Automatic headspace gas chromatography method for rapidly measuring 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 high activation energy
Inactive Publication Date: 2019-09-06
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
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[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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The invention belongs to the technical field of analysis and detection and discloses an automatic headspace gas chromatography method for rapidly measuring chitosan deacetylation degree. After a chitosan sample is dissolved through adoption of a hydrochloric acid solution, certain volume is transferred to a headspace bottle, and then the headspace bottle is sealed. The sodium bicarbonate solutionwith different volume is injected through adoption of an injector. Moreover, the hydrochloric acid solution without the chitosan is taken as blank. Headspace gas chromatography detection is carried out on a prepared sample. A gas chromatography signal value of carbon dioxide is recorded. A difference value between an obtained sample signal and a blank signal is solved. A curve is drawn for the volume of the sodium bicarbonate solution according to the difference value, two outstanding turning points are obtained, and deacetylation degree of the chitosan is computed according to the two outstanding turning points. The method has good measurement precision (RSD is smaller than 0.82%) and good accuracy (compared with a result measured by a reference method, a relative error is smaller than 6.46%). According to HS-GC, automatic sample reaction balance and measurement can be carried out, so the method is relatively effective in batch sample measurement and analysis.
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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Login to View More IPC IPC(8): G01N30/02G01N30/16
CPCG01N30/02G01N30/16
Inventor 闫宁柴欣生
Owner SOUTH CHINA UNIV OF TECH