地塞米松磷酸钠注射液中杂质Ⅰ研究

目的: 研究地塞米松磷酸钠注射液中的杂质Ⅰ。 方法: 采用液相色谱法测定地塞米松磷酸钠原料药和注射液中的有关物质;采用高效液相色谱-四极杆飞行时间质谱技术(HPLC-QTOF-MS) 考察杂质Ⅰ的产生机理;合成、制备、纯化杂质Ⅰ,并进一步采用紫外光谱、红外光谱、质谱、核磁共振技术确证杂质Ⅰ的化学结构。 结果: 杂质Ⅰ为地塞米松磷酸钠与抗氧剂亚硫酸氢钠在高温下的加成产物。 结论: 本研究结果对地塞米松磷酸钠注射液的工艺改进以及质量控制具有指导作用。

Objective: To study the impurity I in dexamethasone sodium phosphate injection. Method: The dexamethasone sodium phosphate and its injection were investigated by HPLC,and HPLC-QTOF-MS was adopted to analyze the generation mechanism of impurity I.The impurity I was synthesized,separated and purified by prep-HPLC,and its structure was identified and proved by UV,IR,MS and NMR. Results: The impurity I was the adduct of dexamethasone sodium phosphate and antioxidant sodium bisulfite under high temperature. Conclusion: The study offers guidance for the improvement of manufacturing process and the quality control of dexamethasone sodium phosphate injection.

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