LC-HR-MS/MS法鉴定头孢丙烯干混悬剂中的未知杂质

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Thermo HyPURITYTMC18,流动相为乙腈-0.013%甲酸水溶液(梯度洗脱),检测波长为230 nm,流速为1.0 m L/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3.8 kV,金属毛细管温度为320℃,鞘气压力为60 Arb,辅助气压力为10 Arb,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17.83~19.31 min,二级母离子均为m/z 436.1500M+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。

Identification of Unknown Impurities in Cefprozil Suspension by LC-HR-MS/MS

OBJECTIVE:To determine 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 HyPURITYTMC18 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 20μL.ESI+full scanning was carried out with electrospray ion source scanning range was mass-charge ratio(m/z)100-1500 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 0.202μg/m L.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 436.1500M+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.