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Preparation method for oleanolic acid type saponin

A technology for oleanolic acid and saponin, which is applied in the fields of medicine and chemical industry, can solve the problems that the purity of the refined product needs to be further improved, the purification efficiency of the reversed-phase preparation process is affected, and the multiple isocratic elution process steps are complicated, so as to achieve automation and The effect of operability, ease of recovery and recycling, and simplified purification process burden

Inactive Publication Date: 2013-01-30
SUZHOU YI HUA BIOMEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method basically realizes the high-efficiency preparation of the target components, but in the scale-up process, there are still some shortcomings: (1) in the macroporous resin refining process, the extract purity is generally greater than 50%, but still contains a large amount of impurities, Affect the purification efficiency of the subsequent reversed-phase preparation process, and the purity of the refined product needs to be further improved; (2) In the reversed-phase column chromatography purification process, the multiple isocratic elution process steps are relatively complicated, and the equipment is low in automation and lacks monitoring methods. Poor process operability

Method used

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  • Preparation method for oleanolic acid type saponin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation of embodiment 1 Pulsatilla saponins PB4 and PB5

[0016] (1) Referring to the analysis results of Pulsatillae medicinal materials (see Shu Zhan, Research on the Chemical Composition of Chinese Medicine Pulsatilla 2, Master Thesis of Soochow University, 2012), select Pulsatilla saponin PB4 [chemical name: 3-O-α-L-rhamnopyranose] -(1→2)-α-L-arabinopyranose lupinin 28-O-α-L-rhamnopyranose-(1→4)-β-D-glucopyranose-(1→ 6)-β-D-glucopyranoside] and PB5 Pulsatilla rhizome medicinal material (place of origin: Anhui, batch PC20091101) as raw materials. Weigh 1 kg of Pulsatilla pulsatillae pieces, extract twice with 8L of 70% ethanol under reflux, each time for 2 hours, filter, combine the filtrate, concentrate under reduced pressure until no alcohol smell, add appropriate amount of water to adjust the liquid medicine so that each 1ml liquid medicine is equivalent to 1.0g crude drug, spare.

[0017] (2) Research on refining process of macroporous resin

[0018] R...

Embodiment 2

[0023]The preparation of embodiment 2 Pulsatilla saponins PB3 and PB7

[0024] PB3 chemical name: 3-O-α-L-rhamnopyranose-(1→2)[β-D-glucopyranose-(1→4)]-α-L-arabinopyranose hedera saponin ; PB3 and PB7 are the main anti-tumor active ingredients in plants such as Pulsatilla.

[0025] (1) Pulsatillae rhizomes rich in Pulsatilla saponins PB39 and PB7 precursor saponins (place of origin: Liaoning, batch PC20111001) were selected as raw materials. Weigh 30kg of Pulsatilla pulsatillae medicinal material, crush it into coarse grains, reflux extract with 420L 75% ethanol twice, each time for 2h, filter the extract, combine, concentrate under reduced pressure until there is no alcohol smell, add water to 100L, adjust and maintain pH9 with NaOH -11, boiled and hydrolyzed for 6 hours, adjusted to pH 7-9 with 1M HCl, diluted with water to 150L, ​​and set aside.

[0026] (2) Macroporous resin refining process

[0027] Select D101 resin column (230cm×300mm i.d., column volume 150L / BV), af...

Embodiment 3

[0030] The preparation of embodiment 3 Patrinia saponin BJ26

[0031] BJ26 chemical name: 3-O-β-D-glucopyranose (1→4)-β-D-xylopyranose (1→3)-α-L-rhamnopyranose (1→2)- β-D-xylopyranose oleanolic acid) 28-O-β-D-glucopyranose (1→6)-β-D-glucopyranose, which is the main component of plants such as chrysanthemum patens and chervil (See Gao Liang, Research on the Chemical Constituents of Patrinia officinalis, Soochow University Master's Degree Thesis, 2011.).

[0032] (1) Extraction: 2.5kg of dried whole herb of Patonia chinensis (Origin: Yunnan, batch 120801), extracted twice by reflux with 10 times the amount of methanol, 1.5 hours each time, combined the extracts, filtered, concentrated and recovered under reduced pressure Methanol, add appropriate amount of water to dilute to 12.5L, set aside.

[0033] (2) Refining: select AB-8 resin column (100cm×10cm i.d., column volume 2.0L / BV), after pretreatment, take the extract from (1) and put it on the column, then use 6BV of water, 3B...

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Abstract

The invention discloses a preparation method for oleanolic acid type saponin. The preparation method comprises the following steps of: (1) selecting plant raw materials containing the oleanolic acid type saponin, adopting water or an ethanol-water mixed solvent to extract, and concentrating and filtering extracting solution, or filtering after hydrolysis treatment; (2) adopting macroporous resin to conduct one-time or repeated adsorption on obtained plant extracting solution, using an ethanol-water mixed solvent to conduct gradient elute, collecting elution portions of corresponding target products, concentrating and drying; and (3) enabling refined extractive to adopt forcing column chromatography, using carbon octadeca-modified silica gel to serve as padding, using carbinol-water in a suitable proportion to serve as a moving phase to conduct elution, respectively collecting flowing contents of the corresponding target products, and concentrating and dying to obtain corresponding products with purity higher than 90%. The preparation method is economic and reasonable in process route, high in efficiency, low in energy consumption, capable of achieving high-efficiency preparation of the target products and easily achieving industrial production. The solvent can be conveniently recycled and reused.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a preparation method of oleanolic acid type saponin in natural plants. technical background [0002] Oleanolic acid-type saponin is a pentacyclic triterpene-type saponin with oleanolic acid as the aglycon and 1-2 glycoside chain substituents at the 3-position and 28-position. This type of ingredients are commonly found in many natural plants, and are the main active ingredients and quality control index ingredients in traditional medicinal materials such as licorice, polygala, and pulsatilla. In recent years, a large number of oleanolic acid saponins have been found in plants of various families and genera such as ivy, pulsatilla, anemone, parrhizae, chervil, etc. This pharmacological activity has attracted people's attention. The preparation method of this type of monomeric saponin has become the working basis for its pharmacological activity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07J75/00C07H15/256C07H1/08A61P35/00
Inventor 杨世林刘江云许琼明王黎明苏胜舒展冯育林李笑然
Owner SUZHOU YI HUA BIOMEDICAL TECH CO LTD
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