HPLC-脉冲安培检测器测定硫酸小诺霉素氯化钠注射液含量

目的：建立液相色谱（脉冲安培检测器）测定硫酸小诺霉素氯化钠注射液中小诺霉素组分含量的方法，为制定该类药的质量控制标准提供参考。方法：用十八烷基硅烷键合硅胶为填充剂（4.0 mm×150 mm，3 μm），以1.25%（v/v）三氟乙酸溶液[含0.025%五氟丙酸，0.85%（v/v）的50%氢氧化钠溶液，用0.5mol·L^-1的氢氧化钠溶液调节pH至2.6]-乙腈（97.5：2.5）为流动相，柱温为30℃，流速为0.7 mL·min^-1；柱后衍生氢氧化钠溶液浓度为0.5 mol·L^-1（含0.005 mol·L^-1乙二胺四乙酸溶液），以流速0.3 mL·min^-1等度淋洗。结果：小诺霉素在19.93~59.80 μg·mL^-1浓度范围内线性关系良好（r=0.999 6），小诺霉素精密度（RSD）为0.55%，检测下限为23.9 ng，平均回收率为99.1%。6批样品测定结果分别为90.7%、91.1%、90.6%、91.2%、90.7%、88.6%，与2015年版《中华人民共和国药典》方法结果无明显差异。结论：经方法学验证，本法适用于硫酸小诺霉素氯化钠注射液中小诺霉素组分含量的控制。

Objective: To establish a new method to analyze micronomicin content in micronomicin sulfate and sodium chloride injection using a liquid chromatographic method with pulsed electrochemical detection(LC-PED),to evaluate the quality of the drug. Methods: The seperation was performed on a C₁₈ column(4.0 mm×150 mm,3 μm). The mobile phase was 1.25%(v/v) trifluoroacetic acid[containing 0.025% pentafluoropropionic acid and 0.85%(v/v) of 50% sodium hydroxide,adjusting the pH to 2.6 with 0.5 mol·L^-1 NaOH]-acetonitrile(97.5:2.5) at a flow rate of 0.7 mL·min^-1. The temperature of the column was set at 30℃. 0.5 mol·L^-1 NaOH(containing 0.5 mol·L^-1 EDTA) was added post column at a flow rate of 0.3 mL·min^-1 to raise the pH of detection to at least 12. Results: The linearity of micronomicin ranges from 19.93 to 59.80 μg·mL^-1 with a correlation coefficient of 0.999 6. The precision(RSD) of micronomicin was 0.55%. The LOD of micronomicin was 5.98 μg·mL^-1(23.9 ng injected). The average recovery rate was 99.1%. The results of six samples were 90.7%,91.1%,90.6%,91.2%,90.7%,88.6%,respectivey. Conclusion: The method is proved to be applicable to the control of the content of micronomicin component in micronomicin sulfate and sodium chloride injection.

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