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Preparation process of alkaloid tabersonine

A preparation process and the technology of taponin, which are applied in the field of preparation process of alkaloid taponin, can solve the problems of high cost, unfavorable large-scale production, difficulty in purification and purification and separation of resin column, etc. Effect

Inactive Publication Date: 2011-11-23
ZHANGJIAKOU GERUI HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a kind of preparation technology of alkaloid tabonin, to solve the large consumption of extraction solvent and the large amount of waste water treatment in the prior art; the difficulty of purification and resin column purification and separation and the high cost, which are not conducive to industrialization production problem

Method used

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  • Preparation process of alkaloid tabersonine
  • Preparation process of alkaloid tabersonine
  • Preparation process of alkaloid tabersonine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] One, the pretreatment of potato seed: the mature potato seed 50Kg, without drying, directly cold press with oil press, collect oil phase weight 10Kg, press cake 38Kg, pulverize into 80 orders with pulverizer, wait use.

[0025] 2. Solvent extraction: 190Kg of xylene (content ≥ 98%, boiling point 138.35°C-144.42°C) was added to 38Kg of crushed cake residue, stirred for 3 hours at 35°C, cooled to 20°C, pumped Filter to dryness, and evaporate the solvent to dryness under reduced pressure to obtain 3Kg of oil, which is set aside.

[0026] 3. Extraction and washing with acid water: add 6.5Kg of oil to 65Kg of xylene and stir for 30 minutes; the first extraction and washing: add 50Kg of sulfuric acid aqueous solution with a mass percentage concentration of 2.5%, stir for 1 hour, stand still for 2 hours, layer and separate The organic phase and the acidic aqueous phase are produced, and the acidic aqueous phase is I.

[0027] The second extraction and washing: add 50Kg of su...

Embodiment 2

[0032] One, the pretreatment of potato seed: the mature potato seed 100Kg, without drying, directly cold press with oil press, collect oil phase weight 25Kg, press cake 70Kg, pulverize into 100 orders with pulverizer, wait use.

[0033] 2. Solvent extraction: Add 140Kg of xylene (content ≥ 98%, boiling point 138.35°C-144.42°C) into 70Kg of crushed cake residue, stir for 3 hours at 55°C, cool down to 20°C, and suction filter to dryness , The solvent was evaporated to dryness under reduced pressure to obtain 5Kg of oil.

[0034] 3. Sour water extraction and washing: Add 15Kg of oil to 75Kg of xylene, and stir for 30 minutes;

[0035] The first extraction and washing: Add 50Kg of 3.5% sulfuric acid aqueous solution, stir for 1 hour, stand still for 2 hours, separate layers, and the acidic aqueous phase is I.

[0036] The second extraction and washing: Add 50Kg of 3.5% sulfuric acid aqueous solution to the organic phase, stir for 1 hour, stand still for 2 hours, separate layers,...

Embodiment 3

[0042] One, the pretreatment of potato seed: the ripe potato seed 100Kg, need not dry, directly cold press with oil press, collect oil phase weight 25Kg, press cake 70Kg, pulverize into 90 orders with pulverizer, wait use.

[0043] 2. Solvent extraction: Add 175Kg of xylene (content ≥ 98%, boiling point 138.35°C-144.42°C) into 70Kg of crushed cake residue, stir for 3 hours at 45°C, cool down to 20°C, and suction filter to dryness , The solvent was evaporated to dryness under reduced pressure to obtain 5Kg of oil.

[0044] 3. Extraction and washing with acid water: Add 15Kg of oil to 105Kg of xylene, and stir for 30 minutes;

[0045] The first extraction and washing: Add 50Kg of 3.0% sulfuric acid aqueous solution, stir for 1 hour, stand still for 2 hours, separate layers, and the acidic aqueous phase is I.

[0046] The second extraction and washing: Add 50Kg of 3.0% sulfuric acid aqueous solution to the organic phase, stir for 1 hour, stand still for 2 hours, separate layers...

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Abstract

The invention relates to a preparation process of alkaloid tabersonine, relating to the technical field of biopharmaceuticals. The traditional biological preparation process of the tabersonine has the problems of large solvent loss amount, high cost, large water consumption, high adsorbent resin price, and the like. The preparation process of the alkaloid tabersonine, disclosed by the invention, comprises the following steps of: squeezing voacanga seeds; carrying out solvent extraction; carrying out acid water extraction and washing; and carrying out acid water purification, alkalinization and extraction. According to the preparation process disclosed by the invention, solvent dimethylbenzene which has high boiling point, low cost and easiness in obtaining is adopted as an extractant, anda mode of the acid water extraction and washing is adopted, and therefore, the using amount and the treatment capacity of acid water are reduced; extracted diluted acid water is treated by adopting the dimethylbenzene, and therefore the adsorption washing or repeated salt transformation purification process of the conventional macroporous resin is saved; the content of the tabersonine reaches more than 98 percent, and the extraction ratio is between 1.8 percent and 2.0 percent; in addition, according to the invention, production cost is reduced, and water consumption and solvent consumption are reduced.

Description

technical field [0001] The invention relates to the technical field of biopharmaceuticals, in particular to a preparation process of the alkaloid tabonin. Background technique [0002] Tabonin, English name Tabersonine, CAS NO 4429-63-4, its chemical name is Aspidospermidine-3-carboxylic acid, 2,3,6,7-tetradehydro-(5α,12β,19γ)-methyl seter, and its molecular formula is C 21 h 24 N 2 o 2， The molecular weight is 336.42. Usually oily liquid, white powder solid with higher purity, its hydrochloride is C 21 h 24 N 2 o 2 HCl, melting point is 196°C, [α] D 25 -318 。 (C=0.58, ethanol), IR: λcm -1 : 3365, 1690, 1630, 1615; UVλmax (Loge): 228 (4.03), 298 (4.02), 331 (4.16). [0003] Boning is a good medicinal material, which has antihypertensive, antitumor, hypoglycemic and diuretic effects, and is used for depression, anxiety and emotional instability caused by stroke sequelae, ischemic hypertensive encephalopathy and cerebrovascular disease. It is suitable for elimina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/20
Inventor 王毅卢鹏孙文
Owner ZHANGJIAKOU GERUI HIGH TECH
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