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A kind of control method of chondroitin sulfate ethanol residue

A chondroitin sulfate and control method technology, applied in the field of chemical pharmacy, can solve problems such as time-consuming, and achieve the effects of being easy to scale up production and easy to operate

Active Publication Date: 2020-06-23
QINGDAO WANTUMING BIOLOGICAL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time, and the drying time alone exceeds 30 hours

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add the refined shark chondroitin sulfate feed solution into 95% ethanol with 4 times the volume of the feed solution, and stir with a high-shear emulsifier to obtain particles with a diameter of 1-2 mm. Add 95% ethanol with twice the volume of the precipitate, stir and add appropriate amount of purified water to make the first dehydration ethanol concentration 75 degrees, time is 1 hour, drain the ethanol and add 95% ethanol with double the volume of the precipitate, stir and Add an appropriate amount of purified water to make the ethanol concentration 86 degrees, and the time is 2 hours. Drain the ethanol in the chondroitin sulfate precipitate, put it into a hot air circulation oven after putting it into a plate, first raise the temperature to 55-65°C, and dry for 3 hours; turn over the plate, then raise the temperature to 75-88°C, and dry until the moisture is less than 10%. The resulting product ethanol residue is 700ppm.

Embodiment 2

[0025] Add the refined chicken breast cartilage chondroitin sulfate feed solution into 95% ethanol with 4 times the volume of the feed solution, and stir with a high-shear emulsifier to obtain particles with a diameter of 1-2 mm. Remove the ethanol in the upper layer, add 95% ethanol with twice the volume of the precipitate, stir and add an appropriate amount of purified water to make the first dehydration ethanol concentration 77 degrees, and the time is 1 hour, drain the ethanol and add 95% ethanol with one volume of the precipitate % ethanol, stir and add an appropriate amount of purified water to make the ethanol concentration 88 degrees for 2 hours. Drain the ethanol in the chondroitin sulfate precipitate, put it into a hot air circulation oven after putting it into a plate, first raise the temperature to 55-65°C, and dry for 3 hours; turn over the plate, then raise the temperature to 75-88°C, and dry until the moisture is less than 10%. The resulting product ethanol resi...

Embodiment 3

[0027] Add the refined bovine nasal bone chondroitin sulfate feed solution into 95% ethanol with 4 times the volume of the feed solution, and stir with a high-shear emulsifier to obtain particles with a diameter of 1-2 mm. Take out the ethanol in the upper layer, add 95% ethanol with twice the volume of the precipitate, stir and add an appropriate amount of purified water to make the first dehydration ethanol concentration 80 degrees, and the time is 1 hour, drain the ethanol and add 95% % ethanol, stir and add an appropriate amount of purified water to make the ethanol concentration 90 degrees for 2 hours. Drain the ethanol in the chondroitin sulfate precipitate, put it into a hot air circulation oven after putting it into a plate, first raise the temperature to 55-65°C, and dry for 3 hours; turn over the plate and then raise the temperature to 75-88°C, and dry until the moisture is less than 10%. The residual ethanol content of the product obtained is 210ppm.

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Abstract

The invention relates to a control method of ethanol residues in chondroitin sulfate and belongs to the technical field of chemical pharmacy. Chondroitin sulfate with precipitated ethanol is crushed into particles with the diameter not larger than 2 mm and dehydrated with ethanol with the gradually increasing concentration, the ethanol in chondroitin sulfate precipitates is sucked, and chondroitin sulfate is placed in a plate, then placed in a hot air circulating oven, firstly heated to 55-65 DEG C and then dried for 3 h; chondroitin sulfate is heated to 75-88 DEG C after the plate is turned and dried until the moisture is up to the standard, and a chondroitin sulfate product with the ethanol content smaller than 1,000 ppm is obtained. The method has the benefits as follows: chondroitin sulfate is gradually dehydrated with ethanol with the gradually increasing concentration, and the treated chondroitin sulfate precipitates can be quickly dried to have very low ethanol residue level with a common hot air circulating oven instead of a vacuum oven; the technology facilitates enlarged production, requires no additional equipment and is easy to operate.

Description

technical field [0001] The invention relates to a method for controlling chondroitin sulfate ethanol residue, which belongs to the technical field of chemical pharmacy. Background technique [0002] In the production process of medicinal chondroitin sulfate, ethanol precipitation is often used to separate chondroitin sulfate from impurities, and to precipitate chondroitin sulfate from the solution. Therefore, in the quality standards of chondroitin sulfate products, ethanol residue is an important inspection index. However, due to the characteristics of chondroitin sulfate amorphous crystal, the content of ethanol is difficult to control. [0003] There are various methods for controlling the residue of ethanol in the existing literature, most of which are found in products such as heparin. For example, in the invention patent of application number 201210551437.5 "A Process for Reducing Organic Solvent Residue in Heparin Sodium", it is mentioned that the method of reducing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
CPCC08B37/0003C08B37/0069
Inventor 李燕妮
Owner QINGDAO WANTUMING BIOLOGICAL PROD
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