文章摘要
朱晓玥,袁耀佐,张玫.HPLC-PAD法测定硫酸依替米星注射液有关物质及含量[J].中国药品标准,2019,20(6):532-536
HPLC-PAD法测定硫酸依替米星注射液有关物质及含量
Determination of related substances and contents in etimicin sulfate injection by HPLC-PAD
投稿时间:2019-10-16  修订日期:2019-11-20
DOI:
中文关键词: 氨基糖苷类抗生素  硫酸依替米星注射液  反相高效液相色谱  脉冲安培电化学检测
英文关键词: aminoglycoside antibiotics  etimicin sulfate injection  RP-HPLC  pulsed amperometric detection(PAD)
基金项目:
作者单位E-mail
朱晓玥 江苏省食品药品监督检验研究院 114549361@qq.com 
袁耀佐 江苏省食品药品监督检验研究院 yuanyaozuo@hotmail.com 
张玫 江苏省食品药品监督检验研究院  
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中文摘要:
      目的:建立硫酸依替米星注射液有关物质及含量的反相高效液相色谱-脉冲安培电化学(HPLC-PAD)法。方法:采用十八烷基硅烷键合硅胶为填充剂(4.6mm×250mm,5μm或效能相当的色谱柱),柱温35℃。以0.2mol.L-1三氟乙酸溶液(含0.05%五氟丙酸,1.5g.L-1无水硫酸钠,0.8%(V/V)的50%氢氧化钠溶液,用50%氢氧化钠溶液调节pH值至3.5)-乙腈(95:5)为流动相,流速为每分钟1.0ml。柱后加碱(50%氢氧化钠溶液1→25,流速每分钟0.5ml)。用积分脉冲安培电化学检测器检测。结果:依替米星在0.075~50μg.mL-1(r =0.9996)内线性关系良好;单个最大杂质的重复性试验的RSD(n =6)为1.4%,总杂质的重复性试验的RSD(n =6)为1.7%,含量测定的重复性试验的RSD(n =6)为0. 8%;方法的检测限(S/N =3)为75ng.mL-1,定量限(S/N =10)为250ng.mL-1;供试品溶液在12 h内稳定性良好。结论:经方法学验证,该方法可以用于硫酸依替米星注射液有关物质及含量的测定。
英文摘要:
      Objective:To establish an HPLC-PAD method for the determination of related substances and contents in etimicin sulfate injection.Methods:The separation was performed on a C18 column (4.6mm×250mm,5μm or a column of comparable performance).The column temperature was set at 35℃.The mobile phase contained 50mL acetonitrile and 950mL of an aqueous solution (adjust pH to 3.5 with 50% sodium hydroxide) containing 0.2mol.L-1 trifluoroacetic acid,0.05% pentafluoropropionic acid and 1.5g.L-1sodium sulphate at a flow rate of 1.0mL.min-1. NaOH(50% NaOH 1→25) was added post column at a flow rate of 0.5mL.min-1. Detected by pulsed amperometric detection (PAD).Results:The linear rang of etimicin was 0.075~50μg.mL-1(r=0.9996); The repeatability RSDs (n=6) of the maximum impurity and total impurities in a sample were 1.4% and 1.7%,respectively; The RSD (n=6) of the content in one sample was 0.8%;The LOD (S/N=3) and LOQ (S/N=10) were 75ng.mL-1 and 250ng.mL-1,respectively;The sample solution was stable within 12h. Conclusion: TheSvalidationSresultsSshowed thatStheSmethod is suitable for the determination of related substances and contents in etimicin sulfate injection.
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