采用HPLC-PED法测定硫酸小诺米星及其注射液有关物质和组分的探讨  

Detection of the related substances and component in micronomicin sulfate and its injection by HPLC-PED

作　　者：赵敬丹 蒋孟虹 刘浩 Zhao Jing-dan;Jiang Meng-hong;Liu Hao(Shanghai Institute for Food and Drug Control,Shanghai 201203)

机构地区：[1]上海市食品药品检验研究院,上海201203

出　　处：《中国抗生素杂志》2022年第10期1065-1069,共5页Chinese Journal of Antibiotics

基　　金：2021年上海市药品监督管理局研究课题(No.LX-2021-08)。

摘　　要：目的新建硫酸小诺米星及其注射液有关物质和组分检查的HPLC-脉冲安培电化学检测(PED)法,并探讨其用于评价硫酸小诺米星及其注射液质量的合理性。方法色谱柱为Welch Ultimate LP-C_(18)(3.9 mm×300 mm,5μm);以1.5%三氟醋酸溶液(用50%氢氧化钠溶液调节pH值至2.6)-乙腈(98:2,V/V)为流动相,脉冲安培电化学检测器检测,金电极为工作电极,四电位波形工作模式,柱后加0.5 mol/L NaOH溶液,流速0.4 mL/min。结果新建的电化学检测法可实现小诺米星相关杂质和小诺米星组分的准确定量,灵敏度是蒸发光散射检测法(ELSD)的近40倍,对于国产硫酸小诺米星及其注射液质量控制具有重要作用。结论HPLC-PED法灵敏度高,重复性好,可替代或和现有蒸发光散射法联合作为硫酸小诺米星及其注射液有关物质和组分检查的分析方法。Objective To establish an HPLC method with pulsed electrochemical detector(PED)for the analysis of micronomicin sulfate and its injection,and evaluate its rationality.Methods A Welch Ultimate LPC_(18)(3.9 mm×300 mm,5μm)column was used,and the mobile phase was 1.5%trifluoroacetic acid solution(the pH of the aqueous solution was adjusted to 2.6 with 50%NaOH solution)-acetonitrile(98∶2)at a flow rate of 1.0 mL/min.A pulsed electrochemical detector was used.The electrochemical cell consisted of a working electrode,a pH-Ag/AgCl reference electrode,and a titanium counter electrode.The working electrode was a gold electrode(diameter 3 mm)and a quadruplepotential waveform was selected as the detection waveform.The 0.5 mol/L NaOH solution was added post column at a flow rate of 0.4 mL/min.Results The method can be used for comprehensive analysis of the impurity profile of micronomicin and its injection,and also the determination of the accurate amount of component of micronomicin.The sensitivity is nearly 40 times higher than that of ELSD,and thus it will play an important role in routine quality control.Conclusion The PED method was proved to be sensitive and repeatable,and can replace the ELSD method as a new method to detect related substances and component of micronomicin.

关 键 词：小诺米星 庆大霉素C_(1a) 杂质 ELSD 脉冲安培检测 

分 类 号：R978.1[医药卫生—药品]