摘要
环丙沙星中有关物质的残留水平应控制在标准规定的限度范围内,以保证其质量安全有效。建立了一种超高效液相色谱-串联三重四极杆质谱法同时测定环丙沙星中5种有关物质(杂质A、B、C、E、H)含量的分析方法。样品以乙腈超声提取,经0.22μm有机滤膜过滤,UPLC-MS/MS检测,采用Waters ACQUITY BEH C18(2.1 mm×100 mm,1.7μm)高性能通用性液相色谱柱分离,以水相为含0.1%甲酸-2 mmol/L乙酸铵的水溶液与有机相为含0.1%甲酸的乙腈溶液进行梯度洗脱,柱温:30℃,进样量:2μL,流速:0.2 mL/min,采用Agilent喷射流电喷雾电离离子源,正离子下以多反应监测模式采集,外标法定量。结果显示,5种有关物质在各自范围内线性关系良好,线性相关系数R 2均大于0.99,重复性的相对标准偏差≤5%,检出限和定量限分别为0.058~0.42和0.19~1.30 ng/mL,3个水平加标回收率为71.3%~118.8%,相对标准偏差为1.0%~7.5%,6批样品中均检出有关物质,含量均符合2020年版《中国药典》限量要求。该方法前处理操作简单、准确灵敏、重复性和稳定性良好,可用于环丙沙星中有关物质的质量控制。
To ensure the quality,safety,and efficacy of ciprofloxacin,the residual levels of relevant substances must be controlled within the limits specified by the regulatory standards.This study developed a method for simultaneous determination of 5 related substances(impurity A,B,C,E,and H)in ciprofloxacin using ultra-high performance liquid chromatography coupled with tandem triple quadrupole mass spectrometry.The samples were extracted by ultrasonic acetonitrile,filtered through a 0.22μm organic filter membrane,and analyzed by UPLC-MS/MS.Separation were performed by Waters ACQUITY BEH C18 column(2.1 mm×100 mm,1.7μm),with a mobile phase of 0.1%formic acid and 2 mmol/L ammonium of aqueous solution(aqueous phase)and 0.1% formic acid of acetonitrile(organic phase)using gradient elution.The column temperature was set at 30℃,the injection volume was 2μL and the flow rate was 0.2 mL/min.Detection was carried out using an Agilent jet current electrospray ionization source in positive ion mode with multiple reaction monitoring mode,and quantification was performed using an external standard method.The five related substances exhibited good linearity over their respective concentration ranges,with correlation coefficients R 2 above 0.99.The method also showed good repeatability,with relative standard deviations(RSDs)not exceeding 5%.The detection limits and quantification were 0.058~0.42 ng/mL and 0.19~1.30 ng/mL,respectively.The spiked recoveries rates at the three spiked levels were 71.3%~118.8%,with RSDs of 1.0%~7.5%.All six batches of samples tested positive for related substances,with contents meets the limit requirement of the 2020 edition of Chinese Pharmacopoeia.This method features simple sample preparation,high sensitivity,good repeatability and stability,and is suitable for quality control of related substances in ciprofloxacin.
作者
许晓辉
李坚
吴福祥
杜锐浒
张晓萍
张生萍
王小乔
XU Xiao-hui;LI Jian;WU Fu-xiang;DU Rui-hu;ZHANG Xiao-ping;ZHANG Sheng-ping;WANG Xiao-qiao(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China)
出处
《化学试剂》
2025年第9期89-95,共7页
Chemical Reagents
基金
甘肃省药品监督管理局科学技术类项目(2024GSMPA051)。
关键词
超高效液相色谱-质谱法
环丙沙星
有关物质
含量
测定
质量控制
ultra high performance liquid chromatography-mass spectrometry
ciprofloxacin
related substances
content
determination
quality control
