Modified crystallization purifying and precipitating method of piperacillin acid

A technology of piperacillin acid and piperacillin is applied in the field of improved crystallization, purification and precipitation of piperacillin acid, which can solve the problems of no fluidity, poor filterability, low production performance and the like, and achieves low residue, high content, The effect of improving stability

Active Publication Date: 2011-01-12
JIANGXI FUSHINE PHARMA CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology allows for better production of pure pimicilide hydrates while reducing their amount of unwanted substances such as ammonium salts or other byproducts that may be found during synthesis processes. These improvements result in improved properties like high water activity (Haw), low extractables) and reduced residues compared to previous methods. Additionally, this new method results in more stable forms without losing any beneficial qualifications against certain types of bacteria called beta lactic acid producing microorganisms.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the properties or purifying specific compounds from various sources such as pharmaceutical products like pimelidine hydrochloride tablets that can cause unwanted side effects during treatment due to their high molecular weight and lacking solubility with other ingredients commonly present in these formulations.

Method used

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  • Modified crystallization purifying and precipitating method of piperacillin acid

Examples

Experimental program
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Effect test

Embodiment 1

[0007] Example 1: The ES2321153 seedling transplanting method described in the background art was adopted.

[0008] Add 800ml purified water to a flask and 400g crude piperacillin, HPLC is 98%, add 10% sodium bicarbonate solution dropwise to adjust PH=6-6.5 and stir to dissolve completely, add 400ml ethyl acetate at 20-25℃, Stir for 15-20min, separate layers, add 1600ml ethyl acetate to the water phase, then adjust pH=2.0 with 2N hydrochloric acid, stir for 2.0h at 20-25℃, filter, and bake at 40℃ vacuum degree> 0.9MPa Material, 360g piperacillin acid was obtained. Appearance is off-white, needle-like powder crystal HPLC99%, content is 96.8%, total impurities 2.0%, ethyl acetate residue is 7200PPm.

Embodiment 2

[0010] Add 20g crude piperacillin to 100ml water, cool to 10-20℃, add 8% NaHCO dropwise 3 Aqueous solution, stir to clear, filter, then add filtered ethyl acetate and acetone mixture (mixing ratio of ethyl acetate in the mixture is 30% by volume) about 200ml, then use refined hydrochloric acid to adjust the pH = 1.5-2.0 , Then cooled to 0-5°C, crystallized for 2.0-3.0h, filtered, vacuum-baked at 50-55°C to obtain 18.6g of white granular crystalline piperacillin acid monohydrate. Its chemical structure is shown below, HPLC≥99.6 %, the content is: 99.9%, single impurity <0.1%, residual ethyl acetate and acetone ≤3000ppm.

[0011]

Embodiment 3

[0013] Add 20g of crude piperacillin to 200ml of acetone, heat to reflux to dissolve, filter while hot, cool the filtrate to 10-20°C, add 150ml of ethyl acetate dropwise (equivalent to the volume of ethyl acetate and acetone mixture The percentage is 42.8%), then cool to 0-5°C, crystallize for 2.0-3.0h, filter, and then wash with a small amount of 10ml of acetone at 0-5°C. Vacuum drying at 40-50°C to obtain 18.1 g of white granular crystals of piperacillin acid monohydrate. The chemical structure is as in Example 1, HPLC≥99.6%, content: 100.2%, single impurity <0.1%, residual Ethyl acetate and acetone≤3000ppm.

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Abstract

The invention provides a modified crystallization purifying and precipitating method of piperacillin acid, comprising the following steps: cooling crude piperacillin acid aqueous solution to 10-20 DEG C; dropwise adding sodium bicarbonate aqueous solution; filtrating; adding the mixed liquor of ethyl acetate and acetone; regulating the pH value to be 1.5-2.0 at the temperature of 10-30 DEG C; cooling to 0-10 DEG C; precipitating crystals; and filtering to obtain piperacillin monohydrate; or heating the crude product; dissolving into the acetone; filtrating while the heated crude product is hot, cooling the filter liquor to 10-20 DEG C; dropwise adding the ethyl acetate, then cooling to 0-10 DEG C to crystallize; and filtrating to obtain the piperacillin monohydrate. The piperacillin monohydrate obtained by adopting the technical scheme of the invention has higher purity, yield and content and lower residual and good fluidity, and is in a granular crystal form; the stacking density is over 0.6; the piperacillin monohydrate not only can obviously improve the stability thereof, and also can keep the inhibiting effect on beta-lactam.

Description

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Claims

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Application Information

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Owner JIANGXI FUSHINE PHARMA CO LTD
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