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LC-HR-MS/MS法鉴定头孢丙烯干混悬剂中的未知杂质
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| 篇名： | LC-HR-MS/MS法鉴定头孢丙烯干混悬剂中的未知杂质 |
| TITLE： | Identification of Unknown Impurities in Cefprozil Suspension by LC-HR-MS/MS |
| 摘要： | 目的：检测头孢丙烯干混悬剂中的未知杂质，并对其进行结构鉴定。方法：采用高效液相色谱-串联高分辨质谱法检测并鉴定头孢丙烯干混悬剂中的未知杂质。色谱柱为ThermoHyPURITYTMC18，流动相为乙腈-0.013％甲酸水溶液（梯度洗脱），检测波长为230nm，流速为1.0mL/min，柱温为40℃，进样量为20μL；以电喷雾离子源行正离子全扫描，扫描范围为质荷比（m/z）100～1500，喷雾电压为3.8kV，金属毛细管温度为320℃，鞘气压力为60Arb，辅助气压力为10Arb，喷雾温度为280℃。结果：在该色谱条件下，杂质K的检测限为0.202μg/mL，精密度、重复性试验的RSD均小于4％。杂质K附近发现3个未知杂质，且互为异构体，离子保留时间为17.83～19.31min，二级母离子均为m/z436.1500[M+H]+，可能为头孢丙烯开环、脱水后的产物。结论：本方法检测出头孢丙烯干混悬剂中杂质K附近的3个未知杂质。 |
| ABSTRACT： | OBJECTIVE：To de termine unknown impurities in Cefprozil suspension ，and to identify its structure. METHODS ： LC-HR-MS/MS method was used to detect and identify unknown impurities in Cefprozil suspension. The determination was performed on Thermo HyPURITY TM C18 with mobile phase consisted of acetonitrile- 0.013％ formic acid solution （gradient elution ） at the flow rate of 1.0 mL/min. The detection wavelength was set at 230 nm，and column temperature was 40 ℃. The sample size was 20 μL. ESI+ full scanning was carried out with electrospray ion source scanning range was mass-charge ratio （m/z）100-1 500 with spray voltage of 3.8 kV，metal capillary temperature of 320 ℃，sheath gas pressure of 60 Arb，auxiliary gas pressure of 10 Arb，spray temperature of 280 ℃. RESULTS ：Under this condition ，the detection limit of impurity K was 0.202 μg/mL. RSDs of precision and reproducibility tests were both lower than 4％. Three unknown impurities were found around impurity K ，which were isomers of each other. The retention time of ions were 17.83-19.31 min，and the secondary parent ion were all m/z 436.150 0[M+ H]+，which may be the product of ring opening and dehydration of cefpropene. CONCLUSIONS ：Three unknown impurities near impurity K in Cefprozil suspension were detected by this method. |
| 期刊： | 2020年第31卷第10期 |
| 作者： | 肖颖，袁晓，林顺权 |
| AUTHORS： | XIAO Ying，YUAN Xiao，LIN Shunquan |
| 关键字： | 高效液相色谱-串联高分辨质谱法；头孢丙烯干混悬剂；杂质K；未知杂质 |
| KEYWORDS： | LC-HR-MS/MS；Determination；Cefprozil suspension ；Impurity K ；Unknown impurities |
| 阅读数： | 644 次 |
| 本月下载数： | 6 次 |
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