Magnetic particle spray mass spectrometry (MPS-MS), an innovative ambient ionization technique proposed by our research group, was employed to determine beta-blockers in human plasma samples. A dispersive solid phase extraction of atenolol, metoprolol, labetalol, propranolol, nadolol, and pindolol was carried out using magnetic molecularly imprinted polymer (M-MIP) particles that were attached to the tip of a metal probe, which was placed in the mass spectrometer inlet. A solvent (1% formic acid in methanol) was dispensed on the particles, and the Taylor cone was formed around them (in high voltage).
View Article and Find Full Text PDFMagnetic nanoparticles modified with tetraethyl orthosilicate (FeO@TEOS) and bovine serum albumin (FeO@TEOS@BSA) were evaluated as sorbent in albumin depletion from human serum samples by magnetic dispersive solid phase extraction. Characterization studies were carried out by X-ray diffraction, thermogravimetry, Fourier transform infrared spectroscopy, zeta potential, and scanning electron microscopy. Both nanoparticles also showed high thermal stability and pH-dependent surface charges.
View Article and Find Full Text PDFThe American continent is experiencing significant economic and industrial development driven by sustainability principles. In this context, discussions on improving energy consumption have become increasingly frequent and dynamic across various sectors of civil society, including the implementation of energy efficiency measures as advocated by the ISO energy management standard. However, there is a pressing need to investigate which socioeconomic aspects are responsible for the issuance of this certification in the Americas and how these factors relate to characteristic industrial emissions, especially particulate matter.
View Article and Find Full Text PDFInt J Biol Macromol
June 2024
Carbon nanotubes are promising materials for biomedical applications like delivery systems and tissue scaffolds. In this paper, magnetic carbon nanotubes (M-CNTs) covered with bovine serum albumin (M-CNTs-BSA) or functionalized with hydrophilic monomers (M-CNTs-HL) were synthesized, characterized, and evaluated concerning their interaction with Caco-2 cells. There is no comparison between these two types of functionalization, and this study aimed to verify their influence on the material's interaction with the cells.
View Article and Find Full Text PDFIn this work, the concept of magnetic particle spray mass spectrometry (MPS-MS) is reported for the first time. Magnetic sorbent particles are used to extract the analytes from a liquid sample. The particles are magnetically attracted to the tip of a magnetic probe that is positioned at the entrance of the mass spectrometer.
View Article and Find Full Text PDFACS Appl Mater Interfaces
December 2023
Small-molecule analyte detection is key for improving quality of life, particularly in health monitoring through the early detection of diseases. However, detecting specific markers in complex multicomponent media using devices compatible with point-of-care (PoC) technologies is still a major challenge. Here, we introduce a novel approach that combines molecularly imprinted polymers (MIPs), electrolyte-gated transistors (EGTs) based on 2D materials, and machine learning (ML) to detect hippuric acid (HA) in artificial urine, being a critical marker for toluene intoxication, parasitic infections, and kidney and bowel inflammation.
View Article and Find Full Text PDFFood Chem
March 2024
In the present study, a highly efficient analytical method based on preconcentration of tetracyclines (TCs) in water and milk samples using a magnetic molecularly imprinted polymer (FeO/SiO/MIP) synthesized by means of a novel semi-covalent synthesis for TCs and determination by HPLC-DAD was proposed. FeO/SiO/MIP showed specific superficial area of 216.0 m/g, superior to FeO/SiO/NIP (non-imprinted material) (103.
View Article and Find Full Text PDFPsychiatric disorders represent a significant socioeconomic and healthcare burden worldwide. Of these, schizophrenia, bipolar disorder, major depressive disorder and anxiety are among the most prevalent. Unfortunately, diagnosis remains problematic and largely complicated by the lack of disease specific biomarkers.
View Article and Find Full Text PDFAnal Chim Acta
April 2023
A procedure of direct magnetic sorbent sampling in flame atomic absorption spectrometry (DMSS-FAAS) was developed in this work. Metal-loaded magnetic sorbents were directly inserted in the flame of the FAAS for direct metal desorption/atomization. Magnetic graphene oxide aerogel (M-GOA) particles were synthesized, characterized, and used as a proof-of-concept in the magnetic dispersive solid phase extraction of Pb ions from water samples.
