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Method for measuring impurity in carboxymethyl chitosan by liquid chromatography

A technology of carboxymethyl chitosan and liquid chromatography is applied in the field of separation and determination of impurities in carboxymethyl chitosan by liquid chromatography, which can solve problems such as limited application and achieve the effect of quality assurance.

Inactive Publication Date: 2009-08-05
OCEAN UNIV OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Chitin is the second largest natural polysaccharide compound after cellulose in storage capacity in nature. Its chemical structure is β-(1→4)-2-N-acetylamino-2-deoxy-D-glucose. The product of acetyl group is chitosan, because neither chitin nor chitosan can be directly dissolved in water, which greatly limits its application

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  • Method for measuring impurity in carboxymethyl chitosan by liquid chromatography
  • Method for measuring impurity in carboxymethyl chitosan by liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0029] Instruments and Conditions

[0030] WATERS high-performance liquid chromatography; chromatographic column: Symmetry300 C18 (4.6 x 150mm); mobile phase: (0.01mmol / L potassium dihydrogen phosphate buffer solution, adjusted to pH2.0 with phosphoric acid)-methanol=97:3; flow rate: 0.5 ml / min; detection wavelength: 210nm; injection volume: 20μl

[0031] Implementation steps

[0032] Take an appropriate amount of carboxymethyl chitosan sample, add methanol:water solution with a volume ratio of 7:3, ultrasonically extract for 10 minutes, centrifuge at 6000r / min for 10 minutes, and dilute with mobile phase to prepare a sample solution to be tested.

[0033] Take the sample solution to be tested, carry out high performance liquid chromatography analysis according to the above conditions, record the chromatogram, the results are shown in the attached figure 1 .

[0034] attached figure 1 The chromatographic peak whose retention time is 3.771min is DGA, attached figure 1 It s...

Embodiment 2

[0036] Instruments and Conditions

[0037] WATERS high-performance liquid chromatography; chromatographic column: Symmetry300 C18 (4.6 x 150mm); mobile phase: (0.005mmol / L potassium dihydrogen phosphate buffer solution, adjusted to pH2.0 with phosphoric acid)-methanol=97:3; flow rate: 0.5 ml / min; detection wavelength: 210nm; injection volume: 20μl

[0038] Implementation steps

[0039] Take an appropriate amount of carboxymethyl chitosan sample, add methanol:water solution with a volume ratio of 7:3, ultrasonically extract for 10 minutes, centrifuge at 6000r / min for 10 minutes, and dilute with mobile phase to prepare a sample solution to be tested.

[0040] Take the sample solution to be tested, carry out high performance liquid chromatography analysis according to the above conditions, record the chromatogram, the results are shown in the attached figure 2 .

[0041] attached figure 1 The chromatographic peak whose retention time is 4.002min is DGA, attached figure 2 I...

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Abstract

The invention relates to a method for separating and measuring the impurity-diglycol acid (natrium) (DGA) in carboxymethyl chitosan by a liquid chromatography method. A high-efficiency liquid chromatography method for separating and measuring the impurity DGA in carboxymethyl chitosan products adopts a chromatographic column taking C18 as stuffing, takes mixed solutions prepared by buffer salts with the PH value being 1.5-3.5 and organic phases according to a certain mixture ratio as a flowing phase, and performs detection and quantization by an ultraviolet detector. The method can effectively separate and measure the impurity DGA in the carboxymethyl chitosan and solves the problem of separation and measurement of the impurity DGA in the carboxymethyl chitosan, thereby ensuring the controllable quality of the carboxymethyl chitosan.

Description

technical field [0001] The invention relates to a method for separating and measuring impurities in carboxymethyl chitosan by liquid chromatography. Background technique [0002] Chitin is the second largest natural polysaccharide compound after cellulose in the storage capacity of nature. Its chemical structure is β-(1→4)-2-N-acetylamino-2-deoxy-D-glucose. The product of the acetyl group is chitosan, and both chitin and chitosan are not directly soluble in water, which greatly limits their application. Chitosan reacts with chloroacetic acid under alkaline conditions to obtain carboxymethylated chitosan. Compared with chitosan, carboxymethyl chitosan has better water solubility, so it is widely used in medicine, biomedical engineering, etc. The field has a wide range of applications. During the healing process after surgery, due to the proliferation and infiltration of fibrous tissue around the incision, adhesions inevitably occur, which can lead to sequelae such as intest...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/50G01N30/36
Inventor 吕志华王远红姜廷福管华诗
Owner OCEAN UNIV OF CHINA
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