HPLC-DAD法测定2-氨基二苯甲酮有关物质

Determination of the related substances of 2-aminobenzophenone by HPLC-DAD

目的建立高效液相色谱-二极管阵列检测器(high performance liquid chromatography coupled with diode array detector,HPLC-DAD)法测定2-氨基二苯甲酮有关物质,并对其进行方法学验证。方法采用十八烷基硅烷键合硅胶为填充剂的色谱柱,以10mmol/L甲酸钱水溶液-乙睛(75:25)溶液为流动相A,乙睛为流动相B,梯度洗脱,2-氨基二苯甲酮、4-氨基二苯甲酮,2-碘苯胺检测波长240nm,苯硼酸检测波长230nm,进样量10μl,流速为1.5ml/min,柱温为40℃.结果上述有关物质均在1~42mg/L范围内线性关系良好,相对校正因子分别为1.0,2.3,3.0和7.8。平均回收率为102.23%~104.25%,相对标准偏差(relative standard deviation,RSD)为2.4%~4.8%。结论本法适用于2-氨基二苯甲酮有关物质的测定。

Objective To establish a high performance liquid chromatography coupled with diode array detector(HPLC-DAD)method for the determination of the related substances in 2-aminobenzophenone.Methods The octadecylsilane bonded silica gel was used as the column.The column was eluted at a gradient mode using 10 mmol/L ammonium formate aqueous solution-acetonitrile(75:25)(mobile phase A)and acetonitrile(mobile phase B)as mobile phase,and the flow rate was 1.5 nil/min.The detection wavelength of 2-aminobenzophenone,4-aminobenzophenone and 2-iodoaniline was set at 240 nm while the detection wavelength of benzene boric acid was 230 nm.The injection volume was 10μl and the column temperature was remained at 40℃.Results The results showed that the linear range of 2-aminobenzophenone,4-aminobenzophenone,2-iodoaniline and benzene boric acid was good in the range of 1-42μg/ml,and the relative correction factors of them were 1.0,2.3,3.0 and 7.8,respectively.The average recoveries of those compounds were in the ranges of 102.23%-104.25%and the values of RSD were in the ranges of 2.4%-4.8%.Conclusions The established method is suitable for the determination of the related substances of 2-aminobenzophenone.