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Gas chromatographic analysis method for rapid determination of characteristic polymer material in mixture

A polymer material, rapid determination technology, applied in material separation, analysis materials, measurement devices, etc., can solve problems such as poor specificity, difficult analysis, and inability to be determined by optical detectors

Active Publication Date: 2015-04-01
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 chromatographic analysis method for rapid determination of characteristic polymer material in mixture
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  • Gas chromatographic analysis method for rapid determination of characteristic polymer material in mixture

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 laye...

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Abstract

The invention discloses a gas chromatographic analysis method for rapid determination of a characteristic polymer material in a mixture. The method comprises the following steps: firstly pouring a mixture powder to be measured into a reaction flask, adding an n-octane internal standard solution and an adipic acid solution; adding hydroiodic acid into the above reaction flask and sealing and weighing; putting the reaction flask into a drying oven, fully reacting, taking out the reaction flask, cooling, weighing, taking a supernatant as a test article for analysis; analyzing the test article by a gas chromatographic analysis method and acquiring data by starting a chromatographic acquisition computer system; and taking methyl iodide, ethyl iodide and isopropyl iodide compounds and transferring the compounds into a small glass bottle with a plug, adding 2ml of the n-octane internal standard solution and 2ml of the adipic acid solution, simultaneously carrying out gas chromatographic analysis, and calculating content of the characteristic polymer material in the mixture. The method provided by the invention has advantages of strong specificity, rapid analysis, strong resistance to 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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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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