【摘要】 目的建立HPLC-MS/MS方法测定酒石酸溴莫尼定滴眼液的含量。方法色谱条件:采用Atlantis T₃（2.1mm×100mm,3μm）色谱柱,柱温30℃,以乙腈-0.2%甲酸为流动相梯度洗脱,流速0.3mL·min^-1。质谱条件:EIS源,正离子检测模式,干燥气温度350℃,干燥气流速10 L·min^-1,毛细管电压4000V,溴莫尼定和内标用于定量的母离子和子离子分别为m/z 292→212.2,285.1→213.1;碎片电压分别为180V,130V,碰撞能分别为36eV,35eV。结果溴莫尼定在2～80mg·mL^-1的浓度范围内与峰面积成良好的线性关系;最低检查限为1ng·mL^-1;低、中、高3个质量浓度的质控样品日内、日间相对误差和变异系数均小于15%;提取回收率为96.9%,RSD为0.223%。结论此方法简便且灵敏度高,可用于测定酒石酸溴莫尼定滴眼液中溴莫尼定的含量。更多还原

【Abstract】 OBJECTIVE To establish a HPLC-MS/MS method for determination of brimonidine tartrate in eye drops.METHODS The HPLC parameters were set as follows:separation was achieved on Atlantis T₃（2.1 mm×100 mm,3 mm） at a temperature of 25℃.Acetonitrile and-0.2% formic acid aqueous solution were applied as the mobile phase with the flow rate at 0.3 mL·min^-1.The MS parameters were set as follows:ESI source,positive ion detection mode,dry gas temperature 350℃,dry gas flow rate 10 L·min^-1,capillary voltage 4000 V.Quantitative determination was operated in the multiple reaction monitoring（MRM） mode,with the ion transitions m/z 292→212.2 for brimonidine and m/z 285.1→213.1 for the internal standard.The fragment voltage/collision energy for brimonidine and the internal standard were 180 eV/36 V,and 130 eV/35 V,respectively.RESULTS Brimonidine showed a good linear coefficient of correlation within the range of 2-80 mg·mL^-1,with the LLOQ at 1 ng·mL^-1.The intra-and inter-day precision for dronedarone were within 15%,and that for accuracy was achieved<100±15% for three QC samples.The mean average recovery was 96.9% with RSD less than 0.223%.CONCLUSION This method is simple and sensitive,and can be used to determine the content of brimonidine in brimonidine tartrate eye drops.更多还原