| 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: |
|
| 摘要点击次数: 908 |
| 全文下载次数: 128 |
| 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． |
|
查看/发表评论 下载PDF阅读器 |
| 关闭 |
|
|
|