LC-PED法测定硫酸依替米星注射液及硫酸依替米星氯化钠注射液中有关物质  

Determination of related substances in etimicin sulfate injection and etimicin and sodium chloride injection by LC-PED

作　　者：吴宇宁[1,2] 赵卫 朱晓玥 袁耀佐 张玫 徐寒梅[2] 潘广文 谭力 

机构地区：[1]江苏省食品药品监督检验研究院,南京210008 [2]中国药科大学生命科学与技术学院,南京210009 [3]赛默飞世尔科技(中国)有限公司,上海201203

出　　处：《中国抗生素杂志》2016年第8期618-623,共6页Chinese Journal of Antibiotics

摘　　要：目的建立硫酸依替米星注射液及硫酸依替米星氯化钠注射液有关物质检查的液相色谱-脉冲安培电化学（LC—PED）检测方法，并与2015版《中国药典》收载硫酸依替米星有关物质第二法——HPLC-ELSD法进行比较。方法新建立方法以0．2mol／L三氟乙酸（含0．05％五氟丙酸，1．5g／L无水硫酸钠，用NaOH调节pH值至3．5）-乙腈=96：4为流动相，柱温为35℃，流速为1．0mL／min，四电位波形检测，柱后加碱（50％氢氧化钠溶液1→25），流速0．5mL／min。HPLC-ELSD法按照2015版《中国药典》硫酸依替米星有关物质第二法实验。结果新建立方法的LOD（S／N=3）为2ng，LOQ（S／N=10）为6ng；方法精密度良好；依替米星在0．24-451．t8：／mL（r=0．9997）内线性关系良好；与HPLC-ELSD法相比，分离能力更强，灵敏度更高，结果更加准确。结论该方法选择性更好，灵敏度更高，可作为硫酸依替米星注射液与硫酸依替米星氯化钠注射液有关物质检查的常规方法。Objective To establish an LC-PED method for determination of related substances in etimicin sulfate injections and etimicin and sodium chloride injections and to compare the analytical performance of LC-PED with HPLC- ELSD（procedure 2） prescribed in Chinese Pharmacopoeia 2015（Ch.P2015） for the analysis of etimicin. Methods The mobile phase contained 40mL acetonitfile and 960mL of an aqueous solution （adjust pH to 3.5 with 50% sodium hydroxide） containing 0.2mol/L trifluoroacetic acid, 0.05% pentafluoropropionic acid and 1.Sg/L sodium sulphate at a flow rate of 1.0mL/ min; a quadruple-potential waveform （QPW） was selected as detection waveform. NaOH（50% NaOH 1→25） was added post column at a flow rate of 0.5mL/min. The HPLC-ELSD method is prepared and practiced according to procedure 2 prescribed in 2015 for the analysis of etimicin. Results About the LC-PED method we developed, the LOD and LOQ of etimicin were found to be 2 and 6ng respectively. The linearity of etimicin ranges from 0.24-45μg/mLwith a coefficient of determination equal to 0.9997. Compared to HPLC-ELSD, this method shows higher selectivity and sensitivity. Conclusion This method proved to be sensitive, repeatable, linear, robust and can be applied to the determination of related substances in etimicin sulfate injectionsand etimicin and sodium chloride injections.

关 键 词：氨基糖苷类抗生素 硫酸依替米星注射液 硫酸依替米星氯化钠注射液 有关物质:脉冲安培电化学检测器 

分 类 号：R978.1[医药卫生—药品]