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acetonitrile; detection limit; fluorescence; food research; hexane; oxidation; pyrogallol; reversed-phase high performance liquid chromatography; saponification; sausages; tetrahydrofuran; vitamin A
Abstract:
... A reliable and sensitive reverse-phase HPLC method is described for the separation and quantification of all-trans-retinol and dl-α-tocopherol in cooked sausages. Samples were chromatographed with UV and fluorescence detection on a 15 cm x 0.4 cm i.d. Spherisorb ODS-2, 5 μm column, using as mobile phase a mixture of 90% acetonitrile and 10% tetrahydrofuran. Sample preparation included saponificati ...
... Glutathione (GSH) is a thiol with an important function in protecting tissue against the oxidative stress which has been related to carcinogenesis in the colon. For this reason the development of probiotic species producing glutathione could be of great interest. To determine the glutathione content of some probiotic bacteria of the Bifidobacterium and Lactococcus genera, a very sensitive and sele ...
... A high-performance liquid chromatographic method has been developed for the simultaneous determination of classical neuroleptics (chlorpromazine, haloperidol, loxapine and clotiapine), atypical antipsychotics (clozapine, quetiapine and risperidone) and their active metabolites (N-desmethylclozapine, clozapine N-oxide and 9-hydroxyrisperidone) in human plasma. Separation was obtained by using a C8 ...
... Amperometric acetylcholinesterase biosensors have been developed for quantification of the pesticides carbofuran, carbaryl, methylparaoxon, and dichlorvos in phosphate buffer containing 5% acetonitrile. Three different biosensors were built using three different acetylcholinesterase (AChE) enzymes--AChE from electric eel, and genetically engineered (B394) and wild-type (B1) AChE from Drosophila me ...
acetonitrile; acetylcholine; cultured cells; detection limit; hydrophilic interaction chromatography; tandem mass spectrometry
Abstract:
... A fast liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the analysis of acetylcholine (ACh) in cultured cells. [²H₄]Acetylcholine (ACh-d ₄) was used as an internal standard for calibration. ACh was extracted from the cell lysate with acetonitrile (ACN)/water (80/20, v/v) and the crude extract was analyzed without further purification. Isocratic hydrophilic interac ...
... A sensitive, selective, and reproducible in-tube polypyrrole-coated capillary (PPY) solid-phase microextraction and liquid chromatographic method for fluoxetine and norfluoxetine enantiomers analysis in plasma samples has been developed, validated, and further applied to the analysis of plasma samples from elderly patients undergoing therapy with antidepressants. Important factors in the optimizat ...
... A simple CE method has been developed for the separation and determination of thyroxine (T₄) enantiomers in pharmaceutical formulations. The method was based on ligand-exchange mechanism using a Cu(II)/L-proline complex as chiral selector. The effects of different parameters affecting separation such as chiral selector concentration, organic additive, buffer pH and temperature were investigated. A ...
... A simple, fast, and sensitive liquid-liquid extraction method followed by nonaqueous capillary electrophoresis (LLE/NACE) was developed and validated for simultaneous determination of four antidepressants (fluoxetine, sertraline, citalopram and paroxetine) in human plasma. Several experimental separation conditions using aqueous and nonaqueous media separation were tested by varying the electrolyt ...
... A simple and rapid open-vessel focused microwave-assisted extraction (FMAE) method followed by LC analysis was developed for the determination of ketoprofen lysine salt in the presence of methyl p-hydroxybenzoate and propyl p-hydroxybenzoate preservatives in topical cream. Extraction were performed in acetone/potassium dihydrogenphosphate (25 mM, pH 3.0) (70:30 v/v) by reaching a target temperatur ...
... Praziquantel (PZQ) is a highly lipophilic drug with low aqueous solubility. Despite this, it is well absorbed from the gastrointestinal tract. In this study, a simple LC method was developed and validated, in order to monitor the concentration of PZQ in TC-199 buffer in vitro, in the rat everted gut sac absorption model. PZQ was analyzed by a reversed-phase LC method with an isocratic mobile phase ...
