论文部分内容阅读
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 )
A capillary electrophoresis-indirect UV detection method was developed for the determination of N-methylpyrrolidine in cefepime hydrochloride for injection. Capillary electrophoresis conditions: A fused silica capillary column (50 μm id × 64.5 cm, effective column length of 56 cm) was charged with 0.1 mol / L benzylamine and 0.025 mol / L formic acid (P H3.6) as the background electrolyte at a voltage of 30 kV, with a column temperature of 25 ℃ and indirect detection at a wavelength of 2 14 nm. Diethylamine as internal standard to improve the precision of the method. A steady baseline can be obtained by applying a pressure of 25 mbar to the inlet of the capillary during separation. This method is certified for selectivity, linearity, accuracy, precision, durability, reproducibility, and detection limits. RSD of component migration time <0.2%. The linear correlation coefficient of N-methyl pyrrolidine in the concentration range of 0.2 ~ 0.400 mg / ml was 1.0 0 0 0. The RSD of the reference solution was 0.09% (n = 10) for repeated injections. The intra-day precision (RSD) of the reference solution and the test solution were 1.6% (n = 10) and 2.9% (n = 6)