填充吸附微萃取-高效液相色谱法检测水中3种肼类

Determination of Three Kinds of Hydrazine in Water Samples Using MEPS-HPLC

建立了基于填充吸附微萃取-液相色谱法检测水中肼、甲肼和偏二甲肼的方法。对影响方法效果的重要参数(如填充吸附微萃取的萃取材料、萃取循环次数和萃取速度、洗脱溶剂和洗脱体积、样品pH等)均进行了测试和优化。明确最优条件为先将样品pH调节为3.5,用HLB作为萃取材料,以15μL/s的速度进行15次重复萃取,用100μL含0.2%乙酸的乙腈进行洗脱。3种目标物在3 min内分离良好,并在10~500μg/L范围内线性良好,相关系数范围为0.997 8~0.999 1,检出限范围为2.0~5.0μg/L。在10、50、100μg/L 3个浓度水平加标实验中,3种肼类的平均回收率为76.7%~96.5%,日内相对标准偏差为5.6%~9.1%,日间相对标准偏差为8.5%~16.7%。该方法能够满足水体中3种肼类物质的快速测定要求。

A method was established for the determination of three kinds of hydrazine(Hydrazine,Methylhydrazine,1,1-Dimethylhydrazine) in water,based on microextraction by packed sorbent-HPLC.Important parameters that affect the effectiveness of the method,such as the extraction materials of MEPS,extraction cycle times and extraction speed,elution solvent and elution volume,and sample pH have been tested and optimized.The optimal conditions were obtained using HLB as the extraction material at a rate of 15 μL/s in 15 repeated extraction cycles after the sample pH was adjusted to 3.5.Then the target compounds were eluted with 100 μL acetonitrile containing 0.2% acetic acid.Three kinds of targets were well separated within 3 minutes.And the analytical method was demonstrated good linearity(10-500 μg/L) with correlation coefficient ranged from 0.9978-0.9991.The limits of detection were in the range of 2.0-5.0 μg/L.At the spiked levels of 10,50 and 100 μg/L,the average spiked recoveries for three kinds of hydrazine were 76.7%-96.5%.The relative standard deviation within the day was 5.6% to9.1%,and the relative standard deviation during the day was 8.5%-16.7%.Overall,the new method can meet the requirement of rapid determination of three kinds of hydrazine in water.