... An original HPLC method coupled to spectrofluorimetric detection is presented for the simultaneous analysis in dried blood spots (DBS) of cocaine and two important metabolites, namely benzoylecgonine (its main metabolite) and cocaethylene (the active metabolite formed in the presence of ethanol). The chromatographic analysis was carried out on a C8 column, using a mobile phase containing phosphate ...
acetonitrile; atmospheric pressure; detection limit; drugs; ionization; liquid chromatography; meat; metabolites; monitoring; tandem mass spectrometry; toltrazuril
Abstract:
... In this work a fast liquid chromatography (LC)–tandem mass spectrometry (MS/MS) method was developed for the analysis of toltrazuril, a coccidiostatic drug, and its metabolites in meat food products. The applicability of atmospheric pressure chemical ionization (APCI) and heated electrospray ionization in both positive and negative modes was studied. APCI in negative mode provided the best results ...
acetonitrile; aqueous solutions; benzylpenicillin; ion exchange; ions; milk; models; molecular imprinting; polymers; propranolol; salts; solid phase extraction; water activity
Abstract:
... Salt ions were found to have an influence on template binding to two model molecularly imprinted polymers (MIPs), targeted to penicillin G and propranolol, respectively, in water-acetonitrile mixtures. Water was detrimental to rebinding of penicillin G whereas propranolol bound in the entire water-acetonitrile range tested. In 100% aqueous solution, 3-M salt solutions augmented the binding of both ...
Saracino, Maria Addolorata; Pieri, Maria Chiara; Raggi, Maria Augusta, et al. ; Marcheselli, Chiara; Somaini, Lorenzo; Gerra, Gilberto; De Stefano, Francesco; Show all 7 Authors
... An isocratic high-performance liquid-chromatographic method has been developed for the simultaneous determination of disulfiram and bupropion in human plasma samples. Analyses were carried out on a C₈ reversed-phase column using a mobile phase composed of 50% acetonitrile and 50% aqueous phosphate buffer, containing triethylamine. Diode-array detection was used, operating at a wavelength of 250 nm ...
... Risperidone is currently one of the most frequently prescribed atypical antipsychotic drugs; its main active metabolite 9-hydroxyrisperidone contributes significantly to the therapeutic effects observed. An original analytical method is presented for the simultaneous analysis of risperidone and the metabolite in plasma, urine and saliva by high-performance liquid chromatography coupled to an origi ...
Adriana Maria Fernandes de Oliveira; José Maria Barbosa-Filho, et al. ; Sócrates Golzio dos Santos; Karine Formiga Queiroga; Josean Fechine Tavares; Stanley Juan Chavez Gutierrez; Margareth de Fátima Formiga Melo Diniz; Marcelo Sobral da Silva; Show all 8 Authors
... Aniba riparia (Nees) Mez. (Lauraceae) is popularly known as “louro”, and is found in Amazonia and in the Guianas, its distribution extends to the Andes. Alkamide alkaloids were isolated from its green fruit; they were denominated riparin I (methyl ether of N-benzoyl tyramine), riparin II (methyl ether of N-2-hydroxy-benzoyl tyramine) and riparin III (methyl ether of N-2,6-dihydroxy-benzoyl tyramin ...
Santoro, Maria Inês Rocha Miritello; Kedor-Hackmann, Érika Rosa Maria, et al. ; García, Pedro López; Gomes, Fabio Pereira; Quero, Jose Luis Vilchez; Montón, Alberto Navalón; Montoya, Guillermo Crovetto; Cabrera, Mercedes Aguilera; Show all 8 Authors
... Vecuronium bromide is a neuromuscular blocking agent used for anesthesia to induce skeletal muscle relaxation. HPLC and CZE analytical methods were developed and validated for the quantitative determination of vecuronium bromide. The HPLC method was achieved on an amino column (Luna 150 × 4.6 mm, 5 μm) using UV detection at 205 nm. The mobile phase was composed of acetonitrile:water containing 25. ...
