摘要
目的建立测定他达拉非中氯乙酸残留量的柱前衍生化高效液相色谱法。方法用2-硝基苯肼盐酸盐对样品进行衍生化,色谱柱为岛津Inertsil ODS-3柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速1.0 mL/min,检测波长392 nm。结果氯乙酸衍生物检测的专属性强,检测限20 ng/mL,定量限50 ng/mL;质量浓度在50~500 ng/mL范围内与峰面积线性关系良好(r=0.999 6);平均回收率为94.68%,RSD为3.94%(n=9)。结论经方法学验证,该方法适用于他达拉非中氯乙酸残留量的测定。
Objective To establish a pre-column derivatization HPLC method for the content determination of residual chloroacetic acid in tadalafil.Methods The samples were derivatized with 2-nitrophenylhydrazine hydrochloride.The chromatographic column was Shimadzu Inertsil ODS-3 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min and the detection wavelength was 392 nm.Results The detection of chloroacetic acid derivatives had strong specificity,the detection limit was 20 ng/mL and the quantitative limit was 50 ng/mL.The chloroacetic acid derivative showed good linear relationship with peak area in the range of 50-500 ng/mL(r=0.999 6).The average recovery was 94.68%and RSD was 3.94%(n=9).Conclusion The method is suitable for the content determination of residual chloroacetic acid in tadalafil through the methodology validation.
作者
徐然
XU Ran(Nanjing Institute for Food and Drug Control,Nanjing,Jiangsu,China 211100)
出处
《中国药业》
CAS
2019年第19期40-42,共3页
China Pharmaceuticals
