摘要
目的 :采用反相高效液相色谱柱前衍生化法测定硫酸依替米星的含量。方法 :衍生化条件 :衍生化试剂为邻苯二醛 ,反应温度为 6 0℃ ,反应时间为 15min。色谱条件 :色谱柱为KromasilC1 8柱 (5 μm ,2 0 0mm× 4 6mm) ;流动相为水 冰醋酸 甲醇 (2 0∶5∶75 )配制的 0 0 2mol L的庚烷磺酸钠溶液 ;检测波长为 330nm ;流速为 1ml min。结果 :线性范围 :0 1～ 1 0mg ml,r=0 9999;该方法与微生物法测定结果基本一致 ,衍生化产物稳定。结论 :所建立的反相高效液相色谱柱前衍生化法能准确测定硫酸依替米星的含量 。
Objective: To develope the determination method of Etimicin Sulfate by a pre-column Derivation HPLC. Methods: The determination method of Etimicin Sulfate by a pre-column Derivation HPLC on a 200 mm×4.6 mm i.d. C 18 column (5 μm particles, Kromasil) with a UV detector set at 330 nm was developed. The mobile phase was 0.02 mol/L Sodium Haptanesulfonate diluted by a mixture consisting of 20 volumes of water, 5 volumes of acetic acid and 75 volumes of Methanol and chromatography was performed at a flow rate of 1 ml/min. Sample was derivatized with o-Phthalaldehyde at 60℃ water bath for 15 minutes. Results: The linear relationship was good in range of 0.1～1.0 mg/ml(r=0.9999), RSD of the method was 0.4%. The difference between the results determined by HPLC and microbial assay are negligible. Conclusion: The method has a good accuracy and reproducibility.
出处
《药学进展》
CAS
2004年第7期314-317,共4页
Progress in Pharmaceutical Sciences