Letícia Maria da Silva Cruz, et al. ; Isarita Martins; Franciely Cristiani Carreira; Larissa S. Canaes; Francisco Alberto de Souza Campos Junior; Susanne Rath; Show all 6 Authors
... Methylparaben (MePa), ethylparaben (EtPa) and propylparaben (PrPa) have been widely used, among others, as chemical preservatives in cosmetics, drugs and foods. As these compounds are linked with allergies, dermatitis and estrogenic properties, it is necessary to control the concentration of these substances in different matrices. The aim of this paper are: to evaluate the electrochemical behavior ...
Maria Fátima G. F. da Silva, et al. ; Karen C. dos Santos; João B. Fernandes; Paulo C. Vieira; Igor Polikarpov; Valtencir Zucolotto; Moacir R. Forim; Show all 7 Authors
... The objective of this work was to develop and validate a rapid Reversed-Phase High-Performance Liquid Chromatography method for the quantification of 3,5,3′-triiodothyroacetic acid (TRIAC) in nanoparticles delivery system prepared in different polymeric matrices. Special attention was given to developing a reliable reproductive technique for the pretreatment of the samples. Chromatographic runs we ...
... Here, we describe an easy field-amplified sample injection capillary electrophoresis method with UV detection for the separation and detection of free plasma arginine and dimethylated arginines. The analytes were baseline-separated within 22 min by using 50 mmol/L Tris phosphate pH 2.3 as running buffer. The plasma samples were treated with acetonitrile/ammonia for protein elimination, the superna ...
... A novel analytical approach has been developed for the determination of clozapine and its metabolites in dried blood spots on filter paper, using a chromatographic method coupled with a microextraction by packed sorbent procedure. The analytes were separated on a RP-C18 column using a mobile phase composed of 20% methanol, 16% acetonitrile and 64% aqueous phosphate buffer. Coulometric detection wa ...
... Lipases from ten different sources and two mycelium-bound lipases isolated from Amazonian fungi were screened as biocatalysts in the acylation reaction of d-ribono-1,4-lactone with a variety of acyl donors in non-aqueous media. Several reaction parameters were evaluated including the type and amount of enzyme, acyl donor, and organic solvent, as well as the influence of water and the recyclability ...
... Four cholesterol bonded phases with different structures were investigated. The columns studied were packed with stationary phase containing cholesterol attached to the silica surface using different types of linkage molecules. The presence of the polar amino and carboxyl groups in the structure of the bonded ligand strongly influence on the solvation process. The possibility of hydrogen bonding, ...
... A tritylation protocol based on the transfer of the triphenylmethylcarbenium ion from trityl acetate to substrates having hydroxyls, in the presence of catalytic amounts of ZnCl₂, is described. The advantages of this method are broad scope, mild conditions, and easy handling. The comparison with the procedure based on the use of equimolar mixture of TrCl and ZnCl₂ in the presence of TEA shows that ...
acetonitrile; aflatoxins; chromatography; hazelnuts; ionization; laws and regulations; methanol; monitoring; tandem mass spectrometry; Italy
Abstract:
... Hazelnut samples of different origin were collected in stores in Northern Italy and analysed for aflatoxin (AF) contamination by a sensitive chromatographic method on the basis of a tandem mass spectrometer with electrospray ionisation. The effects of two extracting solvent mixtures (methanol/water and acetonitrile/water) and different extraction times were tested and compared in terms of recovery ...
RNA-directed DNA polymerase; acetonitrile; antiretroviral agents; detection limit; diphenylamine; drugs; experimental design; high performance liquid chromatography; in vitro studies; nanoparticles; permeability; storage conditions
Abstract:
... Dapivirine, a non-nucleoside reverse transcriptase inhibitor, is being currently used for the development of potential anti-HIV microbicide formulations and delivery systems. A new high-performance liquid chromatography (HPLC) method with UV detection was developed for the assay of this drug in different biological matrices, namely cell lysates, receptor media from permeability experiments and hom ...
