Magnetic single-walled carbon nanotubes-dispersive solid-phase extraction method combined with liquid chromatography-tandem mass spectrometry for the determination of paraquat in urine
Magnetic single-walled carbon nanotubes-dispersive solid-phase extraction method combined with liquid chromatography-tandem mass spectrometry for the determination of paraquat in urine
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DOI：
10.1016/j.jchromb.2014.06.016
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发表时间：
2014-08-15
影响因子：
3
通讯作者：
Lai, Yong-Qiang
中科院分区：
文献类型：
--
作者：
Ruan, Xiao-Lin;Qiu, Jing-Jing;Lai, Yong-Qiang
在这项研究中，磁性单壁碳纳米管（MSWCNTs）的制备通过浸渍磁性Fe 3 O 4纳米粒子的羧基单壁碳纳米管表面的静电相互作用的基础上。以制备的MSWCNTs为吸附剂，对人尿液中的百草枯进行分散固相萃取（DSPE）。吸附后的百草枯用5%TFA的乙腈溶液定量解吸，用HPLC-MS进行测定。通过对碳纳米管吸附剂种类、提取时间、样品体积、洗涤溶剂、解吸溶剂种类和体积等提取参数的优化，获得了较高的DSPE回收率和提取效率。在优化的条件下，线性范围为3.75-375.0 μ g/L，相关系数为0.999 45。检出限（S/N = 3）和定量限（S/N = 10）分别为0.94和2.82 μ g/L。加标真实的尿样的回收率为92.89 ~ 108.9%，相对标准偏差小于3.21%。最后，将该方法成功地用于疑似百草枯中毒患者尿样中百草枯的测定。MSWCNTs表现出合适的性能和较高的吸附能力，用于百草枯的提取。(C)2014爱思唯尔有限公司版权所有。
In this study, magnetic single-walled carbon nanotubes (MSWCNTs) were prepared by impregnating magnetic Fe3O4 nanoparticles onto the surfaces of carboxylic single-walled carbon nanotubes based on electrostatic interactions. The prepared MSWCNTs were used as the adsorbent for the dispersive solid-phase extraction (DSPE) of paraquat from human urine. After adsorption, the paraquat was quantitatively desorbed with 5%TFA in acetonitrile and determined by HPLC-MS. Extraction parameters such as the type of CNT adsorbent, extraction time, sample volume, wash solvent, and the type and volume of desorption solvent were optimized to obtain high DSPE recoveries and extraction efficiencies. Under the optimized conditions, the calibration curve was linear in the range 3.75-375.0 mu g/L with a correlation coefficient of 0.999 45. The LOD (S/N = 3) and LOQ (S/N = 10) were 0.94 and 2.82 mu g/L, respectively. The recoveries ranged from 92.89 to 108.9% for spiked real urine samples with RSDs below 3.21%. Finally, the new method was successfully used to determine paraquat in urine samples of suspected paraquat poisoning patients. The MSWCNTs exhibited suitable properties and a high adsorption capacity for the extraction of paraquat. (C) 2014 Elsevier B.V. All rights reserved.