柱前衍生高效液相色谱法测量碳酰肼的含量

Determination of Carbohydrazide by High Performance Liquid Chromatography with Precolumn Derivatization

建立了苯甲醛衍生测量碳酰肼产品纯度的高效液相色谱法。研究了流动相中pH值、流动相组成、衍生反应时间等因素对测定的影响。采用KromasilC18(250mm×4.6mm,5μm)色谱柱,流动相为乙腈5mmol/L磷酸盐缓冲溶液,流速1mL/min,检测波长310nm,在8min内可完成分析。碳酰肼与苯甲醛在室温下衍生30min后可直接测量。此方法操作简单、快速;方法检出限为0.13mg/L;回收率为105%;RSD<1%,用于碳酰肼产品的纯度分析,结果令人满意。

The content of carbohydrazide was determined by derivatization with benzaldehyde followed by high performance liquid chromatography. The effects of the distribution proportion of the mobile phase, pH value and reaction time on derivatization were studied. Carbohydrazide derivative was separated on a Kromasil C-18 (250 mm x 4.6 mm,5 mm) column using acetonitrile 5 mmol/L phosphate buffer as mobile phase with a flow rate of 1 mL/min and detected at 310 nm within 8 min. The derivatization process took place at room temperature for 30 min. The limit of detection is 0.13 mg/L, recovery of carbohydrazide is 105% and RSD < 1%. This method has been applied to the determination of the qurity of carbohydrazide with satisfactory results.