高效液相色谱法测定沙咪珠利中的水合肼残留量

The Determination of Hydrazine Hydrate Residues in Acetamizuril by HPLC

关键词:  沙咪珠利  水合肼  含量测定  高效液相色谱法

Key words:  Acetamizuril  Hydrazine Hydrate  determination  High Performance Liquid Chromatography (HPLC)

摘要:

建立了一种沙咪珠利中水合肼残留检测的高效液相色谱法。含水合肼样品用盐酸溶液溶解后，加苯甲醛溶液衍生化，再用己烷提取，过滤后进样测定。采用Dikma Technologies Diamonsil C18色谱柱(250×4.6mm, 5μm)；流动相为乙二胺四乙酸钠0.03% m/V，乙腈（300:700，V/V）；流速1mL/min；紫外检测波长268nm。该方法在5ng/mL~150ng/mL的范围内具有良好的线性关系，回归方程Y=260.35X+796.12，R2=0.9993。10ng/mL、50ng/mL、100ng/mL三个添加浓度的添加回收率分别为105.58%、100.21%、102.60%，RSD分别为2.66%、3.16%、2.31%。该方法精密度好，快速准确，适用于沙咪珠利样品中水合肼残留量的检测。

Abstract:

A high performance liquid chromatography (HPLC) method for the determination of hydrazine hydrate residues in Acetamizuril was established. The hydrazine hydrate sample was dissolved in hydrochloric acid solution and then derivatized with benzaldehyde solution, extracted with hexane and filtered to measure the sample. A Diamonsil C18 column (250×4.6mm, 5μm)was used. The mobile phase was Sodium ethylenediaminetetraacetate 0.03% m/V, acetonitrile（300:700，V/V）. The flow rate was 1mL/min and the detection wavelength was 268 nm. The resolute showed that a good linear relationship was obtained with the concentration range of 5~150ng/mL and the regression equation was Y=260.35X+796.12，R2=0.9993. The recoveries at the three concentration of 10、50、100 ng/mL were 105.58%, 100.21%, 102.60% and RSD were 2.66%, 3.16% and 2.31%, respectively. The method was sensitive, accurate, convenient,and it is suitable for the determination of hydrazine hydrate residues in the samples of Acetamizuril.