Ionic liquids of methyltrioctylammonium chloride modified magnetic nanoparticles were prepared, and a new method of magnetic solid phase extraction combined with inductively coupled plasma-optical emission spectrometry was established for the determination of Cu, Zn, and Cd in human hair and urine samples. The effect of pH on the extraction of Cu, Zn, and Cd was investigated. The results show that the ionic liquid played a key role in the extraction of target analytes. The magnetic nanoparticles served as the carriers of the ionic liquid and the base of the phase separation. Several parameters affecting the extraction and desorption of the target analytes were investigated including the sample volume, extraction time, eluent concentration and volume, desorption time, sedimentation time, amount of the ionic liquid and Fe3O4@Si–OH, and the optimized conditions were established. Under the optimized conditions, the detection limits of Cu, Zn, and Cd were 0.54, 0.56, and 0.33 μg L−1, respectively, and the relative standard deviations (n = 7) were 4.9% (c = 2 μg L−1), 3.7% (c = 2 μg L−1), and 5.1% (c = 1 μg L−1), respectively. To validate the accuracy of the proposed method, it was applied to analyze certified reference materials of GBW07601 human hair and GBW09103 human urine. The determined values agree with the certified values. The developed method was also employed to analyze human hair and urine, and the recoveries for the spiked samples were in the range of 89.1% to 120%. The developed method was simple, highly sensitive, solvent-free, chelate-free, and could be considered as a green analytical technique.
Ya Yang,Suyan Zhai,Chao Liu,Xiaoshu Wang,Yifeng Tu
An ultrasensitive disposable immunosensor based on a gold nanoparticles (AuNPs)/indium tin oxide (ITO) substrate has been constructed to detect ketamine (KET) conveniently. In this study, we obtained a AuNPs/ITO basic electrode by only a two-step ecofriendly drip-coating procedure. The self-assembled monolayers of AuNPs were used as a hetero-bifunctional cross-linker and activator, respectively. Ketamine antibody was used as a biorecognition determinant and immobilized onto the AuNPs/ITO through electrostatic interaction or Au–S or Au–N bonds. The architectures of AuNPs/ITO were characterized by transmission electron microscopy, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy mainly. Electrochemiluminescence (ECL) was used to monitor the specific immune response between the antigen and antibody by measuring changes of intensity in the process of ECL. When the immune complex was incubated on the electrode, it blocked the electron communication and mass transfer, and the ECL signal was quenched. According to the quenched ECL signal, the quantification of KET can be realized. Under optimal conditions, the immunoassay showed a linear range from 10 to 100 pg/g. The low detection limit is 5.73 pg/g. The sensor has been applied to detect ketamine in human hair successfully. In addition, the immunosensor has excellent selectivity, outstanding reproducibility, and acceptable stability. What’s more, the immunosensor exhibits low-cost, simplicity, small sample consumption, and easy miniaturization, which allows it to be integrated into portable platforms to be utilized on the site of crime easily.