加校正因子的主成分自身对照法测定盐酸苯海拉明片中有关物质的含量

Correction Factor for Determination of Content of Related Substances in Diphenhydramine Hydrochloride Tablet by HPLC

目的建立加校正因子的主成分自身对照法测定盐酸苯海拉明片中有关物质的含量。方法色谱柱Agilent氰基柱(250mm×4.6mm,5μm),流动相为乙腈-水-三乙胺(50∶50∶0.5)(用冰醋酸调节pH值至6.5),检测波长为258nm,柱温25℃,进样量20μL。测定盐酸苯海拉明和二苯酮的线性方程,以斜率计算二苯酮相对于盐酸苯海拉明的校正因子,用相对保留时间确定其位置。结果二苯甲酮的相对保留时间为0.540,校正因子为0.332。3批样品中二苯酮含量分别为0.15%、0.21%和0.08%,总杂质分别为1.23%、1.89%和0.53%。结论本方法简便、准确可靠,适用于盐酸苯海拉明片中有关物质的控制。

OBJECTIVE The self contrast and correction factor method was established to determine the content of the related substances in Diphenhydramine Hydrochloride Tablet. METHODS Chromatography was carried out by reversed-phase technique on an Agilent NH2 column （250mm×4.6mm,5μm） with a mobile phase composed of acetonitrile, water and triethylamine in the ratio of （50：50：0. 5 ） （adjust with ethanoic acid to a pH of 6.5 ） ,The detection was carried out at 258nm and a column temperature of 25℃. The injection volume was 20μL. The slope of lin- ear equation was used to determine the correction factor between diphenylmethanone and Diphenhydramine Hydro- chloride. The relative retention time was used to determine the position of diphenylmethanone. RESULTS The rela- tive retention time between diphenylmethanone and Diphenhydramine Hydrochloride was 0. 540. The correction factor of diphenylmethanone was 0. 332. The content of diphenylmethanone was 0. 15% ,0. 21% and 0. 08%, respectively. The content of total impurities was 1.23%, 1.89% and 0. 53%, respectively. CONCLUSION The method is simple, accurate and reliable for analyzing the related substances in Diphenhydramine Hydrochloride Tablet.