摘要
建立了同时测定药用复合包装袋中8种水溶性杂质的高效液相色谱-串联质谱法(HPLC-MS/MS)。将药用复合包装袋剪碎,采用超纯水在50℃条件下超声提取30 min。提取液经0.22μm聚四氟乙烯(PTFE)微孔滤膜过滤后,以甲醇-0.1%甲酸为流动相进行梯度洗脱,经ZORBAX Eclipse XDB-C_(18)(3.5μm,4.6 mm×150.0 mm)色谱柱分离,在ESI源正离子模式下进行多反应监测(MRM)扫描,采用外标法定量。对色谱柱、流动相和质谱参数进行优化,并对基质效应进行评价。结果表明:最优条件下的检出限(LOD)为0.20~0.35 ng/g,线性相关系数均高于0.995,平均加标回收率为85.0%~115.8%,相对标准偏差(RSD)为0.3%~9.2%(n=6)。该方法前处理简单,分析时间短至6 min,无明显基质效应,可用于药用复合包装袋中8种水溶性杂质的快速筛查。
A method for determining eight water-soluble impurities in medicinal composite packaging bag by HPLC-MS/MS simultaneously was established.The medicinal composite packaging bag was cut into small pieces and then extracted by ultrapure water with ultrasonic wave at 50℃for 30 min,followed by clean-up through a 0.22μm polytetrafluoroethylene(PTFE)membrane.The separation was conducted on ZORBAX Eclipse XDB-C_(18)(3.5μm,4.6 mm×150.0 mm)with methanol-0.1%formic acid as mobile phase.The target compounds were detected under electrospray ionization(ESI)positive ion multiple reactive monitoring(MRM)mode,and quantified by external standard method.The chromatographic column,mobile phase and mass spectrum parameters were optimized,and the matrix effect was assessed.The results showed that the limits of determination(LOD)were 0.20~0.35 ng/g,the linear correlation coefficients were all higher than 0.995,the average recoveries were 85.0%~115.8%,and the RSD were 0.3%~9.2%(n=6)under the optimized conditions.The method exhibited the advantages of simple pretreatment,short analysis time(6 min)and slight matrix effect,which can be used for the rapid screening of eight water-soluble impurities in medicinal composite packaging bag.
作者
余秋玲
张云冉
邱月
龙梅
杨倩
陆嘉莉
YU Qiuing;ZHANG Yunran;QIU Yue;LONG Mei;YANG Qian;LU Jiai(Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123,China)
出处
《塑料科技》
北大核心
2025年第1期126-130,共5页
Plastics Science and Technology
基金
重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001)
重庆市市场监督管理局科研计划项目(CQSJKJ2022040)。
