Zihong Sun,Zhigang Luo,Cuifen Gan,Shidong Fei,Yingju Liu,Hongtao Lei
A sensitive electrochemical immunosensor for 3-bromobiphenyl (3-BBP) detection was constructed by employing a new polydopamine coated prussian blue-mesoporous carbon (PDOP/PB/CMK-3) nanocomposite as the substrate platform and multi-horseradish peroxidase-double helix carbon nanotubes-secondary antibody (multi-HRP-DHCNTs-Ab 2 ) as the signal label. PB/CMK-3 was firstly successfully in-situ synthesized with the aid of the CMK-3 reduction, which was characterized by transmission electron microscope (TEM), infrared spectroscopy (IR), X-ray diffraction (XRD) and N 2 adsorption–desorption analysis. By using PDOP/PB/CMK-3 as the substrate, it can effectively enhance the specific surface for antigen loading due to the three-dimensional structure of the nanocomposites, while large amount of PB that fixed inside or outside the pore of CMK-3 successfully improved the electrochemical response and the PDOP film can provide a biocompatible environment to maintain the activity of antigen availability. Under the optimized conditions, the proposed immunosensor shows a good current response to 3-BBP in a linear range from 5 pM to 2 nM with a detection limit of 2.25 pM. In addition, the specificity, reproducibility and stability of the immunosensor were also proved to be acceptable, indicating its potential application in environmental monitoring.
Suzuki–Miyaura cross-coupling is one of the most powerful strategies for constructing biaryl compounds. However, classic Suzuki–Miyaura coupling suffers from hour-scale reaction time and competitive protodeboronation. To address these problems, a mild nonaqueous potassium trimethylsilanolate (TMSOK)-assisted Suzuki–Miyaura coupling strategy was designed for the microsynthesis of biaryls in paper spray ionization (PSI). Due to the acceleration power facilitated by microdroplet chemistry in reactive PSI, the microsynthesis of biaryls by reactive PSI was accomplished within minutes with comparable yields to the bulk, showing good substrate applicability from 32 Suzuki–Miyaura reactions of aryl bromides and aryl boronic acid/borates bearing different substituents. Based on the above TMSOK-assisted Suzuki–Miyaura coupling strategy, we further developed a high-sensitivity and selective PSI mass spectrometry (MS) method for quantitative analysis of aryl bromides, a class of environmentally persistent organic pollutants that cannot be directly detected by ambient mass spectrometry due to their low ionization efficiency. In situ derivatization of aryl bromides was achieved with aryl borates bearing quaternary ammonium groups in PSI. The proposed PSI-MS method shows good linearity over the 0.01–10 μmol L–1 range with low detection limits of 1.8–4.8 nmol L–1 as well as good applicability to the rapid determination of six aryl bromides in three environmental water samples. The proposed PSI-MS method also shows good applicability to brominated flame retardants (polybrominated diphenyls/diphenyl esters). Overall, this study provides a simple, rapid, low-cost, high-sensitivity, and high-selectivity strategy for trace aryl bromides and other brominated pollutants in real samples with minimal/no sample pretreatment.
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