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Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration

A technology of hydroxypyrimidine and sulfate, which is applied in the field of sample purity of 2,4,5-triamino-6-hydroxypyrimidine sulfate, and can solve problems such as no analytical methods reported in literature, lack of analytical methods, difficult product quality, etc. , to achieve the effect of simple operation, low cost, high accuracy and precision

Inactive Publication Date: 2011-08-03
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002]2,4,5-Triamino-6-hydroxypyrimidine sulfate is a synthetic broad-spectrum antiviral drug acyclovir and anti-anemia drug folic acid ( folic acid), but the analysis method of its samples has not been reported in the literature
At present, a small number of enterprises in China have begun to synthesize the intermediate, but due to the lack of a unified analysis method, it is difficult to monitor the quality of the product

Method used

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  • Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration
  • Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration
  • Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1. Preparation of 0.5mol / L HCl aqueous solution

[0050] Use a graduated cylinder to measure 12 mL of concentrated HCl, dissolve it in 250 mL of distilled water, and prepare an aqueous HCl solution of about 0.5 mol / L, to be calibrated.

[0051] 2. Calibration of 0.5mol / L HCl aqueous solution

[0052] (1) Blank test

[0053] Using an acidity meter calibrated on site, measure the pH value of the distilled water used to prepare the solution, and record it as pH 空白 , and serve as the end point of the titration.

[0054] (2) Calibration of the concentration of HCl aqueous solution

[0055] Accurately weigh about 0.5 g of anhydrous Na 2 CO 3 , denoted as W NaCO3 , placed in a 250mL beaker, add 100mL of distilled water whose pH value has been measured, and ultrasonically dissolve. Titrate with the prepared aqueous HCl solution to pH 空白 As the titration endpoint, record V 滴定 (Unit: mL), calculate the concentration C of the HCl aqueous solution according to the followin...

Embodiment 2

[0076] Only change the calibration part of HCl standard solution and NaOH standard solution to use commonly used acid-base indicators (such as methyl orange and phenolphthalein) to indicate the titration end point, and the rest of the parts are the same as in Example 1. The sample purity of 2,4,5-triamino-6-hydroxypyrimidine sulfate purchased in this example was determined by this method to be 93.56%, and the relative average deviation was 0.27%.

Embodiment 3

[0078] Change the calibration part of HCl standard solution and NaOH standard solution to use commonly used acid-base indicators (such as methyl orange and phenolphthalein) to indicate the titration end point, and change the calibration of 2,4,5-triamino-6-hydroxypyrimidine sulfate to The titration endpoint indication of the sample and sample is changed from acidity meter indication to bromocresol green sodium (1g / L aqueous solution): chlorophenol red sodium (1g / L aqueous solution) = 1:1 mixed acid-base indicator indication, the color of the end point Change from yellow-green to blue-green. The sample purity of 2,4,5-triamino-6-hydroxypyrimidine sulfate purchased in this example was determined by this method to be 93.59%, and the relative average deviation was 0.52%.

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Abstract

The invention discloses a method for analyzing the purity of a 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration, and the method belongs to the field of medical intermediate analysis. The quantitative analysis of products is carried out by adopting a method of converting sulfate into hydrochloride which is easily dissolved into water and titrating the total acidity in a solution through strong base. The destination of a titration reaction is indicated through an acid-base indicator or an acidometer, and the recovery rate and precision tests of the method verify that the analysis result of the method is accurate and reliable. The method disclosed by the invention has the advantages of mature method, low cost and simplicity and convenience in operation because an acid base titration analysis method is adopted. The accuracy and precision of the method are high by adopting a macro analysis method.

Description

technical field [0001] The present invention relates to a method for the purity of a 2,4,5-triamino-6-hydroxypyrimidine sulfate sample, specifically a method for analyzing the purity of a 2,4,5-triamino-6-hydroxypyrimidine sulfate sample using a titration method , belonging to the field of analysis of pharmaceutical intermediates. Background technique [0002] 2,4,5-triamino-6-hydroxypyrimidine sulfate is an important intermediate in the synthesis of broad-spectrum antiviral drug acyclovir and anti-anemia drug folic acid, but the analysis of its samples has been The method has not been reported in the literature. At present, a small number of enterprises in China have begun to synthesize the intermediate, but due to the lack of a unified analysis method, it is difficult to monitor the quality of the product. Contents of the invention [0003] The purpose of the present invention is to provide a method for analyzing the purity of 2,4,5-triamino-6-hydroxypyrimidine sulfate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 郭建宇
Owner SHANGHAI NORMAL UNIVERSITY
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