Method for determining glucose and gluconic acid in oxidized dextrin

A determination method and a technology for oxidative dextrin, applied in the field of medicine, can solve the problems of low sensitivity, inappropriate peak time, indeterminate gluconic acid content, etc., and achieve the effect of high sensitivity

Pending Publication Date: 2021-03-05
JIANGSU AOSAIKANG PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The ultraviolet spectrophotometer method can only be used to determine the glucose content in the sample, and the gluconic acid content cannot be determined.
High-performance liquid phase (HPLC) method is currently widely used as an analysis method, among which ion chromatography uses ion exclusion to separate, but the peak position of the reactant glucose and its oxidation product sodium gluconate coincides, requiring a series of ultraviolet detectors and differential detectors detection, the sensitivity of this method is relatively low, and the detection results are not ideal enough, and in the existing anion column IonPac AS11-HC utilizing the integral pulse amperometric detection method, NaOH of 5mmol / L is used as the eluent, and the elution ability for glucose is relatively low. Weak, while using a 250mm ion chromatography column, the peak time of glucose is about 3 minutes, and the peak time is not suitable

Method used

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  • Method for determining glucose and gluconic acid in oxidized dextrin
  • Method for determining glucose and gluconic acid in oxidized dextrin
  • Method for determining glucose and gluconic acid in oxidized dextrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of sample solution:

[0041] (1) Weigh 0.1g of the oxidized dextrin sample, add 1ml of sulfuric acid with a mass percentage of 10%, destroy it in an oil bath at 100°C for 1h, and dilute to 10ml with water after cooling;

[0042] (2) Measure 0.2 ml of the solution obtained in step (1), dilute to 100 ml with water, mix well, pass through a 0.22 micron water film as the sample solution.

[0043] Preparation of mobile phase solution:

[0044] (1) Preparation of 200mmol / L NaOH solution: Measure 16ml of NaOH solution with a mass percentage of 50% into a beaker, add 1000ml of water, stir evenly, pass through a 0.22 micron water film, and put it into the mobile phase bottle;

[0045] (2) Preparation of 500mmol / L NaOAc solution: Weigh 41g NaOAc into a beaker filled with 10001ml water, stir to dissolve, pass through a 0.22 micron water film into the mobile phase bottle.

[0046] Preparation of standard curve solution:

[0047] (1) Weigh 20mg of glucose and 5.2mg of...

Embodiment 2

[0051] Ion chromatography instrument selection and parameter setting:

[0052] Instrument model: Thermo-Fisher ICS-5000+

[0053] Guard column name: Dionex CarboPacTM PA20 BioLCTM 3*30mm Guard

[0054] Analytical column name: Dionex CarboPacTM PA20 BioLCTM 3*150mm Analytical

[0055] Column temperature: 30°C

[0056] Electrochemical detector parameter setting:

[0057] Amperometric Parameters (Amperometric Detector) Electrode Material: Gold Electrode

[0058] Reference electrode: Ag / AgCl

[0059] Potential waveform: sugar four potential waveform

[0060] Detector temperature: 28~32℃

[0061] with mobile phase H 2 O, mobile phase NaOH solution (200mmol / L) and mobile phase NaOAc solution (500mmol / L) carry out gradient elution as eluent, and elution condition is as shown in table 1, then setting flow velocity is 0.4ml / min, carries out The sample volume was 5 μL, and the sample was injected for analysis.

[0062] Table 1

[0063] time (min) h 2 O(%)

Embodiment 3

[0065] The standard curve solution prepared in Example 1 was injected with an injection volume of 5 μL, and a standard curve was drawn. The correlation coefficients of the standard curve are shown in Table 2.

[0066] Table 2

[0067] Peak Name Cal. Type linear correlation coefficient intercept slope Linear range (mg / L) glucose LOff 0.9998 1.7420 2.8074 4～20 gluconic acid LOff 0.9999 0.0008 0.3987 1～5

[0068] Then, the sample solution prepared in Example 1 was injected, and the injection volume was 5 μL. After calculation, the contents of glucose and gluconic acid in the sample solution were shown in Table 3.

[0069] table 3

[0070]

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Abstract

The invention provides a method for determining glucose and gluconic acid in dextrin oxide. The method comprises the following four steps: preparing a sample solution, preparing a mobile phase solution, preparing a standard curve solution and detecting by an integral pulse ampere method. According to the determination method, the ion chromatography is matched with the electrochemical detector so that glucose and gluconic acid can be detected at the same time, the sensitivity is high, and the detection limit can reach ppb level.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular, the invention relates to a method for determining glucose and gluconic acid in oxidized dextrin. Background technique [0002] Dextrin is widely used in adhesive industry, paper industry, pharmaceutical industry, mining industry, food industry and textile industry. In the pharmaceutical industry, pyrolytic dextrin is widely used in excipients and binders of granule granules. After pyrolytic dextrin is separated and removed from small molecule pigments and other substances, a relatively simple dextrin is obtained, which is stable in nature and effective Very good viscosity, which can bind the active ingredients of the drug together, and it has excellent solubility, which can quickly dissolve the granules in water. The pyrolytic dextrin added to the tablet can also play a certain disintegration effect because it can be quickly dissolved in water. [0003] Oxidized dextrin is widel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/64
CPCG01N30/02G01N30/34G01N30/64
Inventor 陈庆财赵骞杨瑞峰刘霞王玲昀
Owner JIANGSU AOSAIKANG PHARMA CO LTD
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