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Orlistat purification process

A technology of orlistat and process, applied in the field of chemistry, can solve problems such as the inability to solve the purification requirements of key impurities of orlistat, the environmental pollution of organic solvents and solid waste, and the inability to guarantee product quality and production capacity requirements, etc., to achieve reduction Purchase price, good recovery, low column pressure effect

Active Publication Date: 2017-03-29
ARGUS PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, silica gel column chromatography has the fatal shortcomings of poor process stability and low separation efficiency. Not only can it not guarantee product quality and production capacity requirements, it also faces environmental pollution problems such as a large amount of organic solvents and solid waste, which is not in line with current industrial production and energy saving. The development trend of environmental protection
For the macroporous resin purification process, people have studied different resin types, static or dynamic adsorption capacity, elution conditions, collection window, resin regeneration process, etc., but they have not been able to solve the key impurities of orlistat (relative retention time 0.95 ) purification requirements, and also face the problem of processing a large amount of acid-base waste liquid generated by resin regeneration

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0037] Follow the steps below to purify orlistat

[0038] 1) Take 100 g of crude orlistat (content 89%), dissolve it in 70% methanol to a solution of 100 mg / mL, filter, and filter with a filter mesh of 100 mesh;

[0039] 2) Use DAC300 to prepare the column, match with 30μm C18 filler (C18 has a pore size of 80A, and a carbon load of 20%), and the total amount of the column is 6kg;

[0040] 3) Centrifuge at a centrifugal rate of 10000r / min, and take the supernatant;

[0041]4) Inject the supernatant into the chromatographic system, and use an eluent to elute, wherein the eluent is a mixed solvent of ethanol and water 85:15, the equilibrium pressure is 2Mpa, the wavelength is 210nm, and the injection volume is 0.8%; For isocratic elution, the flow rate of the eluent is 1550mL / min, and the elution time is 50min;

[0042] 5) Collect the eluate from the target section, concentrate it in vacuum at 50°C, the vacuum degree is -0.04Mpa, and then dry it in vacuum at 60°C until the moi...

Embodiment 2

[0044] Follow the steps below to purify orlistat

[0045] 1) Take 500 g of crude orlistat (content 90%), dissolve it in 90% methanol to a solution of 10 mg / mL, filter, and filter with a filter mesh of 100 mesh;

[0046] 2) Use DAC300 to prepare the column, match with 30μm C18 filler (C18 has a pore size of 120A, and a carbon load of 12%), and the total amount of the column is 6kg;

[0047] 3) Centrifuge at a centrifugal rate of 15000r / min, and take the supernatant;

[0048] 4) inject the supernatant into the chromatographic system, and use the eluent to elute, wherein the eluent is a mixed solvent of isopropanol and water 80:20, the equilibrium pressure is 5Mpa, the wavelength is 210nm, and the injection volume is 1.5%; The removal is isocratic elution, the flow rate of the eluent is 600mL / min, and the elution time is 60min;

[0049] 5) Collect the eluate from the target section, concentrate it in vacuum at 50°C, the vacuum degree is -0.04Mpa, and then dry it in vacuum at 70...

Embodiment 3

[0051] Follow the steps below to purify orlistat

[0052] 1) Take 300 g of crude orlistat (content 91%), dissolve it in 70% methanol to a solution of 100 mg / mL, filter, and filter with a mesh number of 100;

[0053] 2) Use DAC300 to prepare the column, match with 25μm C18 filler (the pore size of C18 is 200A, and the carbon load is 8%), and the total volume of the column is 6kg;

[0054] 3) Centrifuge at a centrifugal rate of 15000r / min, and take the supernatant;

[0055] 4) Inject the supernatant into the chromatographic system, and use an eluent to elute, wherein the eluent is a mixed solvent of methanol and water 88:12, the equilibrium pressure is 2Mpa, the wavelength is 210nm, and the injection volume is 1.5%; For isocratic elution, the flow rate of eluent is 600mL / min, and the elution time is 60min;

[0056] 5) Collect the eluate from the target section, concentrate it in vacuum at 50°C, the vacuum degree is -0.04Mpa, and then dry it in vacuum at 60°C until the moisture...

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PUM

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Abstract

The invention provides an orlistat purification process. The purification process is characterized by comprising the steps of filtering, centrifuging, carrying out liquid-phase preparation chromatographic separation, concentrating and drying. The liquid-phase chromatographic separation adopts spherical silica gel filling as a separation medium, and an orlistat crude product is subjected to isocratic elution by utilizing an alcohol type water liquid under the balance pressure of 2Mpa-5Mpa, wherein the alcohol type water liquid is a mixed liquid containing fatty alcohol with 1-3 carbon atoms and water in the volume ratio ranging from (80 to 20)-(92 to 8); and the grain diameter of spherical silica gel is 15 microns-30 microns and the pore diameter is 80A-200A.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to an orlistat purification process. Background technique [0002] Orlistat was developed by Roche, a world-renowned pharmaceutical company, in 1998. It is a new type of gastrointestinal lipase inhibitor. It is currently mainly used clinically for the treatment of overweight and obese patients. Its anti-tumor activity has also been confirmed by research. among. It inhibits the activity of gastrointestinal lipase by selectively covalently binding to the serine residue at the active site of gastrointestinal lipase, thereby preventing the hydrolysis of dietary fat (triacylglycerides) into free fatty acids and monoacids that can be absorbed by the human body. Acylglycerides, which ultimately reduce dietary fat absorption by 30%, are hardly absorbed by the body themselves. Based on this unique mechanism of action, its curative effect and safety are also significantly improved compared with pre...

Claims

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Application Information

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IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 曾静崔江铭彭滢
Owner ARGUS PHARMA
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