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Gas-phase analytical method for rapid determination of characteristic polymeric materials in mixtures

A technology of polymer materials and analysis methods, which is applied in the field of gas-phase analysis for the rapid determination of characteristic polymer materials in mixtures, and can solve problems such as poor specificity, difficult analysis, and inability to be detected by optical detectors.

Active Publication Date: 2016-09-07
NOVAST LABORATORIES (CHINA) LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In practical work, the qualitative and quantitative analysis of some polymers is difficult, especially the mixture of several polymers is difficult to analyze by conventional methods
For example: some commonly used polymer materials: hypromellose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, polyethylene glycol, hydroxyethyl cellulose, Eudragit, etc., are not UV response, cannot be determined by conventional HPLC method with optical detector
[0003] For the above polymer materials, there are usually only corresponding pure product quality control methods, and most of them are determined by chemical volumetric method. These methods have poor specificity and low sensitivity, and are only suitable for constant analysis of pure products.
For example: the method for determining the content of ethyl cellulose in the Chinese Pharmacopoeia 2005 edition is to first digest the sample, and then use sodium thiosulfate titration, the specificity of this method is poor
In the 2010 edition of the Chinese Pharmacopoeia, there are similar methods for the determination of methoxyl, ethoxyl, and hydroxypropoxyl respectively, but they are only applicable to the detection of pure products and are basically incapable of complex systems.

Method used

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  • Gas-phase analytical method for rapid determination of characteristic polymeric materials in mixtures
  • Gas-phase analytical method for rapid determination of characteristic polymeric materials in mixtures
  • Gas-phase analytical method for rapid determination of characteristic polymeric materials in mixtures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Determination of the content and specification of hypromellose in quetiapine fumarate sustained-release tablets (Seruquel®, specification: 200mg):

[0023] (1), instruments and conditions

[0024] Gas chromatograph: American Agilent 7890A chromatographic system and workstation;

[0025] Chromatographic column: Agilent DB-1 Fused Silica, 0.53mm×30m, bonded with 3μm layer of G1;

[0026] Injection port temperature: 250°C; Sampling method: split injection 40:1; Carrier gas: high-purity helium, constant flow rate 4.2 milliliters / minute; Programmable temperature rise: initial temperature 50°C, keep 3 minutes, with Rise to 100°C at 10°C / min, then rise to 250°C at 34.9°C / min, hold for 8 minutes; FID detection port temperature: 280°C, injection volume 1μL;

[0027] (2), experimental steps

[0028] Transfer about 200mg of quetiapine fumarate tablet powder to a reaction flask, add 2ml of internal standard solution and 2ml of adipic acid solution to the reaction flask, then add...

Embodiment 2

[0038] Determination of the content and specification of hypromellose in the core of nifedipine sustained-release tablets (NifedicalTM, specification: 30mg):

[0039]Hypromellose contains methoxy and isopropoxy groups, which can be converted into iodide for content determination. Since the active ingredient nifedipine in the core of the nifedipine sustained-release tablet contains methoxy groups, Therefore, it will interfere with the determination of hypromellose. According to the solubility difference between the two, use the organic solvent ethyl acetate to separate nifedipine and then measure the content of hypromellose;

[0040] (1) Instruments and conditions

[0041] Gas chromatograph: American Agilent 7890A chromatographic system and workstation;

[0042] Chromatographic column: Agilent DB-1 Fused Silica, 0.53mm×30m, bonded with 3μm layer of G1;

[0043] Injection port temperature: 250°C; Sampling method: split injection 40:1; Carrier gas: high-purity helium, constant ...

Embodiment 3

[0053] Glipizide sustained-release tablet (specification: 50mg), simultaneous determination of the content and specification of Eudragit and ethylcellulose in the coating:

[0054] Eudragit contains methoxy groups, and ethyl cellulose contains ethoxy groups. Through the reaction, they can be converted into methyl iodide and ethyl iodide respectively for the content determination of Eudragit and ethyl cellulose. Another polymer polyethylene glycol in the release tablet coating also contains ethoxy groups, so it will interfere with the determination of ethyl cellulose. It has good solubility and is insoluble in water, and Eudragit is also basically insoluble in water, so polyethylene glycol is separated with water to determine Eudragit and ethyl cellulose;

[0055] (1) Instruments and conditions

[0056] Gas chromatograph: American Agilent 7890A chromatographic system and workstation;

[0057] Chromatographic column: Agilent DB-1 Fused Silica, 0.53mm×30m, bonded with 3μm layer...

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Abstract

The invention discloses a gas-phase analysis method for quickly measuring characteristic polymer materials in a mixture, which comprises the following steps: firstly, powder the mixture to be measured into a reaction bottle, then add n-octane internal standard solution and adipic acid solution; added hydrogen Put the iodic acid into the above-mentioned reaction bottle and seal it and weigh it; put the reaction bottle in an oven, react fully, take it out and let it cool, weigh again, and take the supernatant as the test sample for analysis; use gas chromatography to analyze the test sample product, start the chromatographic acquisition computer system to collect data; take methyl iodide, ethyl iodide and isopropyl iodide compounds, and transfer them to a stoppered glass vial, add 2ml of n-octane internal standard solution and 2ml of adipic acid The solution was analyzed by gas chromatography at the same time, and then the content of the characteristic polymer in the mixture was calculated. The invention has the advantages of strong specificity, rapid analysis, strong anti-interference and high sensitivity.

Description

technical field [0001] The invention specifically relates to a gas phase analysis method, in particular to a gas phase analysis method for rapidly determining characteristic polymer materials in a mixture. Background technique [0002] In practical work, the qualitative and quantitative analysis of some polymers is difficult, especially the mixture of several polymers is difficult to analyze by conventional methods. For example: some commonly used polymer materials: hypromellose, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, polyethylene glycol, hydroxyethyl cellulose, Eudragit, etc., are not Ultraviolet response, which cannot be determined by conventional HPLC method with optical detector. [0003] For the above polymer materials, there are often only corresponding pure product quality control methods, and most of them are determined by chemical volumetric method. These methods have poor specificity and low sensitivity, and are only suitable for constan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 胡廷默胡成松王海霞金燕房杏春陈义生张国华
Owner NOVAST LABORATORIES (CHINA) LTD
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