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An automatic headspace gas chromatography method for rapid determination of chitosan deacetylation degree

A technology of headspace gas chromatography and degree of deacetylation, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of daily detection and interference of the degree of deacetylation that cannot be used in chitosan, and achieve batch automatic detection , high precision, and the effect of improving experimental efficiency

Inactive Publication Date: 2021-05-14
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

However, because these methods have some or other problems in the detection principle, such as: the interference of crystal water, adsorbed water or a small amount of impurities in the chitosan sample on the spectroscopic method, these methods have basically not been used for chitosan. In the daily detection of the degree of deacetylation of sugar

Method used

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  • An automatic headspace gas chromatography method for rapid determination of chitosan deacetylation degree
  • An automatic headspace gas chromatography method for rapid determination of chitosan deacetylation degree
  • An automatic headspace gas chromatography method for rapid determination of chitosan deacetylation degree

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Embodiment

[0037] The present embodiment measures the degree of deacetylation of 4 kinds of commercially available chitosans, and the concrete determination steps are as follows:

[0038] (1) Sample preparation: Accurately weigh 0.200g of chitosan sample, dissolve it in a hydrochloric acid solution with a concentration of 0.1mol / L and a volume of 20mL, and accurately pipette 1mL of the above-mentioned mixture into a 21.6mL top with a pipette gun. Immediately seal the empty bottle, and inject the volume with a syringe into 0.40mL, 0.50mL, 0.60mL, 0.70mL, 0.80mL, 0.85mL, 0.90mL, 0.95mL, 1.00mL, 1.05mL, 1.10mL, 1.15mL, 1.20mL, 1.30mL, 1.40mL, 1.50mL of sodium bicarbonate solution, while using hydrochloric acid solution without chitosan as a blank;

[0039] (2) Sample detection: the sample bottle prepared in (1) is placed in the headspace sampler, and the operating conditions of the headspace sampler and the gas chromatograph are set (the operating conditions of the headspace sampler are: eq...

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Abstract

The invention belongs to the technical field of analysis and detection, and discloses an automatic headspace gas chromatography method for quickly measuring the deacetylation degree of chitosan. Dissolve the chitosan sample with hydrochloric acid solution, pipette a certain volume and seal it in a headspace vial, inject different volumes of sodium bicarbonate solution with a syringe, and use the hydrochloric acid solution without chitosan as a blank; then prepare the sample Carry out headspace gas chromatographic detection, record the gas chromatographic signal value of carbon dioxide; make a difference between the obtained sample signal and the blank signal, and draw a curve with the difference value against the volume of sodium bicarbonate solution to obtain two significant turning points, and calculate accordingly The degree of deacetylation of chitosan was obtained. The method has good measurement precision (RSD<0.82%) and accuracy (relative error<6.46% compared with the result measured by the reference method). The HS‑GC is more efficient in batch sample test analysis due to automated sample reaction equilibration and measurement.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to an automatic headspace gas chromatography method for quickly measuring the deacetylation degree of chitosan. Background technique [0002] Chitosan (also known as deacetylated chitin, soluble chitin, etc.) is a deacetylated product of natural polysaccharide chitin, which is composed of two monomers, chitin and chitosan (β-(1,4)-2-acetyl Amino-2-deoxy-D-glucose monosaccharide and β-(1,4)-2-amino-2-deoxy-D-glucan monosaccharide). [0003] In addition to containing hydroxyl groups, chitosan macromolecular chains also contain free amine groups, which make it have good reactivity and solubility in acidic media. Therefore, it is widely used in food, textile, paper, pharmaceutical, environmental protection and chemical industries. It has broad application prospects, such as: it can be used as a fresh-keeping preservative and thickener in food, it can be used as a hemosta...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/16
CPCG01N30/02G01N30/16
Inventor 闫宁柴欣生
Owner SOUTH CHINA UNIV OF TECH
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