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奥拉西坦胶囊中主要未知杂质的鉴定及其含量测定
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| 篇名： | 奥拉西坦胶囊中主要未知杂质的鉴定及其含量测定 |
| TITLE： | Identification and Content Determination of Main Unknown Impurity in Oxiracetam Capsule |
| 摘要： | 目的：鉴定奥拉西坦胶囊中的主要未知杂质并测定其含量，进而提高该制剂的质量控制标准。方法：采用超高效二维液相色谱-离子阱-飞行时间质谱法对该未知杂质进行定性分析。一维液相色谱分析采用STPAKC18ES柱，流动相为0.02mol/L磷酸二氢钠溶液，流速为0.5mL/min，柱温为30℃，进样量为20μL，检测波长为210nm；二维液相色谱分析采用TechmateC18-STⅡ柱，流动相为0.02mol/L醋酸铵溶液，流速为0.5mL/min，柱温为30℃，并采用质谱检测（电喷雾离子源，正、负离子模式数据采集）。通过一维液相色谱对目标杂质成分进行定位后，转入二维液相色谱-质谱系统进行定性分析。采用色谱工作站中的分子式预测模块“AccurateMassCalculator”对该未知杂质结构进行推断；经制备纯化获得杂质精制品，并进行标化和结构确证。采用高效液相色谱法对该杂质含量进行测定（同定性分析的一维色谱条件）。结果：奥拉西坦胶囊中的主要未知杂质为奥拉西坦酸；经制备纯化后获得的杂质精制品含量为99.5％。9批奥拉西坦胶囊中奥拉西坦酸的含量为0.05％～0.14％。结论：所建立的超高效二维液相色谱-离子阱-飞行时间质谱法能准确定位杂质奥拉西坦酸的出峰位置并对其进行结构分析，且相应的含量测定方法能较好地分离杂质与主药及其他成分，灵敏度、精密度、重复性、稳定性、准确度均良好，可较好地控制奥拉西坦胶囊的成品质量。 |
| ABSTRACT： | OBJECTIVE：To identify the main unknow impurity of Oxiracetam capsule and determine its content ，so as to improve the standard of quality control. METHODS ：Two-dimensional UPLC -IT-TOF-MS was adopted to qualitatively analyze the unknown impurity. One-dimensional liquid chromatogram analysis was performed on ST PAK C 18 ES column with mobile phase consisted of 0.02 mol/L sodium dihydrogen phosphate solution at the flow rate of 0.5 mL/min. The column temperature was set at 30 ℃，sample size was 20 μL. The detection wavelength was set at 210 nm. Two-dimensional liquid chromatogram analysis was performed on Techmate C 18-STⅡ column with mobile phase consisted of 0.02 mol/L ammonium acetate solution at the flow rate of 0.5 mL/min. The column temperature was 30 ℃. Mass spectrometry was adopted （electropray ionization source ，MS+ and MS － mode data acquisition ）. After the target impurity was located by one-dimensional liquid chromatography ，it was transferred to two-dimensional liquid chromatography-mass spectrometry system for qualitative analysis. The unknown impurity structure was inferred by means of molecular formula prediction module “Accurate Mass Calculator ”in LCMS Solution ，and the refined impurity products by preparation and purification were standardized and confirmed . The impurity content was determined by HPLC （with the same condition of one-dimensional liquid chromatography for qualitative analysis ）. RESULTS ：The main unknown impurity in Oxiracetam capsules is oxiracetam acid. The content of the refined product was 99.5％ after preparation and purification. The contents of oxiracetam acid in 9 batches of Oxiracetam capsules were 0.05％ -0.14％ . CONCLUSIONS ：The established two-dementional UPLC-IT-TOF-MS method can accurately locate the peak position of the impurity oxiracetam acid ，and analyze its structure，while the corresponding content determination method can better separate the impurity from the main drug and other components，with good sensitivity ，precision，repeatability，stability and accuracy. The quality of the finished product of Oxiracetam capsules can be well controlled by using above method . |
| 期刊： | 2020年第31卷第06期 |
| 作者： | 张菁，孙婷，赵昌梦，姜建国 |
| AUTHORS： | ZHANG Jing，SUN Ting，ZHAO Changmeng，JIANG Jianguo |
| 关键字： | 超高效二维液相色谱-离子阱-飞行时间质谱法；高效液相色谱法；奥拉西坦胶囊；奥拉西坦酸；杂质；鉴定；含量测定 |
| KEYWORDS： | Two-dementional UPLC-IT-TOF-MS；HPLC；Oxiracetam capsule ；Oxiracetam acid ；Impurity；Identification； |
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