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Pipette-tip micro-solid phase extraction based on melamine-foam@polydopamine followed by ultra-high-performance liquid chromatography–quadrupole–time-of-flight mass spectrometry for detection of psychotropic drugs in human serum
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2020-12-31 , DOI: 10.1016/j.jchromb.2020.122499
Xiaodan He , Tangqiang Sun , Ling Wang , Xuehua Jiang

In this work, pipette-tip micro-solid phase extraction (PT-μSPE) which packed by melamine-foam@polydopamine (MF@PDA) 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. MF@PDA 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 MF@PDA-PT-μSPE-UHPLC-QTOF is a sample and reliable method for the detection of psychotropic drugs in serum sample.



中文翻译:

基于三聚氰胺-泡沫@聚多巴胺的移液器尖端微固相萃取-超高效液相色谱-四极杆-飞行时间质谱法检测人血清中的精神药物

在这项工作中,用三聚氰胺-泡沫@聚多巴胺(MF @ PDA)填充的移液器尖端微固相萃取(PT-μSPE)结合超高效液相色谱-四极杆-飞行时间质谱( UHPLC-QTOF)用于提取和测定血清样品中的精神药物。考虑到操作背压,具有3D交联网格结构的三聚氰胺泡沫作为载体材料可提供高渗透性和接触表面。MF @ PDA通过多巴胺在弱碱性条件下的自聚合反应制备,并通过扫描电子显微镜(SEM),能量色散X射线光谱(EDX)和X射线光电子光谱(XPS)进行表征。PDA的表面基团含有儿茶酚结构,醌结构和胺基与精神药物具有多种相互作用,可以增加吸附能力。此外,还研究了影响萃取效率的参数,例如萃取和解吸循环,pH值,洗脱液类型,离子强度和吸附剂含量。基于TOF / MS的高灵敏度和高精度质量测量,在最佳萃取条件下,该方法的检测限(LOD)在0.002–0.1 ng ml范围内-1。线性在0.01ngml -1至600ngml -1的范围内,并且所有相关系数(R 2)均高于0.993。在实际样品测试中,加标回收率在80.04%至109.18%的范围内,RSD值从0.95%至9.85%获得。结果表明,MF @PDA-PT-μSPE-UHPLC-QTOF是一种检测血清样品中精神药物的可靠方法。

更新日期:2020-12-31
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