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

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.