高效液相色谱法测定硝酸羟胺水溶液的含量

Analysis of hydroxylammonium nitrate solution by HPLC

建立了高效液相色谱法(HPLC)测定硝酸羟胺含量的分析方法。采用柱前衍生化方法对样品进行预处理,通过对色谱条件和衍生化条件的优化,确定了以ZORBAX SB-C18色谱柱(100mm×2.1mm,3.5μm)进行分离,以乙腈-水为流动相进行梯度洗脱;使用2-硝基苯甲醛作为衍生化试剂,70℃水浴反应40min的衍生化方法。结果表明,衍生产物和衍生剂实现了完全分离,标准曲线线性关系良好,相关系数R=0.9999,在50μg/mL^150μg/mL加标水平下,加标回收率为99.14%~101.03%,RSD为0.7%~2.6%。该方法检测快速高效,精密度和准确度高,适用于硝酸羟胺含量的测定。

The sample was pretreated by pre-column derivatization,and the chromatographic and derivatization conditions were optimized.The derivatization reagent and derivatization product were separated by gradient elution with water-acetonitrile on a ZORBAX SB-C18 column(100 mm×2.1 mm,3.5μm).2-nitrobenzaldehyde was used as derivatization reagent.The reaction was carried out reacted for 10 min in a waterbath.The test results showed that the derivatization reagent and derivatization product were completely separated,the linear correlation coefficient was 0.9999.At three levels(50μg/mL,100μg/mL,150μg/mL),the average recoveries were within 99.14%-101.03%,and relative standard deviations were within 0.7%-2.6%.This method is rapid,accurate and sensitive.