摘要
目的建立反相高效液相色谱法(RP-HPLC)测定盐酸莫西沙星原料药中醋酸的残留量。方法采用Welch Xtimate C18色谱柱(4.6 mm×150 mm,5μm),以0.07%磷酸(氢氧化钠调pH至2.50,水相)-乙腈(有机相)为流动相,梯度洗脱,流速1.0 mL·min-1,柱温30℃,紫外检测器,检测波长210 nm,进样量10μL。结果空白、供试品溶液中无杂峰干扰醋酸检测;醋酸定量限(LOQ)为1.36μg·mL-1,检测限(LOD)为0.51μg·mL-1;在1.36~125.47μg·mL-1与峰面积线性关系良好,线性方程y=0.3302x-0.0429(r=1.000,n=6);醋酸低、中、高3个浓度水平的加样回收率分别为95.1%、95.8%、96.3%(n=3);醋酸的稳定性、重复性和精密度试验均符合要求。结论该方法简单、方便,准确性、重复性及稳定性均良好,适用于测定盐酸莫西沙星原料药中醋酸残留量。
Objective To determine residual organic solvents of acetic acid in moxifloxacin hydrochloride raw materials by RP-HPLC.Methods The determination was performed on Welch Xtimate C18(4.6 mm×150 mm,5μm)column.The 0.07%phosphoric acid(pH adjusted to 2.50 with sodium hydroxide)-acetonitrile was used as the mobile phase with gradient elution.The flow rate was 1.0 mL·min-1,the column temperature was 30℃,the detection wavelength was 210 nm at UV detector,and the injection volume was 10μL.Results The limit of quantitation of acetic acid was 1.36μg·mL-1,and the limit of detection was 0.51μg·mL-1.The linear range was 1.36-125.47μg·mL-1,y=0.3302x-0.0429(r=1.000,n=6).The recoveries(n=3)of low,medium and high levels of acetic acid were 95.1%,95.8%,and 96.3%.Stability,repeatability and precision tests all met the requirements.Conclusion The established method is easy and convenient,accurate,stable and repeatable,and can be used for determination of residual organic solvents of acetic acid in moxifloxacin hydrochloride raw materials.
作者
罗小妹
赵树军
朱银飞
茅仁刚
LUO Xiao-mei;ZHAO Shu-jun;ZHU Yin-fei;MAO Ren-gang(Shanxi Qianyuan Pharmaceutical Group Corporation Limited,Shanghai 200120)
出处
《中南药学》
CAS
2020年第1期124-127,共4页
Central South Pharmacy
