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Method for measuring industrial-grade aminopyrimidine content

A technology of aminopyrimidine and determination method, which is applied in the field of determination of industrial-grade aminopyrimidine content, can solve problems such as product quality and process control risks, and achieve the effect of saving labor costs and improving product quality

Inactive Publication Date: 2014-11-19
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thiothiamine oxidation process is the CCP (critical control point) of the vitamin B1 synthesis process. The original process of the solution after thiothiamine oxidation with hydrogen peroxide did not establish quality indicators to control the quality of the oxidizing solution. It just judged the appearance and went straight down. circulation, it is easy to bring risks to product quality and process control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 22g of the pyrimidine sample, place the pyrimidine sample in the first container tank with a volume of 750mL, add 200mL of pure methanol, connect the first container tank to the reflux device, heat to 62°C while stirring, and reflux for 0.8 hours , filtered while it was hot, and heated while adding 1.1g of activated carbon in the filtrate, then refluxed for 0.4 hours, after decolorization 4 times, cooled the filtrate to crystallize and filter, put the filtrate into an oven and dry to constant weight to obtain pyrimidine essence Product; Weigh 18g of the pyrimidine refined product into a second container tank with a volume of 150mL, add mobile phase to dissolve and dilute to the scale, then inject the sample, and record the chromatogram for five parallel injections, and normalize by area The results were calculated by the method and averaged to obtain the refined product of pyrimidine.

[0031] Weigh the pyrimidine refined product into the second container tank, ad...

Embodiment 2

[0034] Weigh 22g of the pyrimidine sample, place the pyrimidine sample in the first container tank with a volume of 750mL, add 200mL of pure methanol, connect the first container tank to the reflux device, heat to 65°C while stirring, and reflux for 0.9 hours , filtered while it was hot, and heated while adding 1.1g of activated carbon in the filtrate, and then refluxed for 0.8 hours. After decolorization for 5 times, the filtrate was cooled and crystallized and filtered, and the filtrate was dried in an oven to constant weight to obtain pyrimidine essence. Product; Weigh 18g of the pyrimidine refined product into a second container tank with a volume of 150mL, add mobile phase to dissolve and dilute to the scale, then inject the sample, and record the chromatogram for five parallel injections, and normalize by area The results were calculated by the method and averaged to obtain the refined product of pyrimidine.

[0035] Weigh the pyrimidine refined product into the second c...

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Abstract

The invention discloses a method for measuring industrial-grade aminopyrimidine content. The method comprises the following steps: putting a pyrimidine sample into a first container, adding pure methanol, connecting the first container with a reflux device, heating to 62 to 65 DEG C while stirring, carrying out reflux for 0.8 to 0.9 hour, filtering while the solution is hot, heating the filtrate while adding activated carbon to the filtrate, next, carrying out reflux for 0.4-0.8 hour, after the filtrate is decolored, cooling and crystalizing the filtrate and then filtering the filtrate, and drying the filtered-out material in a drying oven until reaching constant weight, thereby obtaining refined pyrimidine; weighing the refined pyrimidine and putting the refined pyrimidine into a second container, adding a moving phase to the refined pyrimidine so that the refined pyrimidine can be dissolved and diluted to a scale mark, next, injecting the sample for a plurality of times in parallel and recording a chromatogram, calculating results by use of an area normalization method, and averaging the results, thereby obtaining the mass of the refined pyrimidine; weighing the mass of the aminopyrimidine in the sample; calculating the content of the obtained aminopyrimidine by use of a formula. The method for measuring the industrial-grade aminopyrimidine content is capable of well guaranteeing process monitoring and quality control, and improving the product quality.

Description

technical field [0001] The invention relates to the technical field of vitamin production, in particular to a method for determining the content of industrial-grade aminopyrimidine. Background technique [0002] The synthesis of vitamin B1 at home and abroad mainly reflects the synthesis of the intermediate 2-methyl-4-amino-5-(aminomethyl)pyrimidine. Acyl pyrimidine route and malononitrile route. Among them, the route of acrylonitrile formyl pyrimidine synthesis of vitamin B1 mainly includes the steps of aminopropionitrile, sodium substitution, enamine, pyrimidine, chlorate, diethyl ether hydrochloride, thiothiamine, thiamine nitrate and thiamine hydrochloride. The thiothiamine oxidation process is the CCP (critical control point) of the vitamin B1 synthesis process. The original process of the solution after thiothiamine oxidation with hydrogen peroxide did not establish quality indicators to control the quality of the oxidizing solution. It just judged the appearance and ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 沈银元李来成陈英明崔胜凯
Owner 江苏兄弟维生素有限公司