Simple Voltammetric Determination of Iron in Ethanol and Biodiesel Using a Bismuth Film Coated Glassy Carbon ElectrodeAlmeida, Joseany M. S.; Ribeiro, Ana Beatriz P.; Toloza, Carlos A. T.; Alves, Ismael C. B.; Santos, José Ribamar N.; De Azevedo, Lorena C. M.; Aucélio, Ricardo Q.; Marques, Aldaléa L. B.
doi: 10.1080/00032719.2022.2053701pmid: N/A
Abstract Square-wave adsorptive stripping voltammetry (SWAdSV) was used to determine iron in ethanol and biodiesel using a bismuth-film electrode (BiFE) prepared onto the surface of a glassy carbon electrode (GCE) by electrochemical deposition to promote the reduction of Fe (III) previously complexed with 1-(2-pyridylazo)-2-naphthol (PAN) directly in the electrochemical cell. The supporting electrolyte was composed by mixture of acetate buffer (0.1 mol L−1, pH 4.5) and ethanol (40/60% v/v) into which 500 µL of a 0.1 mmol L−1 stock solution of PAN was added as complexing agent. The Fe (III)-PAN complex presented a well-defined current peak at −0.7 V. For biodiesel, a treatment with tetramethylammonium hydroxide (TMAH) was proposed as an efficient mean to minimized matrix interferences. A limit of detection of 6.0 × 10−8 mol L−1 (0.06 µmol L−1) and limit of quantification of 2.0 × 10−7 mol L−1 (0.2 µmol L−1) were obtained for Fe(III). Under the optimized conditions, there were no significant interferences from Cu(II), Al(III), Mn(II), Cr(III), Cd(II), Zn(II) and Ni(II) and Pb(II) while Ni(II) interfered significantly. The analytical curves produced linear responses with equations I (µA) = (-1.315 × 10−7 ± 5.158 × 10−8) + (-0.238 ± 0.01) [Fe (III)] (µmol L−1), R2 = 0.992 and I (µA) = (-6.836 × 10−7 ± 1.124 × 10−8) + (-0.408 ± 0.013) [Fe (III)] (µmol L−1), R2=0.998 for pure ethanol and biodiesel, respectively. The method produced satisfactory results in quantifying original quantities of Fe(III) in fuel ethanol (5.65 ± 0.71 µmol L−1) and biodiesel (1.28 ± 0.25 µmol L−1) at a 95% confidence limit (n = 3).
Characterization of Calcium Oxide Treated Lead–Lead Dioxide Vitroceramics from Recycled Automobile Batteries by X-Ray Diffraction, Infrared and Ultraviolet–Visible Spectroscopy, and VoltammetryPiscoiu, D. N.; Rada, S.; Macavei, S.; Vermesan, H.; Culea, E.
doi: 10.1080/00032719.2022.2053860pmid: N/A
Abstract Today the number of automobiles is increasing, and hence, the demand for lead-acid batteries is enhanced. Improvements regarding reusable car batteries implies the elimination of disadvantages of the traditional recycling methods. The purpose of this work is: (i) to recycle the spent plates from a car battery with high wear by an eco-innovative method and (ii) to characterize the prepared materials and to characterize their electrochemical performance for new electrodes for batteries. The prepared samples were investigated by X-ray diffraction, infrared and ultraviolet–visible spectroscopy, and cyclic voltammetry and linear sweep voltammetry. The results show that following the addition of calcium ions into the lead–lead dioxide recycled matrix and the formation of Ca3(SO3)2SO4 crystalline phase were evident. These results suggest that no emissions of sulfur oxides into the atmosphere.