Maria Papageorgiou, et al. ; Emmanouil D. Tsochatzis; Roxani Tzimou-Tsitouridou; Urania Menkissoglu-Spiroudi; Dimitrios G. Karpouzas; Show all 5 Authors
acetonitrile; azoxystrobin; basins; deltamethrin; detection limit; ecosystems; high performance liquid chromatography; metabolites; molinate; monitoring; paddies; pesticide residues; profoxydim; propanil; rice; solid phase extraction; surface water; tricyclazole; water pollution; water quality; water resources; watersheds
Abstract:
... Rice crop is mainly cultivated in large river basins which constitute unique ecosystems and their ecological quality is invaluable. However, the high loads of pesticides used in rice cultivation contribute to the contamination of the water resources in such rice-cultivated regions. To regularly monitor the quality of such water resources there is a need for a rapid and sensitive multi-residue anal ...
... This paper reports the determination of aflatoxin B₁ (AFB₁), one of the most carcinogenic substances known. A multi-commuted flow injection–solid phase spectroscopy (FI–SPS) system combined with photochemically induced fluorescence (PIF) was developed, for the first time, for its quantitative determination. A strongly fluorescent degradation product was obtained on-line by irradiation with ultravi ...
... Alterations in the plasma aminothiols levels can be considered as important biomarkers for the diagnosis and screening of several human disorders, namely cardiovascular diseases. We aimed to optimize a rapid, sensitive and accurate RP-HPLC methodology with fluorescence detection, for the simultaneous determination of the total concentrations of cysteine, homocysteine, cysteinylglycine and glutathi ...
... Chromatographic properties of four cholesterol bonded phases with different structures were studied. The columns used were packed with a stationary phase containing a cholesterol molecule attached to the silica surface using different types of linkage molecules. Columns were compared according to the retention and separation selectivity of steroid hormones. The measurements were done using binary ...
... A quantitative liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the simultaneous analyses of malachite green (MG), crystal violet (CV) and its major metabolites, leucomalachite green (LMG) and leucocrystal violet (LCV) residues in fish and shrimp samples has been validated. Fish and shrimp samples were extracted with citrate buffer/acetonitrile, and the extracts were purified o ...
... The use of the salting-out effect in analytical chemistry is very diverse and can be applied to increase the volatility of the analytes in headspace extractions, to cause the precipitation of proteins in biological samples or to improve the recoveries in liquid–liquid extractions. In the latter, the salting-out process can be used to create a phase separation between water-miscible organic solvent ...
Maria Eliana Lopes Ribeiro de Queiroz, et al. ; Elisângela Jaqueline Magalhães; Marcus Luiz de Oliveira Penido; Marco Antônio Ribeiro Paiva; Janaína Aparecida Reis Teodoro; Rodinei Augusti; Clésia Cristina Nascentes; Show all 7 Authors
acetonitrile; cattle; cocaine; gas chromatography-mass spectrometry; humans; ionic strength; liver; overdose; pH; sodium chloride; solvents; temperature
Abstract:
... A simple and efficient method was developed for the determination of cocaine in post-mortem samples of human liver via solid–liquid extraction with low temperature partitioning (SLE–LTP) and analysis by gas chromatography coupled to mass spectrometry (GC–MS). The extraction procedure was optimized by evaluating the influence of the following variables: pH of the extract, volume and composition of ...
