Method for purifying lipstatin

A purification method, the technology of Lipus, is applied in the field of purification of liprestatin, which can solve the problems of increasing production safety risks, increasing recycling workload, and increasing hidden costs, so as to reduce the number of times of high-temperature ignition regeneration and improve the use of The effect of life and utilization improvement

Inactive Publication Date: 2013-04-10
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of a large amount of organic solvents not only increases the workload of recycling but also increases the risk of production safety, and the process often contains acetonitrile, a highly toxic and volatile organic solvent, which increases the hidden costs in various aspects

Method used

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  • Method for purifying lipstatin
  • Method for purifying lipstatin

Examples

Experimental program
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Effect test

Embodiment approach

[0041] A method for purifying liprestatin, comprising:

[0042] 1) providing a solid mixture containing riprestatin;

[0043] 2) extracting the solid mixture containing riprestatin obtained in step 1) with a low-polarity or non-polar organic solvent as an extractant to obtain an extract containing riprestatin;

[0044] 3) Adsorbing the liprestatin-containing extract obtained in step 2) with molecular sieves, and eluting with the first eluent, thereby obtaining the first eluate containing liprestatin; and

[0045] 4) The first eluate containing riprestatin obtained in step 3) is further purified by chromatography.

[0046] Wherein, the solid mixture containing riprestatin in the above-mentioned step 1) is a solid mixture containing liprestatin obtained from fermentation broth or other means, and the content of riprestatin in the solid mixture is not particularly limited . Preferably, the solid mixture containing liprestatin obtained by drying the fermented liquid of Streptom...

Embodiment 1

[0077] 1000 g of riprestatin fermentation broth was spray-dried and extracted twice with heptane, the extraction temperature was 30°C, and the amount of heptane used for the first extraction and the second extraction was 5 L and 3 L. The liprestatin in the heptane extraction mixture was detected by HPLC, and its purity was measured to be 20.59%. A small amount of the heptane extraction mixture was concentrated under reduced pressure and vacuum at 40° C. to obtain a concentrated paste, which was measured to have a weight content of 8%; the amount of riprestatin product contained in the remaining extraction mixture was 6.5 g.

[0078] The diameter-to-height ratio of the molecular sieve is 1:7. The 13X molecular sieve is used for molecular screening. Weigh 50 g of the 13X molecular sieve, and soak the molecular sieve in heptane for more than 8 hours before use. The heptane extraction mixture passed through the molecular sieve column at 25°C and a flow rate of 4BV / h. After complet...

Embodiment 2

[0080] 1000 g of riprestatin fermentation broth was sprayed to dry residue and extracted twice with petroleum ether, the extraction temperature was 30°C, and the amount of petroleum ether used for the first extraction and the second extraction was 5 L and 3 L. The purity of riprestatin in the petroleum ether extraction mixture detected by HPLC was 22.7%. A small amount of petroleum ether extraction mixture was concentrated under reduced pressure and vacuum at 40° C. to obtain a concentrated paste with a measured weight content of 7.6%; the content of riprestatin in the remaining extraction mixture was 6 g.

[0081] The diameter-to-height ratio of the molecular sieve is 1:8, and the molecular sieve is a 10X molecular sieve. Weigh 63g of the 10X molecular sieve, and soak the molecular sieve in petroleum ether for more than 8 hours before use. The petroleum ether extraction mixture passed through the molecular sieve column at 25°C and a flow rate of 3BV / h. After completion, conti...

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Abstract

The invention provides a method for purifying lipstatin. The method comprises the following steps: 1) providing a solid mixture containing the lipstatin; 2) extracting the solid mixture by utilizing a low-polarity first organic solvent or a non-polarity organic solvent, so as to obtain an extract liquor containing the lipstatin; 3) adsorbing the extract liquor by a molecular sieve; eluting the extract liquor by a first eluent so as to obtain the first extract liquor containing the lipstatin; and 4) purifying the first eluent containing the lipstatin obtained in the step 3) through chromatography. The method provided by the invention has the following beneficial effects: the solvent containing the lipstatin is selectively adsorbed by adopting the organic molecular sieve; the method is low in cost and more stable at high temperature; the use amount of silica gel is reduced, the utilization ratio of the silica gel is improved, and the separation effect is improved, so that the production running cost is greatly reduced.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to a method for purifying liprestatin. Background technique [0002] Lipstatin is a metabolite of Streptomyces toxytricini, which can selectively inhibit the activity of pancreatic lipase in the gastrointestinal tract and reduce the decomposition and absorption of fat. Its structural formula is shown in formula I. Its tetrahydro derivative orlistat (orlistat) has been successfully developed by Roche Inc. (Roche lnc.) as a weight loss drug - Xenical, which is currently the only drug for the treatment of obesity marketed as a non-central nervous system effect. [0003] [0004] Formula I [0005] The production process of liprestatin through microbial biosynthesis mainly includes the following steps: the microbial fermentation liquid is directly crushed by ultrasound, extracted with an organic solvent, and then concentrated to obtain crude crystals, and then purified by chromatography to o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/12
Inventor 何勇崴赵德
Owner NEW FOUNDER HLDG DEV LLC
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