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Method for detecting residual solvent, monomer and initiator decomposition product of tertiary amine containing methacrylate copolymer

Active Publication Date: 2019-11-26
广州茂丰药业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, liquid chromatography cannot simultaneously detect residual solvents and initiator decomposition products without UV absorption (such as: tetramethylsuccinonitrile)

Method used

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  • Method for detecting residual solvent, monomer and initiator decomposition product of tertiary amine containing methacrylate copolymer
  • Method for detecting residual solvent, monomer and initiator decomposition product of tertiary amine containing methacrylate copolymer
  • Method for detecting residual solvent, monomer and initiator decomposition product of tertiary amine containing methacrylate copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] This embodiment is a method for detecting residual solvents, monomers and initiator decomposition products of tertiary amino methacrylate copolymers of the present invention

[0061] Test products: E100, a product from Evonik Rohm, Germany, E100, a product from Guangzhou Maofeng Pharmaceutical Co., Ltd., and polyacrylic resin IV from a domestic W / Z / S / A manufacturer. Test results such as Figure 1-Figure 7 Shown.

[0062] The method for detecting residual solvents, monomers and initiator decomposition products in the tertiary amino group-containing methacrylate copolymer includes the following steps:

[0063] (1) Preparation of test solution: Take about 70ml of phosphoric acid mixed solution (weigh 93.0g of phosphoric acid, 80.0g of anhydrous sodium sulfate and 5.0g of p-hydroxyanisole, add water to dissolve and dilute to 1000ml, shake well), set In a 150ml conical flask with stopper, electromagnetic stirring. Take 10.0g of the sample to be tested after crushing, accurately w...

Embodiment 2

[0098] This embodiment is an example of detection of the residual solvent, monomer and initiator decomposition products of another tertiary amino methacrylate copolymer in the present invention

[0099] Test product (containing tertiary amino methacrylate copolymer): Guangzhou Maofeng Pharmaceutical Co., Ltd. self-produced methyl methacrylate-diethylaminoethyl methacrylate (55:45) copolymer.

[0100] According to the preparation method of the test solution and the reference solution in Example 1, but the phosphoric acid was replaced with sulfuric acid to prepare the test solution and the reference solution. The calculation is the same as in Example 1.

[0101] Test result: see the test chart of the test solution Picture 9 It can be seen from the figure that the detection method of the present invention can also be applied to the detection of another tertiary amino-containing methacrylate copolymer that is different from Example 1. The residual solvent methanol (5ppm) and ethanol are...

Embodiment 3

[0103] Prepare the solution according to the method in Example 1, prepare the test solution of Guangzhou Maofeng Pharmaceutical Co., Ltd. self-produced E100, add sodium hydroxide solution to adjust the pH to 1.5, 2.5, 3.5, and 5 respectively, and take part of the test product. The solution prepares the reference solution. When pH>5, the precipitation and flocculation in the test solution is difficult to reconstitute and is not applicable, so no comparison was made. Each sample was injected for testing, and another sample was injected 12 hours later. The test results are summarized and compared to the difference in peak area of ​​the test solution and the reference solution. The experimental results are shown in Table 9 and Table 10:

[0104] Table 9 Stability of the test solution under different pH values ​​(peak area comparison table)

[0105]

[0106]

[0107] It can be seen from Table 9 above that the test solution of Example 3 showed no significant change in the peak area of ...

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Abstract

The invention, which belongs to the technical field of polymer copolymer detection methods, relates to a method for detecting a residual solvent, a monomer and an initiator decomposition product of atertiary amine containing methacrylate copolymer. According to the provided detection method, the copolymer is dissolved by using acid or a mixed solution of acid and a high-boiling-point organic solvent; a test solution is prepared when a pH value is adjusted and to-be-tested component reference substances are added into the test solution to prepare a reference solution; and sample injection analysis is carried out by using headspace gas chromatography. According to the provided detection method, residual monomers (C1-C4 alkyl ester of methacrylic acid), residual solvents (methanol, ethanol,isopropanol, butanol and benzene) and initiator decomposition products (methyl isobutyrate, dimethyl methylsuccinate, and tetramethylsuccinonitrile) in the copolymer can be accurately detected at thesame time; and problems of the matrix effect and precipitation of water-insoluble to-be-detected components are solved.

Description

Technical field [0001] The invention relates to a detection method for residual solvent, monomer and initiator decomposition products in a tertiary amino-containing methacrylate copolymer, and belongs to the technical field of detection methods for polymer copolymers. Background technique [0002] The tertiary amino methacrylate copolymer is often used in the fields of moisture prevention, taste masking, isolation, gastric dissolution, coating and dermatology of oral pharmaceutical preparations, and has been widely recognized by the drug regulatory agencies of various countries and included in the national pharmacopoeia . The formula ratio of these copolymer monomers has long been published by the pharmacopoeias and regulations of various countries. Especially well-known types of pharmaceutical excipients, such as polyacrylic resin IV, also called amino methacrylate copolymer (USP / NF-Amino Methacrylate Copolymer), basic butylated methacrylate copolymer (Ph.Eur-BASIC) BUTYLATED ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 杨海峰周凤书
Owner 广州茂丰药业有限公司
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