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 C18(4.6 mm×250 mm, 5 μm)色谱柱;流动相为1 000 mL无二氧化碳的去离子水中加20 mL三氟乙酸,300 μL五氟丙酸,300 μL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0.498 5~9.969 1 μg·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 C18(4.6 mm×250 mm, 5 μm)column was used; the mobile phase was 1 000 mL deionized water containing 20 mL trifluoroacetic acid, 300 μL pentafluoropropionic, 300 μL 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 0.498-9.969 1 μg·mL-1, 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.
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