庆大霉素中C组分含量及有关物质的HPLC-PAD法测定.pdfVIP

中国医药工业杂志 Chinese Jouma1 of Phannaceutica1s 2015 , 46(2) 193 • -，~，~溢血 Z 药品分析与质控 3 Cc. c ‘c.c.c.C.CCc. ccccc.c.c.‘ 庆大霉素中 C 组分含量及有关物质的 HPLC-PAD 法测定 秦峰，赵敬丹，刘浩，闻宏亮，杨吴成* (上海市食品药品检验所，上海 201203) 摘要:建立了高效液相色谱·脉冲安培电化学法测定庆大霉素的C 组分及其有关物质。采用亲水性C8 色谱柱，以 50mmoνL 氢氧化纳溶液(含0.7%三氟乙酸和 0.025% 五氟丙酸，pH2.6) 乙腊 (98.5 : 1.5) 为流动相。脉冲安培检测器， 金电极为工作电极，四电位波形工作模式。庆大霉素主要的 C 组分 (C ，、 C 、 C，和 C，，)分别在 6.233 ~ 249.3 、 5.819 ~ 232.8、 6.923 ~ 276.9 和 4.002 ~ 160.1 μg!m1 浓度范围内线性关系良好。回收率为99.0%~ 102.8% ， RSD 为l.3%~ 2.2% 。 关键词:庆大霉素:有关物质:高效液相色谱:脉冲安培电化学法:测定 中图分类号: R917: 0657.7+2 文献标志码:A 文章编号: 1001-8255 (2015) 02-0193-04 Determination ofGentamicin C and Related Substances by HPLC-PAD QIN Feng , ZHAO Jingdan , LIU Hao , WEN Hongliang , YANG Meicheng* (Shanghai b四itutefor Food Drug Control. Shanghai 201203) ABSTRACT: An HPLC coupled with pulsed amperometric detection (PAD) method was established for the determination of gentamicin C and its related substances. A hydrophilic C8 column was used , with the mobile phase of 50 mmo l/L sodium hydroxide solution (containing 0.7% trifluoroacetic acid and 0.025% pentafluoropropanoic acid , pH 2.6) : acetonitrile (98.5 : 1.5). The working electrode was golden electrode , with working mode of a four potential waveform. It was linear for gentamicin C Ca , C2 and C2a in the ranges of 6.233 - 249.3 、 5.819 - 232.8、 6.923 - 276.9 and 4.002 - 160.1μg1ml， respectively. Their recoveries were 99.0 % - 102.8 %, with RSDs of 1.3 % - 2.2 %. Key Words: gentamicin; related substance; HPLC; pulsed amperometric detection; determination 庆大霉素 (gentamicin， 1)是由绎红小单抱