摘要
目的:建立硫酸依替米星氯化钠注射液有关物质的反相高效液相色谱-脉冲安培电化学(HPLC-PAD)检测方法。方法:采用Welch Ultimate LP-C18(4.6 mm×300 mm,5 μm)色谱柱,柱温30 ℃,以0.2 mol·L-1三氟乙酸(用50%氢氧化钠溶液调pH至2.0)-乙腈(92:8)为流动相,流速1.0 mL·min-1,柱后碱溶液为0.5 mol·L-1氢氧化钠溶液,流速0.5 mL·min-1,检测器为脉冲安培电化学检测器,工作电极为金电极(3 mm直径)。结果:依替米星在0.3~30 μg·mL-1(r=0.9985)内线性关系良好;单个最大杂质的重复性试验的RSD(n=6)为0.8%,总杂质的重复性试验的RSD(n=6)为1.3%;方法的检测限(S/N=3)为2.5 ng,定量限(S/N=10)为7.5 ng;供试品溶液在12 h内稳定性良好。结论:该方法经方法学验证,可以用于硫酸依替米星氯化钠注射液有关物质的测定。
Objective: To establish an HPLC-PAD method for the determination of the related substances in etimicin sulfate and sodium chloride injection. Methods: The separation was performed on a Welch Ultimate LP-C18column (4.6 mm×300 mm,5 μm) and detected by pulsed amperometric detection (PAD) on a gold electrode (diameter:3 mm).The column temperature was set at 30 ℃.The mobile phase consisted of an aqueous solution containing 0.2 mol·L-1 trifluoroacetic acid (pH adjusted to 2.0 with 50% sodium hydroxide solution) and acetonitrile (92:8),the flow rate was 1.0 mL·min-1.The alkaline solution after column was 0.5 mol·L-1 sodium hydroxide solution at a flow rate of 0.5 mL·min-1. Results: The linear rang of etimicin was 0.3-30 μg·mL-1(r=0.9985).The repeatability RSDs (n=6) of the maximum impurity and total impurities in a sample were 0.8% and 1.3%,respectively.The LOD (S/N=3) and LOQ (S/N=10) were 2.5 ng and 7.5 ng,respectively.The sample solution was stable within 12 h. Conclusion: The method is simple,accurate and sensitive,and suitable for the determination of the related substances in etimicin sulfate and sodium chloride injection.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第12期2151-2155,共5页
Chinese Journal of Pharmaceutical Analysis