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(英文)  

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

作　　者：刘浩[1] 仇伟辰[2] 仇士林[1] 

机构地区：[1]上海市药品检验所,上海200233 [2]中美上海施贵宝制药有限公司,上海200240

出　　处：《中国抗生素杂志》2004年第4期217-222,243,共7页Chinese Journal of Antibiotics

摘　　要：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 )N -Methylpyrrolidine in cefepime hydrochloride for injection was detected by capillary electrophoresis with indirect UV detection. Best results were achieved with background 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 regarding selectivity, 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.

关 键 词：毛细管电泳 间接紫外检测 N-甲基吡咯烷 注射用盐酸头孢吡肟 苯甲胺 

分 类 号：O657.8[理学—分析化学] R978.11[理学—化学]