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Method for determining trace carbohydrate impurities in amino acid bulk drug

A technology for amino acids and raw materials, which is applied in the directions of measuring devices, material separation, and analysis of materials, etc. It can solve the problems of large temperature influence, cumbersome operation steps, and low sensitivity of detectors, and achieve high precision, good repeatability, and high sensitivity. Effect

Active Publication Date: 2020-09-08
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sugars have no characteristic ultraviolet absorption characteristics, and can only be detected by ultraviolet detectors after derivatization with chromophoric groups. The operation steps are cumbersome when using ultraviolet detectors.
Although the differential refractive index detector can directly measure carbohydrates, the detector has low sensitivity, is greatly affected by temperature, and is not compatible with gradient elution

Method used

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  • Method for determining trace carbohydrate impurities in amino acid bulk drug
  • Method for determining trace carbohydrate impurities in amino acid bulk drug
  • Method for determining trace carbohydrate impurities in amino acid bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: A pretreatment method for enriching sugar in amino acid raw materials

[0035] (1) Resin pretreatment: Accurately weigh 10.0g of 732 cation exchange resin, place it in a 250ml Erlenmeyer flask, wash with water until the effluent is colorless, treat with 70mL of 5% (v / v) HCl overnight, wash with water until neutral ; Treat with an equal volume of 5% (m / v) NaOH overnight, wash with water until neutral; finally treat with 70mL of 5% (v / v) HCl overnight, then wash with water until neutral, and set aside.

[0036] (2) Amino acid sample pretreatment: Take 1 part of the pretreated resin in a 250mL conical flask, accurately weigh 0.20g of the amino acid sample and dissolve it in 100mL water, add the solution to the conical flask, and place it on a magnetic stirrer at room temperature Low-speed static adsorption until the amino acid is completely adsorbed. The solution was filtered, and the filtrate was rotary evaporated to about 30 mL, and then lyophilized at -80°C,...

Embodiment 2

[0037] Embodiment 2: the selection of pretreatment condition

[0038] (1) Choice of resin type:

[0039] Referring to the method of Example 1, the mixed solution of arginine and glucose (the concentration of arginine in the mixed solution is 2g / mL, and the concentration of glucose is 1mg / mL) is processed, the difference is that the 732 cationic resin is replaced by macroporous Adsorption resin, D113 weak acid type cation exchange resin and D001 type cation exchange resin, other conditions are the same as embodiment 1, utilize the ninhydrin method to investigate the adsorption situation of amino acid, the results are shown in figure 1 .

[0040] The adsorption of amino acid and sugar impurities by macroporous adsorption resin is similar, and the recovery rate of sugar is too low. Depend on figure 1 It can be seen that the adsorption of amino acids by D113 resin is completed within 4.5 hours, and the adsorption capacity is poor. D001 type resin can complete the adsorption of...

Embodiment 3

[0044] Example 3: A method for detecting sugar in amino acid raw materials

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Abstract

The invention discloses a method for determining trace carbohydrate impurities in an amino acid bulk drug, and belongs to the technical field of drug analysis and detection. The method comprises the following steps: treating an amino acid bulk drug sample to be detected by ion exchange resin, adsorbing sugar in an amino acid raw material medicine, determining five carbohydrate impurities in the amino acid raw material medicine by adopting high performance liquid chromatography-evaporative light scattering detection (HPLC-ELSD), performing gradient elution by adopting polar organic phase-wateras a mobile phase, performing separation by adopting a polar bonded phase chromatographic column, and directly introducing a sample by taking nitrogen as an auxiliary gas. Verification proves that themethod can realize baseline separation of the components, and the contents of the five saccharide impurities in the amino acid bulk drug are determined by adopting an external standard method. The method is high in sensitivity, simple and convenient to operate, high in accuracy and suitable for simultaneously determining the contents of the five saccharide impurities in the amino acid bulk drug.

Description

technical field [0001] The invention relates to a method for determining trace carbohydrate impurities in amino acid raw materials, belonging to the technical field of drug analysis and detection. Background technique [0002] Amino acids are the basic units that constitute the first nutritional element in the human body - protein, and play an important role in human growth, reproduction and immunity. The production methods of amino acids mainly include extraction method, fermentation method, chemical synthesis, enzymatic method and other methods. The traditional extraction method, chemical synthesis method and enzymatic method are difficult to achieve the purpose of industrial production due to the high cost of precursors and complicated processes. At present, fermentation methods are generally used in industry. Sugar is introduced into the process as a sugar source for microorganisms in the fermentation process, and may become a trace impurity in amino acid APIs. However,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74G01N30/88G01N30/06G01N30/14G01N30/86G01N30/12G01N30/08G01N30/04G01N30/34
CPCG01N30/02G01N30/04G01N30/06G01N30/08G01N30/12G01N30/14G01N30/34G01N30/74G01N30/8634G01N30/8679G01N30/88G01N2030/047G01N2030/126G01N2030/143G01N2030/8818G01N2030/884G01N2030/8872
Inventor 惠人杰姜峰薛灵杰杨荻
Owner JIANGNAN UNIV