尿中肼的气相色谱测定法

Determination of Hydrazine in Urine by Gas Chromatography

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 highly sensitive and highly selective method for the determination of hydrazine in the urine. [ Methods] Hydrazine in the urine was hydrolyzed, derived, extracted, then separated with a capillary column and determined by GC-NPD. The chromatography operating conditions, hydrolyzed condition, derived condition and extracted condition were selected. [ Results] The detectable limit was 0.0012 mg/L; when the concentration of standard solution was 0.1 -2.0 mg/L, the correlation coefficient of calibration curves was 0.9995, the recovery of urine added standard solution was between 94.6% - 96.0%. The relative standard deviations （ RSD ） were 1.4% -3.7%. [ Conclusion] This method has advantages of symmetrical peak shape, not trailing, short retention time, non-interference of impurities, accurate, high sensitivity, high selectivity, fast and easy, etc.