Method for detecting dexamethasone in reaction liquid in esterification stage in production process of dexamethasone sodium phosphate

Abstract

The invention belongs to the technical field of detection methods, and particularly relates to a method for detecting dexamethasone in a reaction liquid in an esterification stage in a production process of dexamethasone sodium phosphate. The method comprises the following steps: (1) preparing a system applicability solution; (2) preparing a test solution: taking 0.2 ml of dexamethasone phosphate esterification reaction liquid, adding 0.1 ml of concentrated hydrochloric acid and 1ml of water, uniformly shaking, adding a mobile phase, diluting to 10ml, and uniformly mixing to obtain the test solution; (3) taking 10ml of a blank solution as the mobile phase; and (4) detecting the dexamethasone phosphate in the test solution by adopting high performance liquid chromatography; The preparation process of the mobile phase comprises the following step: uniformly mixing 45ml of a triethylamine solution, 47.5 ml of methanol and 7.5 ml of acetonitrile to obtain the mobile phase. The method provided by the invention can effectively detect whether the material dexamethasone is completely reacted in the esterification reaction of dexamethasone sodium phosphate, controls the content of impurity dexamethasone in the product, and improves a yield.

Description

technical field [0001] The invention belongs to the technical field of detection methods, and in particular relates to a detection method of dexamethasone in a reaction liquid in an esterification stage in the production process of dexamethasone sodium phosphate. Background technique [0002] Dexamethasone sodium phosphate products belong to the adrenal cortex hormone drugs, and the dexamethasone phosphate reaction solution is an intermediate control product of dexamethasone sodium phosphate. For the reaction process, see Figure 19 However, due to the large difference in solubility between the dexamethasone phosphate reaction solution and pure dexamethasone, it is difficult to use the detection method of pure dexamethasone, and there is no public detection standard for dexamethasone phosphate reaction solution and Detection method, in view of the above situation, we disclose the detection standard and detection method of dexamethasone sodium phosphate reaction solution, so t...

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Problems solved by technology

[0002] Dexamethasone sodium phosphate products belong to the adrenal cortex hormone drugs, and the dexamethasone phosphate reaction solution is an intermediate control product of dexamethasone sodium phosphate. For the reaction process, see Figure 19 However, due to the large difference in solubility between the dexamethasone phosphate reaction solution and pure dexamethasone, it is difficult to use the detection method of pure dexamethasone, and there is no public detection standard for dexamethasone phosphate reaction solution and Detection method, in view of the above situation, we disclose the detection standard and detection method of dexamethasone sodium phosphate reaction solution, so that better control can be obtained in the process of producing dexamethasone sodium phosphate, thereby improving the product quality of dexamethasone sodium phosphate

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