View Article and Find Full Text PDFThe direct magnetic sorbent sampling flame atomic absorption spectrometry (DMSS-FAAS), recently proposed by our research group, was applied to determine the lead in soy-based juice, whole grape juice, reconstituted grape juice, and orange nectar samples. A dispersive solid phase extraction (d-SPE) of lead was carried out using a magnetic orange peel powder, developed and optimized by Gupta et al (2012), that was inserted into flame by FAAS with a magnetic probe. The limits of quantification (<4.
View Article and Find Full Text PDFThis manuscript describes the development of magnetic restricted-access carbon nanotubes (M-RACNTs) for use as SPME sorbent to determine cannabidiol (CBD) and delta-9-tetrahydrocannabinol (THC) in human plasma samples by UHPLC-MS/MS. The adsorptive phase was immobilized on an SPME device by electromagnetic interactions between the M-RACNTs and a cylindrical neodymium magnet (3-mm diameter x 8-mm height) attached to a stainless-steel rod (3-mm diameter x 40-mm height). The M-RACNTs were synthesized by incorporating FeO magnetic nanoparticles (MNPs) into commercial carbon nanotubes (CNTs); then the surface of the resulting sorbent was further coated with a layer of bovine serum albumin (BSA).
View Article and Find Full Text PDFSmoking is the leading cause of preventable death worldwide. It is responsible for several types of cancer, cardiovascular diseases, and diseases of the reproductive system, among others. Therefore, advances in research are increasingly necessary in order to make smoking cessation treatment more effective.
View Article and Find Full Text PDFAnalyst
June 2022
A rapid and sensitive online restricted access molecularly imprinted solid-phase extraction method coupled to a liquid chromatography-mass spectrometry (LC-MS) system for simultaneous determination of serum bile acids as well as their taurine and glycine conjugates was developed. Reversible liver damage of workers exposed to volatile organic solvents can be investigated based on the level of the analyzed molecules. A restricted access molecularly imprinted polymer coated with bovine serum albumin (RAMIP-BSA) was synthesized and used as the extraction phase.
View Article and Find Full Text PDFUntreated samples were injected directly into a column switching system, an online SPE technique, using an extraction column packed with restricted access hybrid carbon nanotubes (RAHCNTs), a novel type of restricted access material, in an ultra-high performance liquid chromatography, coupled to a mass spectrometer (UHPLC-MS/MS). The synthesis of used restricted access material was relatively simple, quick, and reproducible, and had a high material yield. Compared to its predecessor, which is covered with bovine serum albumin (Restricted Access Carbon Nanotubes-RACNTs), RAHCNTs have improved performance when used for the analysis of organic compounds.
View Article and Find Full Text PDFThe use of conventional molecularly imprinted polymers (MIPs) for biological sample preparation is a difficult procedure due to the presence of high concentrations of proteins which can obstruct the selective binding sites, decrease the adsorption capacity, and compromise the analytical validation. In this way, modifications of conventional MIPs have been carried out in order to give them the ability to exclude macromolecules. Superficial coverings with hydrophilic groups and/or proteins have been the main procedures to obtain these restricted access molecularly imprinted polymers (RAMIPs ).
View Article and Find Full Text PDFBiosens Bioelectron
November 2021
Rational selection of predicted peptides to be employed as templates in molecular imprinting was carried out for the heat-denatured non-structural protein 1 (NS1) of dengue virus (DENV). Conservation analysis among 301 sequences of Brazilian isolates of DENV and zika virus (ZIKV) NS1 was carried out by UniProtKB, and peptide selection was based on in silico data of the conservational, structural and immunogenic properties of the sequences. The selected peptide (from dengue 1 NS1) was synthesized and employed as a template in the electropolymerization of polyaminophenol-imprinted films on the surface of carbon screen-printed electrodes.
View Article and Find Full Text PDFFood Chem
August 2021
FeO magnetic nanoparticles modified with tetraethyl orthosilicate and bovine serum albumin (FeO@TEOS@BSA) were synthesized and efficiently used to separate lysozyme from egg white. Glutaraldehyde was used to crosslink the bovine serum albumine molecules around the nanoparticles. The surface modifications were attested by transmission electron microscopy, infrared spectroscopy, thermogravimetry analysis, and zeta potential.
