Method for extracting oleanolic acid from talinum crassifolium

Abstract

The invention relates to a method for extracting oleanolic acid from talinum crassifolium.After fatting, alcohol extraction and decompressing concentration are conducted on petroleum ether, ethyl acetate is extracted, and then a column chromatography method and a crystallization method are adopted to obtain an oleanolic acid product high in purity.By means of the method, the oleanolic acid in roots and stems of the talinum crassifolium can be fully utilized, the production cost of the oleanolic acid is effectively lowered, and main active ingredients in the roots and stems of the talinum crassifolium are fully utilized.Column chromatography and crystallization are combined, excessive consumption of chemical reagent is reduced, the pure natural property of a product is guaranteed, and the oleanolic acid can be safely provided for industries such as food, cosmetics and pharmacy.

Description

technical field

[0001] The invention belongs to the technical field of natural product extraction, and relates to a method for extracting oleanolic acid from roots and stems of ginseng. Background technique

[0002] Soil ginseng, also known as: cotinus orchid, soil ginseng, blessing ginseng, Shenshihua, cooking flower, false ginseng, ginseng grass, soil Korean ginseng, water ginseng, purple ginseng, etc. It belongs to the central seed order and is an annual of the family Portulaca oleracea or perennial herb. Plants glabrous, 30-100 cm tall. The main root is thick and conical, with a few branches, the bark is dark brown, and the section is milky white. Stem erect, fleshy, base nearly woody, ± branched, terete, sometimes grooved. Leaves alternate or nearly opposite, short-stalked or nearly sessile, leaves slightly fleshy, obovate or obovate-oblong-elliptic, 5-10 cm long, 2.5-5 cm wide, apex acute, sometimes slightly concave, short Pointed, base narrowly cuneate, margin ent...

Examples

Embodiment 1

[0029]After crushing, 100 kg of rhizomes of native ginseng and 300 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain the residue of native ginseng. Add 400L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 2 hours, filter and remove the residue to obtain 350L of filtrate I, take the filtrate I and concentrate it under vacuum or reduced pressure at 60°C to obtain 20L of concentrate I. The concentrated solution I was extracted with 40 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 85% aqueous ethanol solution three to five times the volume of the column to obtain 140L of the eluent I. Concentrate the eluate I at 60°C in vacuum or under reduced pressure to 15 L, let it stand at room temperature for 40 minutes, and filter to obtain 1.84 kg of crude oleanolic acid as the filter residue. Add 3L acetone to the...

Embodiment 2

[0031] After crushing, 200 kg of rhizomes of native ginseng and 500 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain the residue of native ginseng. Add 700L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 1-4h, filter and remove the residue to obtain 660L filtrate I, take the filtrate I and concentrate under vacuum or reduced pressure at 55°C to obtain 35L concentrate I. The concentrated solution I was extracted with 50 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 80% aqueous ethanol solution three to five times the volume of the column to obtain 180 L of eluent I. Concentrate the eluent I at 55°C in vacuum or under reduced pressure to 20 L, let it stand at room temperature for 50 minutes, and filter to obtain 3.98 kg of crude oleanolic acid as the filter residue. Add 6L acetone to the crude product...

Embodiment 3

[0033] After crushing, 400 kg of rhizomes of native ginseng and 1000 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain residues of native ginseng. Add 1000L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 3 hours, filter and remove the residue to obtain 900L of filtrate I, take the filtrate I and concentrate under vacuum or reduced pressure at 60°C to obtain 50L of concentrated liquid I. The concentrated solution I was extracted with 80 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 85% aqueous ethanol solution three to five times the volume of the column to obtain 250 L of eluent I. Concentrate the eluate I at 55°C in vacuum or reduced pressure to 20 L, let it stand at room temperature for 40 minutes, and filter to obtain 8.45 kg of crude oleanolic acid as the filter residue. Add 15L acetone to the cr...

technical field

[0001] The invention belongs to the technical field of natural product extraction, and relates to a method for extracting oleanolic acid from roots and stems of ginseng. Background technique

[0002] Soil ginseng, also known as: cotinus orchid, soil ginseng, blessing ginseng, Shenshihua, cooking flower, false ginseng, ginseng grass, soil Korean ginseng, water ginseng, purple ginseng, etc. It belongs to the central seed order and is an annual of the family Portulaca oleracea or perennial herb. Plants glabrous, 30-100 cm tall. The main root is thick and conical, with a few branches, the bark is dark brown, and the section is milky white. Stem erect, fleshy, base nearly woody, ± branched, terete, sometimes grooved. Leaves alternate or nearly opposite, short-stalked or nearly sessile, leaves slightly fleshy, obovate or obovate-oblong-elliptic, 5-10 cm long, 2.5-5 cm wide, apex acute, sometimes slightly concave, short Pointed, base narrowly cuneate, margin ent...

Examples

Embodiment 1

[0029]After crushing, 100 kg of rhizomes of native ginseng and 300 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain the residue of native ginseng. Add 400L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 2 hours, filter and remove the residue to obtain 350L of filtrate I, take the filtrate I and concentrate it under vacuum or reduced pressure at 60°C to obtain 20L of concentrate I. The concentrated solution I was extracted with 40 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 85% aqueous ethanol solution three to five times the volume of the column to obtain 140L of the eluent I. Concentrate the eluate I at 60°C in vacuum or under reduced pressure to 15 L, let it stand at room temperature for 40 minutes, and filter to obtain 1.84 kg of crude oleanolic acid as the filter residue. Add 3L acetone to the...

Embodiment 2

[0031] After crushing, 200 kg of rhizomes of native ginseng and 500 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain the residue of native ginseng. Add 700L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 1-4h, filter and remove the residue to obtain 660L filtrate I, take the filtrate I and concentrate under vacuum or reduced pressure at 55°C to obtain 35L concentrate I. The concentrated solution I was extracted with 50 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 80% aqueous ethanol solution three to five times the volume of the column to obtain 180 L of eluent I. Concentrate the eluent I at 55°C in vacuum or under reduced pressure to 20 L, let it stand at room temperature for 50 minutes, and filter to obtain 3.98 kg of crude oleanolic acid as the filter residue. Add 6L acetone to the crude product...

Embodiment 3

[0033] After crushing, 400 kg of rhizomes of native ginseng and 1000 kg of petroleum ether are extracted at room temperature, and the petroleum ether extract is filtered to obtain residues of native ginseng. Add 1000L of ethanol to the soil ginseng residue and carry out reflux extraction at 50-70°C for 3 hours, filter and remove the residue to obtain 900L of filtrate I, take the filtrate I and concentrate under vacuum or reduced pressure at 60°C to obtain 50L of concentrated liquid I. The concentrated solution I was extracted with 80 L of ethyl acetate to obtain the extract I. The extract I was adsorbed on a LSA-20 macroporous resin column, and eluted with 85% aqueous ethanol solution three to five times the volume of the column to obtain 250 L of eluent I. Concentrate the eluate I at 55°C in vacuum or reduced pressure to 20 L, let it stand at room temperature for 40 minutes, and filter to obtain 8.45 kg of crude oleanolic acid as the filter residue. Add 15L acetone to the cr...