Saraji Mohammad, Jafari Mohammad Taghi, Mossaddegh Mehdi
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
J Chromatogr A. 2016 Jan 15;1429:30-9. doi: 10.1016/j.chroma.2015.12.008. Epub 2015 Dec 9.
A high efficiency solid-phase microextraction (SPME) fiber coated with porous carbon nanotubes-silicon dioxide (CNTs-SiO2) nanohybrids was synthesized and applied for the determination of some organophosphorus pesticides (OPPs) in vegetables, fruits and water samples. Gas chromatography-corona discharge ion mobility spectrometry was used as the detection system. Glucose, as a biocompatible compound, was used for connecting CNT and SiO2 during a hydrothermal process. The electrospinning technique was also applied for the fiber preparation. The parameters affecting the efficiency of extraction, including stirring rate, salt effect, extraction temperature, extraction time, desorption temperature and desorption time, were investigated and optimized. The developed CNTs@SiO2 fiber presented better extraction efficiency than the commercial SPME fibers (PA, PDMS, and PDMS-DVB). The intra- and inter-day relative standard deviations were found to be lower than 6.2 and 9.0%, respectively. For water samples, the limits of detection were in the range of 0.005-0.020 μg L(-1) and the limits of quantification were between 0.010 and 0.050 μg L(-1). The results showed a good linearity in the range of 0.01-3.0 μg L(-1) for the analytes. The spiking recoveries ranged from 79 (± 9) to 99 (± 8). The method was successfully applied for the determination of OPPs in real samples.
合成了一种涂覆有多孔碳纳米管 - 二氧化硅(CNTs - SiO2)纳米杂化物的高效固相微萃取(SPME)纤维,并将其用于测定蔬菜、水果和水样中的某些有机磷农药(OPPs)。采用气相色谱 - 电晕放电离子迁移谱作为检测系统。葡萄糖作为一种生物相容性化合物,在水热过程中用于连接碳纳米管和二氧化硅。静电纺丝技术也用于纤维制备。研究并优化了影响萃取效率的参数,包括搅拌速率、盐效应、萃取温度、萃取时间、解吸温度和解吸时间。所制备的CNTs@SiO2纤维表现出比市售SPME纤维(PA、PDMS和PDMS - DVB)更好的萃取效率。日内和日间相对标准偏差分别低于6.2%和9.0%。对于水样,检测限在0.005 - 0.020 μg L(-1)范围内,定量限在0.010至0.050 μg L(-1)之间。结果表明,分析物在0.01 - 3.0 μg L(-1)范围内具有良好的线性。加标回收率在79(±9)至99(±8)之间。该方法成功应用于实际样品中OPPs的测定。