View Article and Find Full Text PDFLow concentrations of biomarkers as well as the complexity of biological samples make the clinical diagnoses of several diseases a challenging task. Sample preparation protocols remain a fundamental piece in the puzzle of analytical processes, and smart sorbents including molecularly imprinted polymers (MIPs) have been successfully used in this case. In this review, we depict the state of art for the rational design of MIPs to be used in solid phase extraction of disease biomarkers from biological samples.
View Article and Find Full Text PDFSpectrochim Acta A Mol Biomol Spectrosc
November 2020
In this work, magnetic restricted-access carbon nanotubes (M-RACNTs) were synthesized, characterized and used in the dispersive solid-phase extraction (d-SPE) of organophosphate pesticides (OPPs) from food samples (broccoli, eggplant, cauliflower, and soy milk), followed by spectrophotometric determination in a flow injection analysis system. FeO nanoparticles were incorporated in the multi-walled carbon nanotubes employing dimethylformamide. The dimethylformamide was used as a solvent in the incorporation process, forming the suspension of both particles.
View Article and Find Full Text PDFAnal Chim Acta
March 2020
Magnetic restricted-access carbon nanotubes (M-RACNTs) were synthesised and used for dispersive solid phase extraction of organophosphates (chlorpyriphos, malathion, disulfoton, pirimiphos) from commercial bovine raw milk samples. Due to their magnetic susceptibility, M-RACNTs were easily separated from the samples/solvents using a neodymium magnet, and the extracted organophosphates were analysed by gas chromatography-mass spectrometry. The protein exclusion capacity was about 100%.
View Article and Find Full Text PDFThis manuscript describes the development of the restricted access carbon nanotube (RACNT) as a selective stationary phase for microextraction by packed sorbent (MEPS) to determine antipsychotics (chlorpromazine, clozapine, olanzapine, and quetiapine) in untreated plasma samples from schizophrenic patients by ultra-high liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The synthesis was achieved by chemically covering commercial multi-walled carbon nanotubes with bovine serum albumin (BSA) to subsequently pack the material in a polyethylene conical tube (1000 μL). The RACNTs' sorbents were able to exclude about 97% of the plasma proteins, maintaining the same performance for about 100 assays.
View Article and Find Full Text PDFRestricted-access nanoparticles (RANPs) were prepared from bovine serum albumin by coacervation. They have an average sized of 311 nm. They were characterized and used to capture the β-blockers atenolol, metoprolol and propranolol from untreated biological samples.
View Article and Find Full Text PDFRestricted access molecularly imprinted polymers (RAMIPs) are hybrid materials that present selective binding sites for a template (or similar molecules), and an external hydrophilic layer that avoids the binding of proteins to the material, making them appropriate for the sample preparation of protein fluids. RAMIPs have been used successfully in online and offline solid phase extractions, but there is no application as a fiber in solid phase microextraction (SPME), to the best of our knowledge. In this paper, molecularly imprinted fibers were synthesized inside glass capillary tubes (0.
View Article and Find Full Text PDFThis study aimed to show that the physicochemical proprieties obtained by Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and scanning electronic microscopy (SEM) can be useful tools for evaluating the quality of active pharmaceutical ingredients (APIs) and pharmaceutical products. In addition, a simple, sensitive, and efficient method employing HPLC-DAD was developed for simultaneous determination of lidocaine (LID), ciprofloxacin (CFX) and enrofloxacin (EFX) in raw materials and in veterinary pharmaceutical formulations. Compounds were separated using a Gemini C (250 mm × 4.
View Article and Find Full Text PDFJ Chromatogr A
December 2017
A novel analytical method was developed to determine 5 antihypertensive drugs of different pharmacological classes (angiotensin-converting enzyme inhibitors, calcium channel blockers, α-2 adrenergic receptor agonists, angiotensin II receptor blockers, and aldosterone receptor antagonists) and some of their metabolites in human serum. The untreated samples were directly analyzed in a column switching system using an extraction column packed with restricted access carbon nanotubes (RACNTs) in an ultra-high performance liquid chromatography coupled to a mass spectrometer (UHPLC-MS/MS). The RACNTs column was able to exclude approximately 100% of proteins from the samples in 2.
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