... A highly selective water compatible molecularly imprinted polymer (MIP) for 3-nitro-l-tyrosine (3NT), an oxidative stress marker associated with neurodegenerative disorders, was prepared and its use as solid-phase extraction (SPE) sorbent material was demonstrated. The MIP was prepared by bulk polymerization using methacrylic acid as functional monomer and acetonitrile as porogen with traces of ac ...
acetone; engineering; methanol; industry; variance; models; acetonitrile; least squares; near-infrared spectroscopy; principal component analysis; water content; distillation; spectral analysis; sulfonic acids; wavelengths; titration; gas chromatography; prediction
Abstract:
... Near-infrared spectroscopy (NIRS) in conjunction with multivariate calibration have proved to be adequate techniques to predict water content as well as methanol concentration in a industrial multicomponent mixture. The calibration models were developed using real industrial complex samples of water, methanol, and several other components in variable but lower concentrations such as sulfonic acids ...
... This work aimed to assess the influence of soil copper content on the sorption processes of thiram, a fungicide widely used in agriculture, most of the times together with copper. Two different types of studies were performed: (1) desorption studies of thiram with acetonitrile after batch adsorption equilibration, and ageing of the wet soil for a variable period of time; (2) kinetic studies of thi ...
absorption; acetonitrile; ambient temperature; geometry; solvents; spectral analysis; van der Waals forces; zwitterions
Abstract:
... A systematic theoretical and computational investigation is performed to determine the keys governing the existence, in acetonitrile solutions, of dimers of bis-tetrathiafulvalene (bis-TTF)-functionalized diphenylglycoluril molecular clips (clip₂ⁿ⁺) that are stable at room temperature for n ≤ 4. Although the experimental structure of these dimers in solution is unknown, electronic absorption studi ...
... Eight 2-phenyl-3H-imidazo[4,5-b]quinoline-9-carbonitriles 15 are prepared in four steps from N′-arylbenzamidines 11 and tetracyanoethylene (TCNE) in ∼70–90% yields. The transformation involves the initial formation of N-aryl-N′-(1,2,2-tricyanovinyl)benzamidines 12 in 87–99% yields, which in MeCN undergo a 5-exodig cyclization to give the 2-[1-aryl-5-imino-2-phenyl-1H-imidazol-4(5H)-ylidene]malonon ...
acetonitrile; bile salts; cyclodextrins; dimethyl phthalate; electrolytes; micellar electrokinetic capillary chromatography; pH; perfumes; sodium; surfactants; temperature
Abstract:
... A new CE method has been developed for the simultaneous separation of a group of parent phthalates. Due to the neutral character of these compounds, the addition of several bile salts as surfactants (sodium cholate (SC), sodium deoxycholate (SDC), sodium taurodeoxycholate (STDC), sodium taurocholate (STC)) to the separation buffer was explored showing the high potential of SDC as pseudostationary ...
... A new gradient reversed-phase HPLC method with pre-column derivatization was developed and validated for simultaneous determination of reduced glutathione, carnosine and taurine in new pharmaceutical eye drops. Chromatographic separation was achieved with a fused core analytical column Supelco Ascentis Express C18 (100 mm × 4.6 mm, 2.7 μm). A 30 mM triethylamine in acetonitrile with 30 mM triethyl ...
... Organophosphate triesters are common flame retardants used in a wide variety of consumer products from which they can migrate and pollute the indoor environment. Humans may thus be continuously exposed to several organophosphate triesters which might be a risk for human health. An analytical method based on direct injection of 5μL urine into an ultra performance liquid chromatography system couple ...
... Using combined confocal laser scanning and atomic force microscopy (CLSM/AFM), bacterial viability under organic solvent stress was assessed at single cell level. Solvent-exposed bacteria stained with the LIVE/DEAD BacLight fluoresced green or red, allowing viable and dead cell discrimination. However, with toluene, butanol and acetonitrile, dually fluorescent cells appeared having compromised cel ...
