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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,5μm)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0.3~30μg·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 a method for the determination of related substances in etimicin sodium chloride injection by reversed-phase high performance liquid chromatography-pulsed amperometry (HPLC-PAD). METHODS: The column was packed on a Welch Ultimate LP-C18 (4.6 mm × 300 mm, 5 μm) column at 30 ℃ with 0.2 mol·L-1 trifluoroacetic acid (adjusted to pH 2.0 with 50% sodium hydroxide solution) (92:8) as the mobile phase at a flow rate of 1.0 mL · min-1. After the column, the alkaline solution was 0.5 mol·L-1 sodium hydroxide solution and the flow rate was 0.5 mL · min-1. The detector was pulsed amperometric electrochemical detector , The working electrode is a gold electrode (3 mm diameter). RESULTS: Etilizumab showed a good linearity within the range of 0.3-30 μg · mL-1 (r = 0.9985). The RSD (n = 6) was 0.8% for the single largest impurity reproducibility test. The RSD (n = 6) was 1.3%. The limit of detection (S / N = 3) was 2.5 ng and the limit of quantification was 7.5 ng. The stability of the test solution was good within 12 h. Conclusion: This method is validated by methodology and can be used for the determination of related substances in etimicin sodium chloride injection.