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A kind of purification method of milbemycin oxime crude product

A technology of milbemycin oxime and milbemycin oxime, which is applied in the field of purification of crude milbemycin oxime, can solve problems such as incomplete crystal form, decreased extraction yield, and wide crystal particle size distribution, so as to reduce the pressure on environmental protection , Improving the quality of finished products and enhancing the competitiveness

Active Publication Date: 2017-12-26
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1 Using activated carbon for decolorization, the extraction yield decreased by about 3%
[0005] 2 It has been verified that the patent "a method for preparing high-purity milbexime" only uses resin chromatography technology, which cannot effectively remove impurities introduced during the synthesis process, and the effective content is less than 95%
[0006] 3 The patent states that the conventional cooling crystallization method may easily lead to low purity of milbemycin oxime crystals, incomplete crystal form, excessively wide crystal particle size distribution, and prone to crystal bonding
Difficult for long-term storage, transportation and use
[0007] 4 The product properties of milbemycin oxime do not meet the standards of the United States Pharmacopoeia

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Milbemycin oxime crude product 100kg, add purified water 1300L, add 30% ammonia solution, adjust the pH to 8, stir for 40min, obtain the wet product of Milbemycin oxime after filtration, continue to add purified water 600L, stir for 20min, filter The wet product of milbemycin oxime was obtained.

[0034] Milbemycin oxime wet product is dissolved in butyl acetate, the concentration is controlled at 16%, and the volume is 625L.

[0035] The milbemycin oxime solution is decolorized by macroporous resin, the feed rate is controlled at 2BV / h, and the output rate is controlled at 1.1BV / h. The filtrate 624L was collected.

[0036] Add 1875 L of purified water to the milbemycin oxime solution, stir for 30 minutes, let stand to separate layers and filter to obtain 678 L of milbemycin oxime organic solution.

[0037] Add 2.71 kg of anhydrous calcium chloride to the milbemycin oxime solution, and collect 625 L of filtrate after filtration.

[0038] Add 625 L of purified water t...

Embodiment 2

[0042] Milbemycin oxime crude product 100kg, add 1400L of purified water, add 33% ammonia solution, adjust the pH to 8.2, stir for 45min, obtain the wet product of milbemycin oxime after filtration, continue to add 700L of purified water, stir for 25min, filter The wet product of milbemycin oxime was obtained.

[0043] Milbemycin oxime wet product is dissolved in isobutyl acetate, the concentration is controlled at 17%, and the volume is 590L.

[0044] The milbemycin oxime solution is decolorized by macroporous resin, the feed rate is controlled at 2.3BV / h, and the output rate is controlled at 1.2BV / h. The filtrate 589L was collected.

[0045] Add 2061 L of purified water to the milbemycin oxime solution, stir for 35 minutes, let stand to separate layers and filter to obtain 640 L of milbemycin oxime organic solution.

[0046] Add 3.2 kg of anhydrous calcium chloride to the milbemycin oxime solution, and collect 590 L of filtrate after filtration.

[0047] Add 767L of purif...

Embodiment 3

[0051] Milbemycin oxime crude product 100kg, add purified water 1500L, add 35% ammonia solution, adjust the pH to 8.5, stir for 50min, obtain the wet product of Milbemycin oxime after filtration, continue to add purified water 800L, stir for 30min, filter The wet product of milbemycin oxime was obtained.

[0052] Milbemycin oxime wet product is dissolved in butyl acetate, the concentration is controlled at 18%, and the volume is 556L.

[0053] The milbemycin oxime solution is decolorized by macroporous resin, the feed rate is controlled at 2.5BV / h, and the output rate is controlled at 1.5BV / h. Collect filtrate 555L.

[0054] Add 2220 L of purified water to the milbemycin oxime solution, stir for 40 minutes, let stand to separate layers and filter to obtain 602 L of milbemycin oxime organic solution.

[0055] Add 3.6 kg of anhydrous calcium chloride to the milbemycin oxime solution, and collect 601 L of filtrate after filtration.

[0056] Add 902 L of purified water to the mil...

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Abstract

The invention relates to a purification method of a milbemycin oxime crude product. The method includes the process steps that firstly, the milbemycin oxime crude product is washed at the pH of 8-9; then, a milbemycin oxime wet product obtained after filtering is dissolved in butyl acetate or isobutyl acetate and then decolored with macroporous resin, water is added for mixing, standing layering and filtering are carried out, obtained filter liquor is dried with anhydrous calcium chloride, filter liquor is collected after filtering, water is added again for mixing, filtering and drying are carried out after heating crystallization, and a milbemycin oxime pure product can be obtained. By means of the method, impurities in the milbemycin oxime crude product are effectively separated, the quality of the finished product is improved, and the home and abroad market competiveness of the product is easily enhanced.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction, in particular to a method for purifying crude milbemycin oxime. Background technique [0002] Milbemycin oxime is a new type of semi-synthetic macrolide anthelmintic drug, which is an oxime derivative of milbemycin A3 and A4, and has a good effect on the control and prevention of most common parasitic diseases. It is usually used to prevent heartworm disease, control dog and cat diseases caused by nematodes and hookworms, and whipworm disease in dogs. Because milbexime has good repellent effect on both internal and external parasites, and has less toxicity to dogs sensitive to avermectins, its application and research have attracted more and more attention. [0003] At present, relevant domestic literature reports the purification of milbemycin by using activated carbon decolorization and chromatography; the patent "a method for preparing high-purity milbemycin" (CN201410429785.4) ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 任勇
Owner 宁夏泰瑞制药股份有限公司
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