氨基脲
色谱法
化学
检出限
尿
串联质谱法
质谱法
再现性
萃取(化学)
电喷雾
电喷雾电离
液相色谱-质谱法
定量分析(化学)
高效液相色谱法
残留物(化学)
生物化学
有机化学
作者
Haibo Yang,Xiaoli Jiang,Yanli Wang,Chen Li,Hang Li,Weihong Huang
标识
DOI:10.1080/19440049.2021.1898678
摘要
An ultra-performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry (UPLC-ESI-MS/MS) with pre-column derivatisation was developed and validated for the determination of semicarbazide in human urine. Urine samples were derivatised with 2-nitrobenzaldehyde and subsequently extracted with acetonitrile. Extracts were concentrated and then analysed by UPLC-MS/MS. The time per run was 7 min. Good results were observed for the linearity of matrix-matched calibration curves (R2 > 0.99) in the concentration range of 1–100 µg/L. The absolute recovery ranged from 98.7% to 108.6%, with the relative standard deviations (RSDs) of 2.2%-3.6%. The limit of detection and quantification for the semicarbazide was 0.5 µg/L and 1 µg/L, respectively. The method showed good extraction efficiency, high sensitivity, and good reproducibility. It was suitable for the detection of semicarbazide in human urine. Residues of semicarbazide were between 1.0 and 41.5 μg/L in children’s 24-h urine. This work is the first report on the quantitative analysis of SEM in 24-h human urine samples.
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