柱前衍生-高效液相色谱法测定盐酸度洛西汀原料甲醛含量

目的采用HPLC法定量检查盐酸度洛西汀原料残留的甲醛。方法盐酸度洛西汀原料中残留的甲醛与2,4-二硝基苯肼生成具有强紫外吸收的衍生物,通过HPLC检查该衍生物含量,从而检查甲醛的含量。结果甲醛衍生物检查方法的专属性,进样精密度、灵敏度、重复性、线性和准确性均符合检测要求。S/N约为10∶1时,甲醛的灵敏度为0.011%,S/N约为3∶1时,甲醛的灵敏度为0.003%;甲醛浓度在0.04~2.00μg/ml范围内,甲醛浓度与峰面积呈良好的线性关系Y=53119X+2286.6(r=0.9997);平均回收率为101.42%。色谱条件和衍生条件的耐用性均良好。结论所用方法可用于盐酸度洛西汀原料中残留的甲醛检测。

Determination of formaldehyde in duloxetine hydrochloride by HPLC with precolumn derivatization

Objective To determine formaldehyde in duloxetine hydrochloride by HPLC.Methods The residual formaldehyde in duloxetine hydrochloride and 2,4-dinitrophenylhydrazine formed a derivative with strong UV absorption.The content of the derivative was determined by HPLC,so as to check the formaldehyde content.Results The specificity,precision,sensitivity,repeatability,linearity and accuracy of the method met the requirements.When the S/N ratio was about 10∶1,the sensitivity of formaldehyde was 0.011%,and when the S/N ratio was about 3∶1,the sensitivity of formaldehyde was 0.003%;when the formaldehyde concentration was in the range of 0.04~2.00μg/ml,there was a good linear relationship between formaldehyde concentration and peak area,Y=53119 X+2286.6(r=0.9997);the average recovery was 101.42%.The durability of chromatographic conditions and derivatization conditions were good.Conclusion The method can be used for the determination of residual formaldehyde in duloxetine hydrochloride.