离子色谱法测定硫酸阿米卡星及其制剂的有关物质

Determination of related substances of amikacin sulfate and its preparation by ionchromatography

目的:建立离子色谱法测定硫酸阿米卡星及其制剂的有关物质。方法:采用YMC ODS-Aq C_(18)(4.6 mm×250 mm,5μm)色谱柱;流动相为1000 mL无二氧化碳的去离子水中加20 mL三氟乙酸,300μL五氟丙酸,300μL七氟丁酸,50%(v/v)氢氧化钠溶液8 mL,用50%(v/v)氢氧化钠溶液调节pH为3.3,最后加乙腈10 mL;流速为1.0 mL·min^(-1);柱后溶液为42 mL·L^(-1)的50%(v/v)氢氧化钠溶液;柱后流速为0.3 mL·min^(-1);柱温为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),检测电位为糖四电位。结果:阿米卡星质量浓度在0.4985~9.9691μg·mL^(-1)范围内线性关系良好,阿米卡星检测限为2.0 ng;各杂质与阿米卡星峰均能完全分离。8批次硫酸阿米卡星原料总杂含量为1.2%~1.7%,77批次硫酸阿米卡星注射液总杂含量为1.1%~2.3%;10批次注射用硫酸阿米卡星总杂含量为1.2%~2.2%。结论:该方法准确、灵敏,可用于阿米阿星及其制剂的质量控制。

Objective:To establish an ion chromatography method for determination of the related substances of amikacin sulfate and its preparation.Methods:A YMC ODS-Aq C;(4.6 mm×250 mm,5μm)column was used;the mobile phase was 1000 mL deionized water containing 20 mL trifluoroacetic acid,300μL pentafluoropropionic,300μL heptafluorobutyricacid,and 8 mL 50%(v/v)sodium hydroxide solution.The pH was adjusted to 3.3 with 50%(v/v)sodium hydroxide solution.Then 10 mL of acetonitrile was added.The flow rate was 1.0 mL·min^(-1),the post-column solution was 42 mL·L^(-1) sodium hydroxide solution and the flow rate was 0.3 mL·min^(-1).The column temperature was 35℃and the pulsed amperometric detection was adopted.The working electrode was gold electrode(3 mm),with working mode of a four potential waveform.Results:The linear range of amikacin was 0.498-9.9691μg·mL;,the detection limits of amikacin was 2.0 ng.Therelatedsubstances and amikacin could be separated completely.Conclusion:This method is accurate and sensitive,and suitable for the quality control ofamikacin sulfate and its preparation.