化学
色谱法
萃取(化学)
检出限
质谱法
固相萃取
三聚氰胺
吸附
分析化学(期刊)
富集因子
有机化学
作者
Xiaodan He,Tangqiang Sun,Ling Wang,Xuehua Jiang
标识
DOI:10.1016/j.jchromb.2020.122499
摘要
In this work, pipette-tip micro-solid phase extraction (PT-μSPE) which packed by [email protected] ([email protected]) coupled with ultra-high-performance liquid chromatography–quadrupole–time-of-flight mass spectrometry (UHPLC-QTOF) was developed for extraction and determination of psychotropic drugs in serum samples. Considering the operation back pressure, the melamine-foam as carrier material with 3D cross-linked grid structure can provide high permeability and contact surface. [email protected] was prepared by self-polymerization reaction of dopamine under weak alkaline conditions and characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The surface group of PDA containing catechol structure, quinone structure and amine group has multi-interaction with psychotropic drugs which can increase the adsorption capacity. Moreover, the parameters affecting extraction efficiencies such as extraction and desorption cycle, pH value, eluent type, ionic strength and amount of sorbent were investigated. Based on the high sensitivity and accuracy mass measurement by TOF/MS, under the optimized extraction condition, the limits of detection (LOD) of this method were obtained in the range of 0.002–0.1 ng ml−1. The linearity was ranged from 0.01 ng ml−1 to 600 ng ml−1, and all the correlation coefficients (R2) were above 0.993. The spiked recoveries were in the range of 80.04% to 109.18% in real sample test and RSD values obtained from 0.95% to 9.85%. The results demonstrate that [email protected]μSPE-UHPLC-QTOF is a sample and reliable method for the detection of psychotropic drugs in serum sample.
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