反相高效液相色谱法测定聚甲酚磺醛溶液中三组分含量

Determination the Contents of Three Components in Policresulen Solution Using Reversed-Phase High Performance Liquid Chromatography

目的 建立聚甲酚磺醛溶液的反相高效液相色谱分析方法 ;方法 以ODS柱 ,1%NH4Ac 甲醇 (85∶15 )为流动相 ,于2 6 5nm测定m 甲酚 4 磺酸 (M 4A)和m 甲酚 6 磺酸 (M 6A) ;1%NH4Ac 甲醇 (5 5∶4 5 )为流动相 ,于 2 80nm测定聚甲酚磺醛 (PCS)的含量。结果 精密度RSD <0 .94 % ,在 13h内三种对照品均稳定 (RSD <0 .4 6 % ,检测限 <2 .3mg·L-1,回收率在 99.4 %～10 0 .0 %之间。结论 该法简便、快速、准确 ,可用于控制聚甲酚磺醛溶液的质量。

Aim A reversed phase high performance liquid chromatographic method was developed for the quantitative determinations of benzenesulfonic acid,hydroxymethyl ,4 hydroxy 2 methy,benzenesulfonic acid,hydroxymethyl ,2 hydroxy 4 methyl and policresulen in the policresulen solution.Methods The operation was carried out in the ODS column with the mobile phase consisting of a mixture of 1%NH 4Ac Methanol(85∶15,v/v), in which the flow rate of 1.0ml/min and UV detection wavelength at 265nm were set to determine the contents of the former two components.The third component was determined with mobile phase of 1%NH 4Ac Methanol(55∶45 v/v),the flow rate of 0.9ml/min and UV detection at 280nm (temperature at 22℃).20μl were injected into the chromatographic system.Results The relative standard deviations of the three components were less than 0.94% and the three standards were all stable in 13 hours (RSD<0.46%).The mean recoveries were all between the range of 99.4%～100.0%,and the detectable limits were less than 2.3mg·L -1 .Conclusion The method is simple,sensitive,rapid and accurate,and can be used for the quality control of the policresulen solution.