亲水作用色谱-四极杆/静电场轨道阱高分辨率质谱快速测定水样中氨基脲

建立了亲水作用色谱-四极杆/静电场轨道阱高分辨质谱快速检测水中氨基脲的方法。水样中加入0.1 mol/ L NaOH 溶液后,以乙腈为提取剂,加入过量 Na2 SO4,使乙腈与水分层,乙腈提取液再经无水 Na2 SO4脱水后,采用亲水作用色谱柱 Amide 色谱柱分离,以0.1%甲酸水溶液及0.1%甲酸乙腈溶液为流动相进行梯度洗脱,四极杆/静电场轨道阱高分辨率质谱电喷雾正离子、选择离子监测模式检测,同位素内标法进行定量分析。在最优实验条件下,氨基脲在0.2~20μg/ L 浓度范围内线性相关系数为0.997,方法的检出限为0.09μg/ L,定量限为0.30μg/ L。以淡水和海水为空白样品,在添加浓度为0.5,1.0和5.0μg/ kg 水平下,氨基脲的加标回收率为82.3%~92.0%,相对标准偏差小于7.6%。本方法适用于环境水样中氨基脲的快速分析。

Fast Determination of Semicarbazide in Water Sample by Hydrophilic Interaction Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

A method for rapid determination of semicarbazide in water by hydrophilic interaction chromatography-quadrupole / electrostatic field orbitrap high resolution mass spectrometry was developed. The sample was extracted with acetonitrile after 0. 1 mol/ L NaOH was added in the sample and then excessive amounts of Na2 SO4 was added to stratify acetonitrile from the mix solution. The acetonitrile extraction solution was dehydrated with anhydrous sodium sulfate. The preparation was separated by an amide column using as hydrophilic interaction column, and gradient elution program was employed by using water and acetonitrile containing 0. 1% formic acid as mobile phase, then it was detected in positive and selected ion monitoring mode by a quadrupole / electrostatic field orbitrap high resolution mass spectrometry. Internal standard method was used for quantitative analysis. The linear correlation coefficient of semicarbazide was 0. 997 in the concentration range of 0. 2 -20 μg / L under the optimal conditions. The limit of detection was 0. 09 μg / L, while the limit of quantitation was 0. 30 μg / L. The recoveries were 82. 3% to 92. 0% , and the relatively standard deviations were less than 7. 6% at the spiked levels of 0. 5, 1. 0 and 5. 0 μg / L using river water and sea water as blank samples. The developed method is suitable for the analysis of trace semicarbazide in environment water samples.