利用磁固相萃取技术结合表面增强拉曼散射快速检测葡萄汁中的三唑磷

Rapid determination of triazophos in grape juice by magnetic solid phase extraction combined with surface enhanced Raman scattering

中文关键词:  磁固相萃取  表面增强拉曼散射  三唑磷  快速检测  葡萄汁

英文关键词:magnetic solid phase extraction  surface enhanced Raman scattering  triazophos  rapid detection  grape juice

中文摘要:

      目的 建立一种磁固相萃取技术结合表面增强拉曼散射(surface enhanced Raman scattering, SERS)方法, 用于快速检测葡萄汁中的三唑磷。方法 以Fe3O4为磁芯, 三醛基间苯三酚(trihydroxy-benzene tricarbaldehyde, Tp)和联苯胺(benzidine, BD)为配体合成共价有机框架(covalent organic framework, COF)包裹的磁性纳米材料Fe3O4@COF (TpBD)。以Fe3O4@COF (TpBD)为吸附材料, 通过π-π相互作用和氢键作用吸附样品溶液中的三唑磷, 实现复杂基质中三唑磷的分离和富集。以金纳米颗粒为SERS增强基底, 结合便携式拉曼光谱仪建立一种三唑磷的快速检测和定量分析方法。结果 利用1000、1409和1596 cm?1拉曼位移处的SERS信号强度计算的三唑磷检出限分别为2.97、3.57和3.44 nmol/L, 相关系数分别为0.96478、0.96774和0.95796。利用该方法检测葡萄汁中三唑磷的回收率为67.56%~86.80%, 相对标准偏差为0.99%~1.68%。结论 本研究建立的磁固相萃取结合SERS方法在三唑磷的快速检测和定量分析中表现出了良好的灵敏度、准确性和稳定性, 具有应用于果汁中三唑磷快速检测的潜力。

英文摘要:

      Objective To establish a rapid method for the determination of trizophos in grape juice by magnetic solid phase extraction combined with surface enhanced Raman scattering (SERS). Methods Using Fe3O4 as magnetic core, trihydroxy-benzene tricarbaldehyde (Tp) and benzidine (BD) as ligands, covalent organic framework (COF) covered magnetic nanomaterial Fe3O4@COF (TpBD) was synthesized. Using Fe3O4@COF (TpBD) as adsorption material, trizophos in the sample solution was separated and enriched by π-π interaction and hydrogen bonding, and the separation and enrichment of triazophos in complex matrix were realized. Using gold nanoparticles as SERS enhancing substrates and a portable Raman spectrometer, a rapid detection and quantitative analysis method of triazophos was established. Results The calculated limits of detection (LODs) of triazophos using the intensities of SERS signals at the Raman shifts of 1000, 1409 and 1596 cm?1 were 2.97, 3.57 and 3.44 nmol/L, respectively, and the correlation coefficients were 0.96478, 0.96774 and 0.95796, respectively. In addition, the method had been applied to the detection of triazophos in grape juice with recovery rates of 67.56%?86.80% and relative standard deviations of 0.99%?1.68%. Conclusion The established magnetic solid phase extraction combined with SERS method shows good sensitivity, accuracy and stability in the rapid detection and quantification of triazophos, and exhibits the potential to be applied in the rapid detection of triazophos in fruit juice.