Maria da Conceição Ferreira de Oliveira; Nágila Maria Pontes Silva Ricardo, et al. ; Marcos Reinaldo da Silva; Marcos Carlos de Mattos; Telma Leda Gomes de Lemos; Gonzalo de Gonzalo; Iván Lavandera; Vicente Gotor-Fernández; Vicente Gotor; Show all 9 Authors
... Several phenylalanine analogs have been synthesized through a four-step route starting from easily available ethyl acetamidocyanoacetate. In a first reaction, and making use of phase transfer catalysts, this compound reacted with several alkyl halides, being benzyltributylammonium chloride identified as the best one for the production of a series of quaternary amino acids in moderate to excellent ...
Maria C. M. Young, et al. ; Camila M. Oliveira; Geraldo H. Silva; Luis O. Regasini; Lisinéia M. Zanardi; Alana H. Evangelista; Vanderlan S. Bolzani; Angela R. Araujo; Show all 8 Authors
... In the course of our continuous search for bioactive metabolites from endophytic fungi living in plants from the Brazilian fl ora, leaves of Alibertia macrophylla (Rubiaceae) were submitted to isolation of endophytes, and two species of Penicillium were isolated. The acetonitrile fraction obtained in corn from a culture of Penicillium sp.1 afforded orcinol (1). On the other hand, Penicillium sp.1 ...
Maria T. Matyska, et al. ; Chadin Kulsing; Yuanzhong Yang; Caesar Munera; Colby Tse; Joseph J. Pesek; Reinhard I. Boysen; Milton T.W. Hearn; Show all 8 Authors
... In this study, the zeta potentials of type-B silica, bare silica hydride, the so-called Diamond Hydride™ and phenyl substituted silica hydride stationary phases have been measured in aqueous-organic media and correction procedures developed to account for the more negative zeta potential values in media containing different acetonitrile contents. Retention studies of 16 basic, acidic and neutral c ...
... In this work, a simple methodology was developed for the determination of ethyl carbamate (EC) in spirits by high performance liquid chromatography with fluorimetric detection. The sample is subjected to salting-out assisted liquid–liquid extraction (SALLE) using a 9-xanthydrol/acetonitrile solution for the simultaneous extraction and derivatisation of EC. Extraction/derivatization occurs under ac ...
acetonitrile; desorption; detection limit; effluents; endosulfan; environmental quality; gas chromatography; ionization; mass spectrometry; mechanization; mixing; river water; screening; sodium chloride; surface water; wastewater; water policy; Spain
Abstract:
... A new analytical method has been developed for the screening, evaluation and determination of sub µg/L concentrations of chlorinated chemicals in environmental waters. Ten different compounds included in the European water policy have been considered and determined by stir bar sorptive extraction (SBSE) followed by liquid desorption and negative chemical ionization gas chromatography coupled to tr ...
... Hansen solubility parameters (HSP) aid in the a priori prediction of which low molecular weight molecules have the potential to act as low molecular weight organogelators (LMOGs) and can immobilize certain liquids. The hydrogen-bonding HSP parameter individually has some predictive capacity on whether a molecule will form a gel, solution, or precipitate in a known liquid; in the case of benzene, g ...
... A nicotine imprinted polymer was synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization using methacrylic acid (MAA) as a functional monomer. The resulting molecularly imprinted polymers were monodispersed beads with an average diameter of 1.55 μm. The molecular selectivity of the imprinted polymer beads was evaluated by studying the uptake of nicotine and its struct ...
Maria da Conceição Castilho, et al. ; Andreia Freitas; Sara Leston; João Rosa; Jorge Barbosa; Paulo Rema; Miguel Ângelo Pardal; Fernando Ramos; Show all 8 Authors
Sparus aurata; acetic acid; acetonitrile; chloramphenicol; fish culture; macrolides; maximum residue limits; muscles; penicillins; quinolones; sulfonamides; tandem mass spectrometry; tetracyclines; trimethoprim; ultra-performance liquid chromatography
Abstract:
... This paper describes a method for the determination of 41 antibiotics from seven different classes in gilthead sea bream (Sparus aurata) by ultra-high-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol were simultaneously determined. Fourteen procedures for sample treatment ...
