【摘要】：目的:建立柱前衍生化高效液相色譜法測定異煙肼注射液中游離肼含量。方法:以苯甲醛為衍生化試劑,將游離肼衍生化為苯甲醛吖嗪,然后進(jìn)行高效液相色譜測定。采用Ultimate XB-C_(18)色譜柱(250 mm×4.6 mm,5μm),流動相為0.1%乙二胺四乙酸二鈉溶液-乙腈(30∶70),流速1.0 m L·min~(-1),檢測波長為310 nm,柱溫40℃。結(jié)果:游離肼質(zhì)量濃度在2.5~100μg·m L~(-1)范圍內(nèi)與其衍生物的峰面積呈良好線性關(guān)系,在低、中、高3個添加水平范圍內(nèi)的平均回收率為96.9%~101.0%,RSD在0.2%~3.0%之間,游離肼的檢出限為0.5μg·m L~(-1),定量限為2.5μg·m L~(-1)。3個批次樣品的測定結(jié)果分別為0.014%、0.043%和0.095%。結(jié)論:本文方法為異煙肼注射液的質(zhì)量控制提供了有效的檢測方法。
[Abstract]:Objective: to establish a precolumn derivatization HPLC method for the determination of free hydrazine in isoniazid injection. Methods: benzaldehyde was used as derivatization reagent, free hydrazine was derivatized to benzaldehyde azide, and then determined by high performance liquid chromatography. Ultimate XB-C_ (18) column (250 mm 脳 4.6 mm,5 渭 m),) was used as mobile phase of 0.1% ethylenediamine tetraacetic acid disodium solution-acetonitrile (30:70). The flow rate was 1.0 mL min~ (-1). The detection wavelength was 310 nm, at 40 鈩，

本文編號：2248617