分析化学2016，Vol.44Issue(6)：864-869,6.DOI:10.11895/j.issn.0253-3820.150895
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
Fast Determination of Semicarbazide in Water Sample by Hydrophilic Interaction Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
摘要
Abstract
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.关键词
亲水作用色谱/高分辨质谱/水样/氨基脲Key words
Hydrophilic interaction chromatography/High resolution mass spectrometry/Water samples/Semicarbazide引用本文复制引用
谢冬冬,沈金灿,淮文蓓,卞学海,叶刚,康海宁..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[J].分析化学,2016,44(6):864-869,6.基金项目
本文系国家自然科学基金(No.31201444)资助This work was supported by the National Natural Science Foundation of China (No.31201444) （No.31201444）
