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目的:建立HPLC-ECD法测定盐酸大观霉素有关物质。方法:应用高效液相色谱-电化学检测器,Waters XBridge C18色谱柱(4.6 mm×250 mm,5μm),以pH 3.2的草酸盐缓冲溶液-乙腈(1000∶105)为流动相,流速为1.0 mL.min-1;柱后溶液为21 g.L-1的氢氧化钠溶液,流速0.5 mL.min-1;ECD系统参数:极性为阳性,检波+0.12 V,氧化电位+0.70 V,还原电位-0.60 V,范围20μA。结果:盐酸大观霉素有关物质在2.25～45μg.mL-1范围内呈良好的线性关系,r=0.9999;Y轴截距在100%浓度响应值的7.3%处,在100%浓度的25%～500%的范围内,对任一点的响应值在此点理论值的97.7%至103.6%的范围内;平均回收率(n=9)为98.9%,RSD为2.9%。结论:该方法简便易行,准确度高,重复性好,可用于盐酸大观霉素及相关制剂产品的质量控制。
Objective: To establish HPLC-ECD method for the determination of spectinomycin hydrochloride related substances. Methods: The mobile phase was eluted with a mobile phase of oxalic acid (pH = 3.2) and acetonitrile (1000:105) using a Waters XBridge C18 column (4.6 mm × 250 mm, 5 μm) 1.0 mL · min-1; the column was a 21 g L-1 sodium hydroxide solution at a flow rate of 0.5 mL · min-1; the ECD system parameters: positive polarity, detection +0.12 V, oxidation potential +0.70 V, Potential -0.60 V, range 20μA. Results: The spectinomycin hydrochloride showed a good linear relationship in the range of 2.25-45 μg.mL-1, r = 0.9999. The Y-intercept was 7.3% of the 100% To 500%, the response to any point is within the range of 97.7% to 103.6% of the theoretical value at this point; the average recovery (n = 9) is 98.9% and the RSD is 2.9%. Conclusion: The method is simple, accurate, reproducible and can be used for the quality control of spectinomycin hydrochloride and related preparations.