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Method for measuring amino group contents of chitosan derivatives on basis of headspace gas chromatography

A chitosan derivative, headspace gas chromatography technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of difficulty in popularization, expensive nuclear magnetic resonance equipment, etc., and achieve the effect of less sample consumption

Inactive Publication Date: 2019-07-30
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although NMR has been established as the standard for the determination of chitin deacetylation and is usually used to calibrate other methods, NMR equipment is expensive and requires professional technicians to operate, making it difficult to popularize

Method used

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  • Method for measuring amino group contents of chitosan derivatives on basis of headspace gas chromatography
  • Method for measuring amino group contents of chitosan derivatives on basis of headspace gas chromatography
  • Method for measuring amino group contents of chitosan derivatives on basis of headspace gas chromatography

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Embodiment

[0037] (1) Standard sample preparation: Accurately weigh five samples of glucosamine hydrochloride (0.0100g, 0.0150g, 0.0200g, 0.0250g, 0.0300g), put them into 20ml headspace sampling vials respectively, and pour them into the headspace vials. Add 7ml of 0.01g / mL ninhydrin solution to the sample to disperse the sample evenly, then gently put it into the glass vial, carefully add 0.9mL of sodium bicarbonate solution (concentration 1.2mol / L) with a pipette gun, and seal it with the bottle cap ; put the whole headspace vial in a water bath at 90°C for 15 minutes, shake the vial manually to mix the sodium bicarbonate in the glass vial with the ninhydrin solution containing chitosan derivatives, and then place it at 60 ℃ water bath reaction for 60 minutes; also prepare a control blank bottle (does not contain glucosamine hydrochloride), and the others are exactly the same as above. After the reaction, it can be clearly found that purple substances were formed in the headspace vials...

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Abstract

The invention discloses a method for measuring amino group contents of chitosan derivatives on the basis of headspace gas chromatography. According to the method, excess ninhydrin is reacted with a standard substance containing an amino group; sodium hydrogencarbonate is reacted with the remaining ninhydrin to generate carbon dioxide; the standard substance is not added in a control group; the peak area of carbon dioxide is measured through the headspace gas chromatography; the relative reduction of the carbon dioxide is in a linear relationship with the mass of the standard substance; a standard curve is established and the standard substance is replaced by a chitosan derivative, the amino group content of which is to be measured; and the peak area of the carbon dioxide is detected; the mass of the corresponding standard substance at the moment is obtained according to the standard curve; and calculation is carried out to obtain the amino group content at the moment. When the method is compared with the traditional conductometric titration method, the relative errors do not exceed 13.03%, and for the detection of a same sample, the maximum relative standard deviation is 4.83%, sothe results are objective and accurate and the method is higher in speed when being compared with the traditional measuring methods.

Description

technical field [0001] The invention relates to the technical field of determining the amino content of chitosan derivatives, in particular to a method for measuring the amino content of chitosan derivatives based on headspace gas chromatography. Background technique [0002] Headspace gas chromatography, also known as headspace gas chromatography. Headspace gas chromatography uses the principle that after the volatile components in the liquid (solid) body reach equilibrium in a closed constant temperature system, the ratio of the volatile components in the gas phase and the liquid (solid) phase is constant, and the vapor in the upper part of the liquid (solid) after equilibrium is analyzed. Perform gas chromatographic analysis. It can also carry out targeted chemical reactions during the sample balance process, and convert the components (non-volatile) that cannot be determined by gas chromatography into volatile components, so as to realize the detection of the non-volati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/16
CPCG01N30/02G01N30/16
Inventor 万小芳刘梦珍陈广学柴欣生
Owner SOUTH CHINA UNIV OF TECH
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