离子色谱法测定硫酸庆大霉素片的C组分及有关物质

目的：建立离子色谱法测定硫酸庆大霉素片的C组分含量及有关物质。方法：采用ThermoAcclaim^TM AmG C₁₈（4.6 mm×150 mm，3 μm）色谱柱，流动相为0.7%三氟乙酸（含0.025%五氟丙酸，50%氢氧化钠4 mL，用50%氢氧化钠溶液调节pH至2.6）-乙腈（96.5：3.5）；流速为1.0 mL·min^-1，柱后溶液为2%的氢氧化钠溶液，柱后流速0.3 mL·min^-1，柱温35℃；检测器为脉冲安培电化学检测器，工作电极为金电极（直径3 mm），检测电位为四电位。结果：硫酸庆大霉素片C₁、C_1a、C₂、C_2a分别在1.328~132.8、1.606~160.6、7.378~737.8、1.276~127.6 μg·mL^-1浓度范围内线性关系良好，回收率范围为98.2%~101.8%；有关物质测定，西索米星在2.632~52.64 μg·mL^-1、小诺霉素在2.006~25.07 μg·mL^-1浓度范围内线性关系良好，西索米星检测下限为0.01 μg，小诺霉素检测下限为0.02 μg；各杂质与硫酸庆大霉素各C组分色谱峰间均能完全分离。结论：该方法准确灵敏，可用于硫酸庆大霉素片的质量控制。

Objective:To establish an ion chromatography method for determination of the C components and related substances of gentamicin sulfate tables.Methods:A ThermoAcclaim^TM AmG C₁₈ (4.6 mm×150 mm, 3 μm) column was used, the mobile phase was 0.7% trifluoroacetic acid (containing 0.025% pentafluoropropanoic acid and 4 mL of 50% sodium hydroxide solution, adjusted pH to 2.6 with 50% sodium hydroxide solution) -acetonitrile (96.5:3.5).The flow was 1.0 mL·min^-1, the post-column solution was 2% sodium hydroxide solution and the flow was 0.3 mL·min^-1, the column temperature was 35℃.Pulsed amperometric detection was used with the working electrode of gold electrode (3 mm), and working mode of a four potential waveform.Results:The linear ranges of gentamicin C₁, C_1a, C₂, and C_2a, were 1.328-132.8 μg·mL^-1, 1.606-160.6 μg·mL^-1, 7.378-737.8 μg·mL^-1, 1.276-127.6 μg·mL^-1 respectively, the range of recoveries were 98.2%~101.8%.The linear ranges of sisomicin and micronomicin were 2.632-52.64 μg·mL^-1 and 2.006-25.07 μg·mL^-1 with the detection limits of sisomicin and micronomicin of 0.01 μg and 0.02 μg, respectively.The related substances and gentamicin c components could be separated completely.Conclusion:This method is accurate and sensitive, and suitable for the quality control of gentamicin sulfate tables.

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