Method for preparing high-purity Orlistat

An orlistat, high-purity technology, applied in the field of medicine, can solve the problems of difficulty in scaling up, high equipment investment, and high production costs, and achieve the effects of cleaner production, less investment, and lower production costs

Active Publication Date: 2012-01-04
鲁南新时代生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to break through the technical problem of purifying orlistat to the high quality standard required by ICH, and at the same time to overcome the shortcomings of high equipment investment, high production cost and difficult scale-up in the preparation of chromatographically purified orlistat, the inventors through repeat

Method used

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  • Method for preparing high-purity Orlistat

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1, a kind of method for preparing high-purity orlistat

[0037] ①Extraction: 3M 3 The liprestatin fermentation broth was filtered through a plate and frame filter press, and the filter cake was blown dry with nitrogen, and the filtered bacteria were transferred to an extraction tank, and ethanol 5 times the weight of the bacteria was added, and stirred and extracted for 8 hours. Collect the filtrate by plate and frame filtration;

[0038] ②Extraction: add water to the filtrate to adjust the ethanol concentration to 40%, add 1 / 5 of heptane according to the volume of the filtrate for extraction, stir, stand and separate, collect the upper phase, concentrate the upper phase under reduced pressure to 1 / 5 of the original volume 7. Remove the insoluble particles by filtration to obtain a concentrated solution of lipostatin with a concentration of 220g / L, which is to be applied to the chromatographic column;

[0039] ③ Chromatography: Prepare a stainless steel med...

Embodiment 2

[0046] Embodiment 2, a kind of method for preparing high-purity orlistat

[0047] ①Extraction: 3M 3 The liprestatin fermentation broth was filtered through a plate and frame filter press, and the filter cake was blown dry with nitrogen, and the filtered bacteria were transferred to an extraction tank, and methanol 10 times the weight of the bacteria was added, and stirred and extracted for 4 hours. Collect the filtrate by plate and frame filtration;

[0048] ②Extraction: add water to the filtrate to adjust the concentration of methanol to 65%, add 1 / 2 of ethyl acetate according to the volume of the filtrate for extraction, stir, let stand to separate layers, collect the upper phase, and concentrate the upper phase under reduced pressure to 1% of the original volume. / 8, filter to remove insoluble particles, get the lipostatin concentrated solution, the concentration is 220g / L, and wait for the upper chromatographic column;

[0049] ③ Chromatography: Prepare a stainless steel...

Embodiment 3

[0056] Embodiment 3, a kind of method for preparing high-purity orlistat

[0057] ①Extraction: 3M 3 The liprestatin fermentation broth was filtered through a plate and frame filter press, and the filter cake was blown dry with nitrogen, and the filtered bacteria were transferred to an extraction tank, and acetone 4 times the weight of the bacteria was added, and stirred and extracted for 12 hours. Collect the filtrate by plate and frame filtration;

[0058] ②Extraction: add water to the filtrate to adjust the concentration of acetone to 30%, add 1 / 6 of petroleum ether according to the volume of the filtrate for extraction, stir, stand and separate layers, collect the upper phase, concentrate the upper phase under reduced pressure to 1 / 3 of the original volume 4. Remove the insoluble particles by filtration to obtain a concentrated solution of lipostatin with a concentration of 210g / L, which is to be applied to the chromatographic column;

[0059] ③ Chromatography: Prepare a ...

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Abstract

The invention belongs to the technical field of medicine, particularly relates to a method for preparing high-purity Orlistat, and more particularly relates to a method for preparing high-purity Orlistat by utilizing mixed silica gel medium-pressure chromatography and crystallization as core technologies. The specific scheme of the method comprises filtration, lixiviation, extraction, chromatography, decoloring, hydrogenation, crystallization and drying processes of fermentation broth. According to the invention, the method provided by the invention is adopted to prepare Orlistat, the total yield of Orlistat is larger than 30%, and the productivity of Orlistat can reach 1.5-3 ton/month; and by detection of HPLC (high performance liquid chromatography), the purity of Orlistat is above 99.5%, the single impurity content in Orlistat is less than 0.1% and is higher than a medicinal standard. In addition, equipment used in the method provided by the invention is common chemical equipment, thus investment is less, and used solvents can be recovered and reused, thereby greatly reducing production cost and environmental pollution and achieving clean production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and particularly relates to a method for preparing high-purity orlistat, and more particularly relates to a method for preparing high-purity orlistat by using mixed silica gel medium-pressure chromatography and crystallization as core technologies. Background technique [0002] Orlistat is a tetrahydrogenated derivative of lipstatin, a secondary metabolite of Streptomyces toxytricini, after catalytic hydrogenation. Orlistat is the first non-central nervous system effect weight loss drug developed by Hoffmann Roche in Basel, Switzerland. It is a long-acting and potent specific gastrointestinal lipase inhibitor, which can effectively reduce Fat digestion and absorption, weight control, used in the treatment of obesity. [0003] [0004] In addition to the semi-synthetic method for the production of orlistat, there is also a chemical total synthesis method. Chinese invention patent application...

Claims

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Application Information

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IPC IPC(8): C07D305/12
Inventor 赵志全董惠钧隋华芹
Owner 鲁南新时代生物技术有限公司
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