摘要
目的:建立采用 HPLC-蒸发光散射检测器(ELSD)法测定硫酸新霉素含量并对新霉胺杂质进行限度检查。方法:色谱条件为:Kromasil C_(18)色谱柱(250 mm×4.6 mm,5 μm),流动相:含0.7%五氟丙酸的25 mmol·L^(-1)乙酸铵溶液-甲醇(44:56),流速:1.0 mL·min^(-1);漂移管温度:110℃,载气流速:2.6 L·min^(-1)。用硫酸新霉素对照品测定新霉素的含量,以新霉胺对照品对新霉胺杂质进行限度检查。结果:新霉素进样量在7.2～35.8μg范围内,峰面积与进样量呈良好的线性关系(r=0.9996)。新霉胺的最低检出限和最低定量限分别为0.1μg和0.2μg。结论:方法快速、简便,重现性好,灵敏度高,可用于硫酸新霉素的含量测定及新霉胺杂质的控制。
Objective：To approach an assay method of determination for neomycin sulfate and a test method for its related substance neamine by HPLC - ELSD. Methods： The conditions were as follows ： an ELSD as the detector, Kromasil C18（250 mm ×4. 6 mm,5 μm）column as analytical column,0. 7% pentafluoropropionic acid of 25 mmol · L^-1 ammonium acetate solution - methanol （44： 56） as mobile phase,the flow rate was 1.0 mL · min^-1 ;the temperature of the drift tube was set at 110 ℃ ,and the flow rate of gas was 2. 6 L · min^-1. The contents of neomycin and neamine according to those of reference substances were determined. Results： The calibration curve of neomycin was linear over the range 7. 2 -35.8 μg. The limit of detection and the limit of quantitation for neamine were 0. 1 μg and 0. 2 μg. Conclusion：The method is proved to be rapid, sensitive, accurate and convenient. Furthermore, it gives good separation of neomycin and neamine within 10 minutes to finish an analysis. An excellent method for the assay of neomycin sulfate and limit test of neamine is proposed.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第2期212-215,共4页
Chinese Journal of Pharmaceutical Analysis
