolialine, that is, the Molish reaction of...

Technical field:

[0001] The invention belongs to the field of traditional Chinese medicine, and relates to a method for preparing magnolialine from the traditional Chinese medicine celandine. Background technique:

[0002] Celandine is the whole herb of Celandine majus L. Bitter in the mouth, cool in nature. poisonous. Have heat-clearing and toxic substances removing, pain relieving, the merit of relieving cough. Celandine contains a variety of chemical components, which can be divided into two categories: non-alkaloid and alkaloid. Magnoline, also known as magnoflorine, is one of the main active ingredients, which is an aporphylloid alkaloid with anti-inflammatory, anti-microbial and cytotoxic effects.

[0003] In the existing technology, the extraction methods of celandine mainly include Soxhlet extraction, stirring extraction, ultrasonic extraction, supercritical extraction, microwave radiation technology extraction and alcohol extraction, etc. These methods are mainl...

Examples

Embodiment 1

[0070] (1) Extraction: get celandine, cut off, add 12 times, 10 times, 8 times of 70% ethanol to reflux and extract 3 times, combine the extracts, filter, and the filtrate is concentrated under reduced pressure to 1: 1 (the concentration of the medicinal solution is 1 gram medicinal material / ml, the same below), stir and add ethanol until the ethanol content is 80%, stand still, filter, the filtrate is recovered under reduced pressure until there is no alcohol smell, add water to dilute the medicinal liquid concentration to contain 2 gram medicinal material / ml, let stand , filter, discard the insoluble matter, adjust the pH of the filtrate to 1-3, add water to dilute to 1:1, and obtain the standby solution I;

[0071] (2) Resin purification for the first time: take the spare solution I, pass it through the D-101 macroporous resin chromatographic column, and appropriate amount of water (the amount of water is based on not eluting magnolialine, that is, the Molish reaction of the...

Embodiment 2

[0075] (1) Extraction: get celandine, cut off, add 6 times of 60% ethanol to reflux extraction, filter the extract, concentrate the filtrate under reduced pressure to 1:1 (the concentration of the medicinal solution is 1 gram of medicinal material / ml), stir and add ethanol to The ethanol content is 70%, stand still, filter, and the filtrate is recovered under reduced pressure until there is no alcohol smell, and the concentration of the medicinal solution is diluted with water to contain 2 grams of medicinal materials / ml, stand still, filter, discard insolubles, and adjust the pH of the filtrate to 1 to 3, dilute to 1:1 with water to obtain stock solution Ⅰ;

[0076] (2) Resin purification for the first time: take the spare solution I, pass it through the D-101B macroporous resin chromatographic column, water (the amount of water is subject to the eluting of magnolialine, that is, the Molish reaction of the eluent is negative, or Paper spot reaction or thin-layer chromatograph...

Embodiment 3

[0080] (1) Extraction: get celandine, cut off, 10 times of 70% ethanol reflux extraction 3 times, combine the extracts, filter, and the filtrate is concentrated under reduced pressure to 1:1 (the concentration of the medicinal solution is 1 gram of medicinal material / ml, the same below ), stir and add ethanol until the ethanol content is 80%, leave standstill, filter, and the filtrate is recovered under reduced pressure until there is no alcohol smell, and the concentration of the medicinal solution is diluted with water to contain 2 grams of medicinal materials / ml, leave standstill, filter, discard the insoluble substance, the filtrate was adjusted to pH 1-3, and diluted with water to 1:1 to obtain stock solution Ⅰ;

[0081] (2) The first resin purification: take the spare solution I, pass it through the XDA-1 macroporous resin chromatographic column, and appropriate amount of water (the amount of water is subject to the eluting of magnolialine, that is, the Molish reaction of...

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