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目的:利用高效液相色谱-四极杆飞行时间质谱法(HPLC-QTOF/MS)对奥替拉西钾中主要杂质进行结构推定,并且分析其来源。方法:采用Waters Sunfire C_(18)(250mm×4.6 mm,5μm)色谱柱,柱温30℃,以甲醇-10 mmol·L~(-1)乙酸铵溶液(用乙酸调节pH至4.3)(5∶95)为流动相,流速0.8 mL·min~(-1),检测波长220 nm;采用ESI离子源,正离子扫描模式。结果:通过对奥替拉西钾及其主要杂质的一级与二级高分辨质谱图进行分析,推定主要杂质的分子结构为1,3,5-三嗪-2,4-(1氢,3氢)-二酮和2-(3-氨基甲酰脲基)-2-羰基乙酸。2个主要杂质均由奥替拉西钾降解得到。结论:所建立的方法能够有效地将奥替拉西钾中的主要杂质分离检测,杂质结构的确定为药品的质量控制提供了依据。
OBJECTIVE: To characterize the major impurities in the main constituents of otolacillin by HPLC-QTOF / MS and to analyze their origin. Methods: A Waters Sunfire C_ (18) (250 mm × 4.6 mm, 5 μm) column was used. The column was heated at 30 ℃ with methanol-10 mmol·L -1 ammonium acetate solution (adjusted to pH 4.3 with acetic acid) : 95) as the mobile phase at a flow rate of 0.8 mL · min -1 with a detection wavelength of 220 nm. The ESI ion source and positive ion scan mode were used. Results: The primary and secondary high-resolution mass spectra of potassium and its major constituents of otolacillin were analyzed and the molecular structure of the major impurities was presumed to be 1,3,5-triazine-2,4- (1H, 3 hydro) -dione and 2- (3-carbamoylureido) -2-carbonylacetic acid. Two major impurities were degraded by oteracil potassium. CONCLUSION: The established method can effectively separate and detect the main impurities in the assay of the device of the device of the invention, and the determination of impurity structure provides the basis for the quality control of the product.