苯甲胺作探针的毛细管电泳-间接紫外检测法检测注射用盐酸头孢吡肟中的N-甲基吡咯烷

建立了毛细管电泳 -间接紫外检测法检测注射用盐酸头孢吡肟中的 N-甲基吡咯烷。毛细管电泳条件 :采用熔融石英毛细管柱 (5 0μm i.d× 6 4 .5 cm,有效柱长为 5 6 cm ) ,以含 0 .0 1mol/ L苯甲胺和 0 .0 2 5 mol/ L甲酸的溶液 (p H3.6 )为背景电解质 ,电压为30 k V,柱温为 2 5℃ ,在 2 14 nm波长处间接检测。选用二乙胺作内标以提高方法的精密度。分离过程中在毛细管的进口处加 2 5 mbar的压力可得到稳定的基线。在选择性、线性、准确度、精密度、耐用性、重复性和检测限等方面 ,对该方法进行了认证。组分迁移时间的 RSD<0 .2 %。 N-甲基吡咯烷在 0 .0 2～ 0 .4 0 mg/ ml的浓度范围内的线性相关系数为 1.0 0 0 0。对照品溶液重复进样的 RSD为0 .9% (n=10 )。对照品溶液和供试品溶液分析的日内精密度 (RSD)分别为 1.6 % (n=10 )和 2 .9% (n=6 )

Indirect UV detection of N-methylpyrrolidine in cefepime hydrochloride for injection by capillary electrophoresis using benzylamine as a probe

N-Methylpyrrolidine in cefepime hydrochloride for injection was detected by capillary electrophoresis with indirect UV detection.Best results were achieved with back ground electrolyte constituting of 0.01mol/L benzylamine adjusted to pH3.6 with formic acid and an applied voltage of 30kV in a bare fused-silica capillary.Indirect UV detection was performed at a wavelength of 214nm.For precision improvement,diethylamine was utilized as internal standard.The application of a small amount of inlet pressure during the separation assisted the attainment of a stable baseline.The optimized method was validated regardingselectivity,linearity,accuracy,precision,ruggedness,repeatability and detection limits.Careful control of capillary conditioning enable migration time precisions values of＜0.2% RSD.The correlation coefficient for N-methylpyrrolidine,within the range of 0.02～0.40mg/ml,was 1.0000.The precision of standard solution injection was 0.9% RSD.The intra-day precisions for analysis of standard solution and sample solution were 1.6%RSD (n=10) and 2.9%RSD (n=6),respectively.