Determination of Abrin by a Magnetic Affinity Immunoassay (MAIA) Based on the Signal Amplification of the Aptamer and Staphylococcal Protein A (SPA) Functionalized Gold Magnetic Microparticles (GMPs)Mu, Xihui; Du, Bin; Liu, Houfang; Gao, Chuan; Liu, Zhiwei; Wang, Jiang; Liu, Shuai; Liu, Bing; Xu, Jianjie; Tong, Zhaoyang
doi: 10.1080/00032719.2022.2053983pmid: N/A
Abstract A new magnetic affinity immunoassay (MAIA) was developed for the determination of abrin based on signal amplification of staphylococcal protein A (SPA) functionalized gold magnetic microparticles (GMPs) and the aptamer. This assay consisted of a sandwich format in which SPA-coated GMPs coupled anti-abrin monoclonal antibodies (mcAb) were used as the magnetic capture probe and the enzyme-labeled abrin aptamer was used as the signal probe. Abrin was successfully determined by the proposed strategy. This method exhibited a linear response to abrin from 0.031 to 31.25 μg/L with a detection limit of 0.031 μg/L. The staphylococcal protein A, gold magnetic microparticles, and aptamer increased the sensitivity by 4 times, 2 times and 2 times, respectively The integrated amplification produced by these parameters increased the sensitivity by 16-fold compared to the traditional double-antibody sandwich enzyme linked immunosorbent assay (ELISA). This method possesses a low detection limit, acceptable reproducibility, and high specificity, which demonstrates that the MAIA shows promise in trace toxin determination.
Detection of Biomarkers Associated with Acute Kidney Injury by a Gold Nanoparticle Based Colloidal Nano-Immunosensor by Fourier-Transform Infrared Spectroscopy with Principal Component AnalysisOrtega-Hernández, Noelia; Ortega-Romero, Manolo; Medeiros-Domingo, Mara; Barbier, Olivier Christophe; Rojas-López, Marlon
doi: 10.1080/00032719.2022.2053982pmid: N/A
Abstract A colloidal nano-immunosensor based on gold nanoparticles covered in their surface with protein A and the immunoglobulin anti-kidney injury molecule-1 was prepared and tested in human urine to identify a biomarker that diagnose acute kidney injury. The urine was obtained from patients with cancer treated with cisplatin, diagnosed with acute kidney injury, and from healthy individuals. Fourier-transform infrared spectroscopy analysis showed important spectral differences between both types of groups, primarily for the intervals from 1750 to 1500 cm−1 and from 1000 to 891 cm−1 where the amide I group (C = O) and the glycosylated functional groups of this protein absorb. The principal component analysis applied to the vibrational signals obtained with the nano-immunosensor allows adequate discrimination of urine from patients with acute kidney injury from samples from healthy individuals. The simplicity of the proposed method, from the preparation of the nano-immunosensor to the spectral and chemometric analysis, may make this method an interesting alternative to practically diagnose acute kidney injury using a small volume of urine.
Characterization of Rose Essential Oils by Double-Region Atmospheric Pressure Chemical Ionization Mass Spectrometry (DRAPCI-MS) with Principal Component Analysis (PCA), Hierarchical Cluster Analysis (HCA), and Heatmap AnalysisLi, Minglei; Zhang, Yihan; Xi, Hui; Fu, Yingjie; Wang, Hui; Zhang, Yipeng; Sun, Shihao
doi: 10.1080/00032719.2022.2055563pmid: N/A
Abstract Double-region atmospheric pressure chemical ionization – tandem mass spectrometry (DRAPCI-MS/MS) was used for the direct determination of the volatiles of Chinese Kushui rose essential oil (CKREO), Bulgaria Damask rose essential oil (BDREO), Turkish Damask rose essential oil (TDREO), and Moroccan Damask rose essential oil (MDREO). Eight shared aroma compounds of rose essential oils (REOs) were identified by DRAPCI-MS/MS. Twenty REOs of different species and geographical origins were conducted by principal component analysis (PCA), hierarchical cluster analysis (HCA), and heatmap analysis. Moreover, the volatile components of REOs were determined by gas chromatography – mass spectrometry (GC-MS). Cluster analysis and a Venn diagram demonstrated significant differences among four populations of REOs. Both methods showed that the REOs from these populations were divided into two groups based on the species, presenting the reliability of the quantitative and chemometrics results of DRAPCI-MS. These results demonstrate that the DRAPCI-MS is suitable to identify the species responsible for the REOs.
