An improvement method of pre-column derivatization LC-UV for assaying kanamycin in amikacin sulfate injection
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摘要: 目的 改进柱前衍生化-HPLC方法用于定量测定硫酸阿米卡星注射液中已知杂质卡那霉素。 方法 采用更低浓度的样品检测溶液,色谱柱:Agilent ZORBAX SB-C18柱 (4.6 mmá150 mm,5 μm);流动相:0.27%磷酸二氢钾溶液(用2.2%的氢氧化钾溶液调节pH值至6.5)-甲醇(30:70);检测波长:340 nm;进样量:50 μl;流速:1.0 ml/min;柱温:30℃。 结果 卡那霉素在2~80 μg/ml(r=0.999 8)浓度范围内呈线性关系,平均回收率为(93.08±9.65)%,样品稳定性提高。 结论 本法专属性强,灵敏度高,准确度好,为硫酸阿米卡星注射液的安全性评价提供了一个新的角度。Abstract: Objective To develop and evaluate the stable method for the determination of impurity D (kanamycin) in amikacin sulfate injection with pre-column derivatization HPLC. Methods The lower concentration of sample was used. An Agilent ZORBAX SB-C18 column(4.6 mmá150 mm, 5 μm) was used for the chromatographic separations. The mobile phase consisted of mixture of a 2.7% solution of potassium dihydrogen phosphate adjusted to pH 6.5 (using 22 g/L solution of potassium hydroxide) and methanol (30:70, v/v). The flow rate was 1 ml/min. A 50μl volume of each sample was injected. The column temperature was maintained at 30℃. Results The linear range of kanamycin was 2~80 μg/ml (r=0.999 8), accuracy was (93.08±9.65)%. Conclusions The development method was successfully applied to the quantitative determination of kanamycin in amikacin sulfate injection and also offered a new perspective for safety evaluation of amikacin sulfate injection.
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Key words:
- kanamycin /
- amikacin sulfate /
- HPLC /
- stability indicating /
- pre-column derivatization
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