Method for measuring content of acetonedicarboxylic acid in sodium citrate solution

Abstract

The invention discloses a method for determining the content of acetonedicarboxylic acid in a sodium citrate solution. The method comprises the following steps of: 1) preparing a system applicable solution, specifically, taking a proper amount of acetonedicarboxylic acid reference substance and a proper amount of citric acid reference substance, dissolving the acetonedicarboxylic acid reference substance and the citric acid reference substanceby using a mobile phase, and diluting an obtained solution to prepare a solution containing about 100 micrograms of citric acid and 100 micrograms of acetonedicarboxylic acid per 1ml; 2) preparing a test solution, specifically, precisely measuring 2ml of a 2.5% sodium citrate solution, placing the 2.5% sodium citrate solution in a 10ml measuring flask, diluting the 2.5% sodium citrate solution to a scale by using a mobile phase, and performing uniform shaking; and 3) preparing a reference substance solution, specifically, taking a proper amount of an acetonedicarboxylic acid reference substance, dissolving the acetonedicarboxylic acid reference substance with a mobile phase, and diluting an obtained solution to prepare a solution containing about 100 microgramsof acetonedicarboxylic acid per 1ml. According to the method, the content of the acetonedicarboxylic acid in the sodium citrate solution is measured through the high performance liquid chromatography, so that main degradation products of the sodium citrate solution are controlled, the process conditions and storage conditions of the sodium citrate solution are favorably controlled, and meanwhile, the yield in the synthesis process of the acetonedicarboxylic acid can be accurately obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical pharmacy, and in particular relates to a method for determining the content of acetone dicarboxylic acid in sodium citrate solution. Background technique [0002] Acetone dicarboxylic acid is an important intermediate in organic synthesis, which can be used in the industrial synthesis of compounds such as granisetron, endortropine and coumarin, and its derivatives can be used to synthesize anti-osteoporosis drugs such as strontium ranelate . Because of their good reactivity, they have always been a research hotspot in organic synthesis. There have been a lot of research results on its synthesis method. The synthesis method of acetone dicarboxylic acid is mostly obtained by using sodium citrate as raw material and decarboxylation by concentrated sulfuric acid or hydrogen peroxide. [0003] However, the method for determining the content of acetone dicarboxylic acid is rarely mentioned. Because s...

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Problems solved by technology

[0003] However, the method for determining the content of acetone dicarboxylic acid is rarely mentioned. Because sodium citrate will be degraded to varying degrees under the conditions of oxidation, light and high temperature, the main degradation product is acetone dicarboxylic acid. The traditional method uses hydrogen Sodium oxide titration method, but the generated sodium acetone dicarboxylate is a strong base and weak acid salt, and the use of phenolphthalein indicator to judge the end point will affect the accurate judgment of the result. Therefore, it is urgent to invent a more accurate and quick method to measure acetone dicarboxylate. Carboxylic acid content

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