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目的建立一种高灵敏度、高选择性测定尿中肼的新方法。方法尿中肼经水解、衍生和萃取后,用毛细管柱分离,氮磷检测器气相色谱法测定,对色谱操作条件、水解、衍生和萃取条件进行选择。结果方法的检出限为0.0012mg/L;当标准溶液浓度为0.1～2.0mg/L时标准曲线的相关系数为0.9995,尿样加标回收率在94.9%～96.0%之间,方法精密度(RSD)为1.4%～3.7%。结论该方法具有色谱峰形对称、不拖尾、保留时间短、无杂质干扰、准确、高灵敏度、高选择性、快速简便等优点。
Objective To establish a new method for the determination of hydrazine in urine with high sensitivity and selectivity. Methods Hydrazine in urine was hydrolyzed, derivatized and extracted. After separation by capillary column and gas chromatography with nitrogen and phosphorus detector, the operating conditions, hydrolysis, derivatization and extraction conditions were selected. The detection limit of the method was 0.0012mg / L. The correlation coefficient of standard curve was 0.9995 when the concentration of standard solution was 0.1-2.0mg / L, and the recoveries of spiked urine samples were between 94.9% and 96.0%. The method precision (RSD) was 1.4% ~ 3.7%. Conclusion The method has the advantages of symmetrical chromatographic peaks, no tailing, short retention time, no impurity interference, accurate, high sensitivity, high selectivity, quick and easy.