http://XBYZ.cbpt.cnki.netLC-MS/MS法同时测定诺氟沙星胶囊中的3种杂质曹旭1,张琤2,刘涛1,王群葆11.邢台市食品药品检验所,邢台054000;2.邢台市第五医院,邢台054000摘要:目的建立液相色谱与串联质谱联用(liquidchromatographytandemmassspectrometry,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ACQUITYUPLCBEHShieldRP18色谱柱(100mm×2.1mm,1.7μm),以乙腈-2mL·L-1甲酸为流动相进行梯度洗脱,流速为0.3mL·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(electrosprayionization,ESI),正离子模式,多反应监测(multiplereactionmonitoring,MRM)。杂质A检测离子对为m/z270.223→224.227/168.246,杂质E检测离子对为m/z336.323→318.327/247.220,杂质K检测离子对为m/z306.332→262.346/288.346,诺氟沙星检测离子对为m/z320.272→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、3.984~398.400ng·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%;12h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。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DOI:10.3969/j.issn.1004-2407.2023.05.008中图分类号:R927.2文献标志码:A文章编号:1004-2407(2023)05-0042-06Simultaneousdeterminationof3impuritiesinNorfloxacinCapsulesbyLC-MS/MSCAOXu1,ZHANGCheng2,LIUTao1,WANGQunbao11.XingtaiFoodandDrugInspectionInstitute,Xingtai054000,China;2.XingtaiCityFifthHospital,Xingtai054000,ChinaAbstract:ObjectiveToestablishanliquidchromatographytandemmassspectrometry(LC-MS/MS)methodforthesimultaneousdeterminationofimpurityA,impurityEandimpurityKinNorfloxacinCapsules.MethodsTheseparationwasperformedonanACQUITYUPLCBEHShieldRP18column(100mm×2.1mm,1.7μm).Thegradientelutionwascarriedoutwithacetoni-trile-2mL·L-1formicacidasthemobilephase,theflowratewas0.3mL·min-1,thecolumntemperaturewas40℃,andthein-jectionvolumewas0.5μL.Theanalyteswereanalyzedbyelectrosprayionization(ESI)inthemultiplereactionmonit...
