Method for detecting content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate

A technology of methyl propionate methylsulfate and trimethylhydrazine, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, so as to achieve strong specificity and separation ability High effect with low sample consumption

Inactive Publication Date: 2014-11-19
DONGLI NANTONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are few reports on the detection method of 3-(2,2,2-trimethylhydrazine) methyl propionate methyl sulfate content, therefore, develop a k

Method used

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  • Method for detecting content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate
  • Method for detecting content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate
  • Method for detecting content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate

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Embodiment 1

[0018] 1. Sodium hydroxide test solution

[0019] Take a certain amount of sodium hydroxide, add water to dissolve to 100mL.

[0020] 2. Sulfuric acid titration solution (0.01mol / L)

[0021] Preparation: Take 3mL of sulfuric acid, slowly pour it into an appropriate amount of water, cool to room temperature, add water to dilute to 1000mL, and shake well.

[0022] Calibration: Take about 0.15g of standard anhydrous sodium carbonate dried at 270-300°C to constant weight, accurately weigh it, add 50mL of water to dissolve, add 10 drops of methyl red-bromocresol green mixed indicator solution, and titrate with this solution When the solution turns from green to purple, boil for 2 minutes, cool to room temperature, and continue titration until the solution turns from green to dark purple. Every 1mL of sulfuric acid titrant (0.05mol / L) is equivalent to 5.30mg of anhydrous sodium carbonate. Calculate the concentration of this solution based on the consumption of this solution and t...

Embodiment 2

[0030] Precision weighing C 7 h 17 N 2 o 2 SO 4 - CH 3 Put about 0.10g of the sample in a Kjeldahl flask, add 30ml of water to dissolve it, add 100ml of sodium hydroxide test solution, heat and distill, and introduce the distillate into 50ml of 2% boric acid solution, and stop the distillation when the volume reaches about 130ml. Add 4 drops of methyl red-bromocresol green mixed indicator solution, and titrate with sulfuric acid titration solution (0.0101mol / L) until the solution changes from blue-green to gray-purple as the end point, and the titration result is corrected with a blank test. Every 1ml of sulfuric acid titrant (0.01mol / L) is equivalent to 5.436mg of C 7 h 17 N 2 o 2 SO 4 - CH 3 .

[0031] Neutralization titration (Kjeldahl method) and high performance liquid chromatography of the present invention C 7 h 17 N 2 o 2 SO 4 - CH 3 The measurement results are shown in Table 2.

[0032] Table 2 sample determination data

[0033]

[0034] High ...

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Abstract

The invention provides an analytical method for measuring the content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate by use of nonaqueous titration, and relates to an analytical method for measuring the content of a mildronate crude drug intermediate. The analytical method is characterized in that kjeldahl determination is adopted and nitrogen in a C7H17N2O2SO4-CH3 monomer is measured by use of a neutral titration method after digestion, and therefore, the purpose of measuring the main content of the intermediate can be achieved. The analytical method comprises the following specific measurement steps: putting a test sample into a Kjeldahl flask, adding water for dissolving, adding a sodium hydroxide test solution, heating for distillation, guiding the distillate into a boric acid solution, taking methyl red-bromocresol green as an indicating liquid, titrating by use of an inorganic acid titrant until the terminal point that the solution turns to grey purple from blue-green, and then calculating the content of C7H17N2O2SO4-CH3 according to the dosage of the titrant. The detection result obtained by the method is capable of achieving basically consistent effects with an HPLC (High Performance Liquid Chromatography) detection result. The method is simple and quick, precise in measurement result and high in accuracy, and can be applied to conventional analysis and quality control of the mildronate crude drug intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate.

Description

technical field [0001] The invention discloses a method for detecting the content of meldonium intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methyl sulfate, and relates to the technical field of quality control of meldonium raw material drug intermediates. Background technique [0002] Meldonium (also known as THP, MET-88 and mildronate) is a new type of cardioprotective drug, which is a structural analog of carnitine, and its chemical name is 3-(2,2,2-trimethylhydrazine) propionate dihydrate. [0003] Various methods are known for the preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate, wherein 3-(2,2,2-trimethylhydrazine)propionate methyl Sulfate is an important intermediate for the preparation of Meldonium, and then hydrolyzed and deionized, and then crystallized in ethanol to obtain Meldonium. [0004] The described method of Meldonium intermediate usually comprises: 1,1-dimethylhydrazine reacts with methyl acrylate to form 3-(2,2-dimethylhydr...

Claims

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Application Information

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IPC IPC(8): G01N21/78
Inventor 阿依别克·马力克阿拉法特·阿依别克衣伟男
Owner DONGLI NANTONG CHEM
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