【摘要】：目的通過(guò)對(duì)柱后衍生化-HPLC-熒光檢測(cè)法和HPLC-蒸發(fā)光散射檢測(cè)法測(cè)定硫酸異帕米星注射液含量和有關(guān)物質(zhì)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(zhì)量控制的合理方法。方法色譜柱為YMC-pack ODS AM(4.6mm×250mm,3μm);流動(dòng)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(yīng)溫度為45℃,熒光激發(fā)波長(zhǎng)為360nm,發(fā)射波長(zhǎng)為440nm。結(jié)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(guān)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(cè)限為0.57ng,比HPLC-蒸發(fā)光散射檢測(cè)法的靈敏度高200多倍。結(jié)論本方法可以彌補(bǔ)采用現(xiàn)行中國(guó)藥典方法檢測(cè)靈敏度低、D-異帕米星和異帕米星同時(shí)洗脫的問(wèn)題;也可以彌補(bǔ)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(shí)洗脫、異帕米星和3N-異帕米星分離差的問(wèn)題。本方法檢測(cè)靈敏度高,簡(jiǎn)便快速,結(jié)果準(zhǔn)確可靠,適用于硫酸異帕米星及其注射液的質(zhì)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(hào)：2465958