Method for measuring chloride ions in amino acid-N-formic anhydride

A determination method and technology of chloride ions, which are applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of expensive ion chromatography, harsh operation, and the need for organic solvents, and achieve the effects of reducing equipment weight, reducing workload, and improving body strength.

Pending Publication Date: 2021-05-07
安徽瑞达健康产业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method is harsh, requires organic solvents, and requires expensive ion chromatography

Method used

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  • Method for measuring chloride ions in amino acid-N-formic anhydride
  • Method for measuring chloride ions in amino acid-N-formic anhydride
  • Method for measuring chloride ions in amino acid-N-formic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Accurately weigh 0.165g of sodium chloride to a 1000ml measuring bottle, add an appropriate amount of water to dissolve and dilute to the mark, shake well, and use it as a stock solution; accurately measure 10ml of the stock solution to a 100ml measuring bottle, add water to dilute to the mark, and shake well to obtain ( Every 1ml is relative to the Cl) sodium chloride standard solution of 10ug.

[0037] Accurately measure NaCl standard solution (1ml, 3ml, 5ml) and stock solution (1ml, 2ml) respectively to a 25ml measuring bottle, add 5% NaOH 10ml, add nitric acid 2ml, 0.1mol / L silver nitrate 1ml, add water to volume. After standing in the dark for 0.5 hours, measure the absorbance at 440nm, and make a working curve.

[0038] Table I

[0039] Chloride ion concentration (ug / ml) Absorbance 0.4 0.018 1.2 0.049 2 0.091 4 0.172 8 0.332

Embodiment 2

[0041] Repeat Example 1 (in order to obtain the working curve of the external standard method).

[0042] The 500mg aspartic acid-NCA that accurately weighs is transferred in the round bottom flask of 100ml, adds the alkali solution of 40ml 5%NaOH (wt), 100 ℃ of heating and stirring for half an hour, after cooling to room temperature, the reaction solution is transferred to In a 100ml volumetric flask, add 15ml of concentrated nitric acid to adjust the pH to acidic, then add 5ml of 0.1NAgNO3, react at 25°C for 0.5 hours, and then add deionized water to make it volume. Measure the absorbance of the solution under the condition of 440nm, and conduct a blank test at the same time.

Embodiment 3

[0044] Repeat Example 1 (in order to obtain the working curve of the external standard method).

[0045] Accurately weighed 500mgL-aspartic acid-4-benzyl ester-N-carbonyl anhydride is transferred to a 100ml round-bottomed flask, and 40ml of 5%NaOH (wt) alkali solution is added, heated and stirred at 25°C for half an hour, and the Transfer the reaction solution to a 100ml volumetric flask, add 15ml of concentrated nitric acid to adjust the pH to acidic, then add 5ml of 0.1NAgNO3, react at 25°C for 0.5 hours, and then add deionized water to make it volume. Measure the absorbance of the solution under the condition of 440nm, and conduct a blank test at the same time.

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Abstract

The invention provides a method for measuring the content of chloride ions in amino acid-N-formic anhydride. The method comprises the following steps: directly adding a sample into an inorganic alkali aqueous solution, titrating by using silver nitrate, testing the absorbance of the treated sample, and calculating to obtain the content of chloride ions in amino acid-N-formic anhydride. The measurement method is simple, accurate and low in cost.

Description

technical field [0001] The invention relates to the technical field of determination methods of chloride ions, in particular to a determination method of chloride ions in amino acid-N-formic anhydride. Background technique [0002] Amino acid-N-formic anhydride (3-substituted oxazoline-2,5-dione, referred to as amino acid NCA, the structural formula is as follows) [0003] [0004] Many polypeptides can be degraded into amino acids that are beneficial to the human body in the body. In recent years, they have been widely used in biomedicine and biotechnology, such as tissue engineering, drug carriers, and disease treatment. The ring-opening polymerization of amino acid NCA is an important method for the synthesis of peptides, and the quality of amino acid NCA is one of the keys to the polymerization reaction. There are many ways to prepare amino acid NCA, such as using phosgene, diphosgene, triphosgene, etc., wherein the content of chloride ions is the key to the quality ...

Claims

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Application Information

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IPC IPC(8): G01N21/31
CPCG01N21/31
Inventor 陈冉冉
Owner 安徽瑞达健康产业有限公司
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