摘要
建立反相高效液相色谱-脉冲安培检测法(RP-HPLC-PAD)测定硫酸新霉素含量及有关物质方法。采用Thermo Acclaim^(TM) AmG C_(18)(4.6 mm×150 mm,3μm)色谱柱,以2%三氟乙酸溶液[含0.01%五氟丙酸+0.6%氢氧化钠]为流动相,采用积分脉冲安培电化学检测器四电位波形做为检测波形进行检测。测得新霉素B和新霉素C及13个杂质分离良好,新霉素B和新霉素C的检出限均为1.75 ng,定量限均为3.5 ng,新霉素B在0.14～27.89μg/mL内线性关系良好(r=0.998 5),新霉素C在0.14～4.69μg/mL内线性关系良好(r=0.999 6)。该HPLC-PAD法专属性强、灵敏度高、线性范围宽,具有良好的应用前景,为硫酸新霉素标准制定和质量控制提供了依据。
A novel method was developed for the content assay and related substances determination of neomycin sulfate by high performance liquid chromatography combined with pulsed amperometric detection (HPLC-PAD).The HPLC was performed on Thermo Acclaim^TM AmG C18 (4.6mm×150mm,3μm).The mobile phase consisted of aqueous solution with 2% trifluoroacetic acid containing 0.01% pentafluoropropionic acid and 0.6%NaOH.The pulsed amperometric detector was operated with aquadruple-potential waveform for the detection.Neomycin B,Neomycin C and thirteen related substances were adequately separated by the established HPLC conditions.The limits of detection (LOD) and quantification (LOQ) of neomycin B and neomycin C were both 1.75 ng and 3.5 ng,respectively.Good linearities of neomycin B and neomycin C were found in their respective ranges which their correlation coefficients were greater than 0.998 5.The established method is characterized by high specificity,sensitivity and wide range of linearity which has a good application prospect and provides the basis for improving the standard and quality control of neomycin sulfate.
作者
张倩
黄敏文
FANG Wang
张玫
杭太俊
袁耀佐
ZHANG Qian;HUANG Minwen;FANG Wang;ZHANG Mei;HANG Taijun;YUAN Yaozuo(Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China;St Jude Children′s Research Hospital,Memphis,TN,USA)
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2019年第2期193-199,共7页
Journal of China Pharmaceutical University
关键词
反相高效液相色谱-脉冲安培检测法
硫酸新霉素
含量测定
有关物质
high performance liquid chromatography combined with pulsed amperometric detection(HPLC-PAD)
neomycin sulfate
content
related substance
