【摘要】：目的通過對柱后衍生化-HPLC-熒光檢測法和HPLC-蒸發(fā)光散射檢測法測定硫酸異帕米星注射液含量和有關物質的方法的比較,優(yōu)化并建立了硫酸異帕米星及其注射液質量控制的合理方法。方法色譜柱為YMC-pack ODS AM(4.6mm×250mm,3μm);流動相為含己烷磺酸鈉和冰醋酸的硫酸鈉溶液-乙腈(99:1),柱溫為35℃,流速為0.8m L/min。柱后衍生化試液為鄰苯二甲醛溶液,流速為0.8m L/min,衍生化反應溫度為45℃,熒光激發(fā)波長為360nm,發(fā)射波長為440nm。結果 D-異帕米星、1N,3N-異帕米星、異帕米星和3N-異帕米星之間分離良好,異帕米星在124.8~291.2μg/m L濃度范圍內(nèi)線性關系良好(r=1.0000),平均回收率為100.9%,RSD=0.9%(n=9)。該方法異帕米星的檢測限為0.57ng,比HPLC-蒸發(fā)光散射檢測法的靈敏度高200多倍。結論本方法可以彌補采用現(xiàn)行中國藥典方法檢測靈敏度低、D-異帕米星和異帕米星同時洗脫的問題;也可以彌補采用現(xiàn)行日本藥局方方法1N,3N-異帕米星和異帕米星同時洗脫、異帕米星和3N-異帕米星分離差的問題。本方法檢測靈敏度高,簡便快速,結果準確可靠,適用于硫酸異帕米星及其注射液的質量控制。
[Abstract]:Objective to compare the methods for the determination of isopamil sulfate injection and its related substances by post-column derivatization-HPLC- fluorescence detection and HPLC- evaporative light scattering detection. A reasonable method for the quality control of isopamil sulfate and its injection was optimized and established. Methods the column was YMC-pack ODS AM (4.6mm 脳 250 mm, 3 渭 m, the mobile phase was composed of sodium hexanesulfonate and acetic acid sodium sulfate solution-acetonitrile (99:1), the column temperature was 35 鈩，

本文編號：2465958