Citation: XIE Dong-Dong, SHEN Jin-Can, HUAI Wen-Bei, BIAN Xue-Hai, YE Gang, KANG Hai-Ning. Fast Determination of Semicarbazide in Water Sample by Hydrophilic Interaction Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(6): 864-869. doi: 10.11895/j.issn.0253-3820.150895 shu

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

1.
Food Inspection & Quarantine Center of Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen Key Laboratory of Detection Technology R&D on Food Safety, Shenzhen 518045, China;
2.
Traditional Chinese Medicine College of Guangdong Pharmaceutical University, Guangzhou 528458, China

Received Date: 8 November 2015
Revised Date: 6 January 2016

Fund Project: This work was supported by the National Natural Science Foundation of China (No.31201444)

Figures(3)

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 Na₂SO₄ 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.
- Hydrophilic interaction chromatography,
- High resolution mass spectrometry,
- Water samples,
- Semicarbazide
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沈阳化工大学材料科学与工程学院沈阳 110142