LC-MS/MS法同时测定诺氟沙星胶囊中的3种杂质  

Simultaneous determination of 3 impurities in Norfloxacin Capsules by LC-MS/MS

作　　者：曹旭 张琤 刘涛 王群葆 CAO Xu;ZHANG Cheng;LIU Tao;WANG Qunbao(Xingtai Food and Drug Inspection Institute,Xingtai 054000,China;Xingtai City Fifth Hospital,Xingtai 054000,China)

机构地区：[1]邢台市食品药品检验所,邢台054000 [2]邢台市第五医院,邢台054000

出　　处：《西北药学杂志》2023年第5期42-47,共6页Northwest Pharmaceutical Journal

基　　金：河北省市场监督管理局科研计划项目(编号:2020ZC49)。

摘　　要：目的建立液相色谱与串联质谱联用(liquid chromatography tandem mass spectrometry,LC-MS/MS)法同时测定诺氟沙星胶囊中杂质A、杂质E、杂质K。方法用ACQUITY UPLC BEH Shield RP18色谱柱(100 mm×2.1 mm,1.7μm),以乙腈-2 mL·L^(-1)甲酸为流动相进行梯度洗脱,流速为0.3 mL·min^(-1),柱温为40℃,进样量为0.5μL;质谱离子化方式为电喷雾电离(electrospray ionization,ESI),正离子模式,多反应监测(multiple reaction monitoring,MRM)。杂质A检测离子对为m/z 270.223→224.227/168.246,杂质E检测离子对为m/z 336.323→318.327/247.220,杂质K检测离子对为m/z 306.332→262.346/288.346,诺氟沙星检测离子对为m/z 320.272→276.356/302.351。结果杂质A、杂质E和杂质K质量浓度分别在4.108~410.780、4.120~412.000、3.984~398.400 ng·mL^(-1)范围内与其峰面积线性关系良好,相关系数r分别为0.9994、0.9984、0.9987;精密度实验,上述3个杂质峰面积的RSD值均小于3%;12 h稳定性实验,杂质A、杂质E和杂质K峰面积的RSD值均小于6%,杂质A、杂质E和杂质K的平均回收率(n=9)分别为105.55%、102.44%、106.75%,RSD值均小于10%。结论该方法可同时测定诺氟沙星胶囊中杂质A、杂质E、杂质K。Objective To establish an liquid chromatography tandem mass spectrometry(LC-MS/MS)method for the simultaneous determination of impurity A,impurity E and impurity K in Norfloxacin Capsules.Methods The separation was performed on an ACQUITY UPLC BEH Shield RP18 column(100 mm×2.1 mm,1.7μm).The gradient elution was carried out with acetonitrile-2 mL·L^(-1)formic acid as the mobile phase,the flow rate was 0.3 mL·min^(-1),the column temperature was 40℃,and the injection volume was 0.5μL.The analytes were analyzed by electrospray ionization(ESI)in the multiple reaction monitoring(NMR)positive ion mode.The optimized mass ion-pairs for quantitation were impurity A m/z 270.223→224.227/168.246,impurity E m/z 336.323→318.327/247.220,impurity K m/z 306.332→262.346/288.346,norfloxacin m/z 320.272→276.356/302.351.Results The linearity ranges of impurity A,impurity E and impurity K were 4.11-410.78 ng·mL^(-1)(r=0.9994),4.12-412.00 ng·mL^(-1)(r=0.9984)and 3.98-398.40 ng·mL^(-1)(r=0.9987),have a good linear relationship with their peak areas,respectively.In the precision test,the RSDs of the above 3 impurity peak areas were less than 3%.In the 12 hours stability test,the RSDs of the peak areas of impurity A,impurity E and impurity K were less than 6%,and the average recoveries of impurity A,impurity E and impurity K(n=9)were 105.55%,102.44%and 106.75%respectively,and the RSDs were less than 10%.Conclusion This method is suitable for the determination of impurity A,impurity E and impurity K in Norfloxacin Capsules.

关 键 词：诺氟沙星 诺氟沙星胶囊 氟喹诺酮药物杂质 质量控制 

分 类 号：R927.2[医药卫生—药学]