Central Composite Design (CCD) and Box-Behnken Design (BBD) for the Optimization of a Molecularly Imprinted Polymer (MIP) Based Pipette Tip Micro-Solid Phase Extraction (SPE) for the Spectrophotometric Determination of Chlorpyrifos in Food and JuiceTamandani, Mahsa; Hashemi, Sayyed Hossein
doi: 10.1080/00032719.2022.2056192pmid: N/A
Abstract A novel micro-solid phase extraction protocol based on a new molecularly imprinted polymer (MIP) sorbent is reported for the isolation of chlorpyrifos from rice, juice and fish samples followed by spectrophotometric determination. The MIP sorbent was packed into a pipette tip. The type and volume of the eluent, pH, mass of MIP, sample volume, and number of extraction and elution cycles were evaluated utilizing a one-variable-at-a-time protocol, central composite design, and Box-Behnken design. The results demonstrated the optimum performance of central composite design. The linear range under the optimal conditions for chlorpyrifos was from 1 to 1000 µg L−1 with a limit of detection of 0.17 µg L−1 and a relative standard deviation less than 4.3%. The protocol was successfully employed for the determination of trace concentrations of chlorpyrifos in fish, juice, and rice.
Electrodeposition of a Silver Nanoparticle Substrate with Application for Surface-Enhanced Raman Spectroscopy (SERS)Zhang, Nan; Zhao, Jianwei; Chen, Deli; Yuan, Guiyun
doi: 10.1080/00032719.2022.2056745pmid: N/A
Abstract A silver substrate with fine nanograins was prepared by electrodeposition. The deposition potential was approximately −1.0 V which was consistent with a mechanism dominated by progressive nucleation. Scanning electron microscopy (SEM) showed that the Ag nanoparticles were between 8 and 16 nm in size mainly. The electrodeposition and the nucleation mechanism were further studied by a three-electrode system. The crystalline particles were small and closely arranged due to the dominance of progressive nucleation. The uniformity of the substrate was determined by two-dimensional surface-enhanced Raman spectroscopy (SERS) mapping using rhodamine 6 G (R6G) as the probe. The Raman surface enhancement was evaluated. The results showed that when the analyte concentration was 10−12 mol·L−1 the most intense rhodamine 6 G peak at 611 cm−1 was present.
Electrodeposition of Cerium Oxide Nanoparticles on the Graphenized Carbon Ceramic Electrode (GCCE) for the Sensitive Determination of Isoprenaline in Human Serum by Differential Pulse Voltammetry (DPV)Shafaei, Sepideh; Akbari Nakhjavani, Sattar; Kanberoglu, Gulsah Saydan; Khalilzadeh, Balal; Mohammad-Rezaei, Rahim
doi: 10.1080/00032719.2022.2057525pmid: N/A
Abstract Cerium oxide nanoparticles (CeO2) are widely used as the electrocatalyst in solar cells, fuel cells, water splitting, and electroanalytical experiments. Therefore, controlled electrodeposition of CeO2 on the surface of electrodes may improve the performance of electrochemical devices. CeO2 was electrochemically deposited on the surface of a graphenized carbon ceramic electrode (GCCE) for the determination of isoprenaline in biological samples. The pH, temperature, deposition time, and applied potential were optimized for the electrodeposition. According to differential pulse voltammetry, the linear range, detection limit, and sensitivity of the designed assay were from 5 to 310 nM, 3.03 nM and 25.21 × 10−5 µA µM−1 cm−2, respectively. Easy preparation, low cost, and high production repeatability of the developed CeO2/GCCE suggest further applications. The prepared modified electrode was successfully utilized for the determination of isoprenaline in human serum with satisfactory results.
Determination of Heterocyclic Aromatic Amines (HAAs) in Urban Particulate Standard Reference Material and Wildfire-Influenced Particulate Matter by High-Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS)Miller-Schulze, Justin P.; Dal Porto, Rachael; Fagundes, Ashley; Oanh Pham, Kim; Olson, Michael; Schauer, James J.
doi: 10.1080/00032719.2022.2058522pmid: N/A
Abstract Heterocyclic aromatic amines (HAAs) are carcinogenic and mutagenic compounds formed by the cooking of meat and combustion of biomass. There are relatively few data on HAAs in atmospheric particulate matter (PM). We developed an analytical method using high performance liquid chromatography – tandem mass spectrometry (tandem quadrupole, HPLC-MS/MS(QqQ)) to analyze PM samples for 12 HAAs. We applied this method to an urban air standard reference material and wildfire-impacted PM2.5 from the 2018 wildfire season in Northern California. The PM sample matrix adversely impacted the MS/MS response, with high levels of ion suppression for sample masses >4 mg and higher ion suppression in wildfire-impacted particulate matter compared with the standard reference material. Despite detection limits at the low ng level, no HAAs were detected in the standard reference material, but β-carboline norharman (0.34 ng/m3) was detected in one wildfire sample.