摘要
为了建立医药中间体醋氯芬酸叔丁酯的液相检测方法,采用色谱柱Utimate ODS-3(250mm×4.6mm,5μm),流动相:A相为磷酸盐缓冲液(0.112mg/mL磷酸水溶液,NaOH溶液调节pH值至7.0),B相为V(纯净水)∶V(乙腈)=10∶90的溶液,并采用线性梯度模式进行洗脱,流动相速度为0.9mL/min,柱温箱温度为25℃,紫外检测波长235nm。试验结果表明:检测方法的特异性结果较好;线性方程为y=1 249.85x+10.89,R~2=0.990;精密度良好,RSD为0.78%;加样回收率的平均值为100.07%;方法可重复性较好,RSD为0.69%;耐用性中各参数水平均符合标准;此法测定3批供试样品,经计算其质量分数分别为99.46%,100.22%,99.62%。该方法专属性好,线性关系良好,精密度、准确度以及耐用性测定结果均在标准规定范围内。
In this work,a RP-HPLC method was established for determining mass fraction of aceclofenac tert-butyl ester.Ultimate ODS-3 column(250 mm×4.6 mm,5μm)with a mobile phase composing of acetonitrile-water(90∶10)and phosphate buffer(0.112 mg/mL,pH=7)were applied for gradient elution.The flow velocity,column temperature and UV detector wavelength was 0.9 mL/min,25℃and 235 nm,respectively.The results showed that the RP-HPLC method had good specificity for the determination of aceclofenac tert-butyl ester.The linear regression equation was y=1249.85x+10.89(R 2=0.990)and the precision was good with a RSD value of 0.78%.The average recovery rate and the repeatable RSD was 100.07%and 0.69%,respectively.Parameters of durability were in accordance with the standard.Three batches of samples have been measured by the RP-HPLC method and the calculated contents was 99.46%,100.22%,and 99.62%,respectively,showing that this method is good for detecting the aceclofenac tert-butyl ester.
作者
侯晓蓉
肖玲琳
单伟光
HOU Xiaorong;XIAO Linglin;SHAN Weiguang(College of Pharmaceutical Science,Zhejiang University of Technology,Hangzhou 310014,China)
出处
《浙江工业大学学报》
CAS
北大核心
2021年第2期174-177,共4页
Journal of Zhejiang University of Technology