... The use of veterinary drugs may cause the presence of residues in food of animal origin if appropriate withdrawal periods are not respected. A high-performance liquid chromatography (HPLC) method has been developed for the simultaneous detection of 11 benzimidazole residues, including metabolites – albendazole, albendazole sulphoxide, albendazole sulphone, fenbendazole, fenbendazole sulphoxide (ox ...
European Union; Sudan dyes; acetonitrile; chromatography; detection limit; quantitative analysis; sorbents; spices; statistical analysis; temperature
Abstract:
... The presented work describes the development of a simple, fast and effective on-line SPE–UHPLC–UV/vis method using fused core particle columns for extraction, separation and quantitative analysis of the nine illegal dyes, most frequently found in chilli-containing spices. The red dyes Sudan I–IV, Sudan Red 7B, Sudan Red G, Sudan Orange G, Para Red, and Methyl Red were separated and analyzed in les ...
... A simple, rapid and cost-effective sample preparation method for the determination of fumonisin B1 in rice was optimised using a strategy of sequential experimental designs. Initially, a Plackett–Burman design was applied to select the statistically significant variables for the determination of fumonisin B1, and then, a central composite rotatable design was used to define the optimal conditions ...
acetonitrile; automation; formic acid; humans; ionization; liquid chromatography; monitoring; pharmacokinetics; phospholipids; quality control; solid phase extraction; tandem mass spectrometry
Abstract:
... A semi-automated method for quantification of budesonide in human plasma was developed, validated, and applied for high-volume analysis of samples in connection with a pharmacokinetic study. Protein and phospholipid removal was performed using an Ostro 96-well filter plate and subsequently combined with C18 solid-phase extraction on a Hamilton Microlab STARlet automation robot. The final extracts ...
acetonitrile; chemical structure; herbicides; metabolites; model validation; neural networks; prediction; response surface methodology; reversed-phase high performance liquid chromatography; solutes; triazines
Abstract:
... In this paper, a multilayer artificial neural network is used to model simultaneously the effect of solute structure and eluent concentration profile on the retention of s‐triazines in reversed‐phase high‐performance liquid chromatography under linear gradient elution. The retention data of 24 triazines, including common herbicides and their metabolites, are collected under 13 different elution mo ...
... A series of hydrosilated stationary phases were compared with respect to their hydrophilic–hydrophobic properties. The stationary phases were also compared to the bare silica gel used for this synthesis. The investigations were done using microcalorimetric measurements of methanol and acetonitrile heats of immersion. Because these stationary phases are used in both the reversed-phase and aqueous n ...
... Reacting (Z)-N-(4-chloro-5H-1,2,3-dithiazol-5-ylidene)-1H-pyrazol-5-amines 5 with Et₂NH and then with concd H₂SO₄ gives 5H-pyrazolo[3,4-e][1,2,4]dithiazine-3-carbonitriles 7 in good yields (74–85%) and 6H-pyrazolo[3,4-f][1,2,3,5]trithiazepine-4-carbonitriles 9 as minor products (0–6%). Furthermore, the 1,3-dimethylpyrazole analogue 5a was transformed into the dithiazine 7a in two discrete steps, a ...
acetonitrile; air; ammonia; dielectrophoresis; electric current; electric field; electrodes; electrophoresis; nanomaterials; prototypes; temperature
Abstract:
... Interconnected network of nanostructured polyaniline (PANI) is giving strong potential for enhancing device performances than bulk PANI counterparts. For nanostructured device processing, the main challenge is to get prototypes on large area by requiring precision, low cost and high rate assembly. Among processes meeting these requests, the alternate current electric fields are often used for nano ...
... Bis(dithiolene)tungsten complexes, WⱽᴵO₂ (L = dithiolene)₂ and WᴵⱽO (L = dithiolene)₂, which mimic the active site of formate dehydrogenases, have been characterized by cyclic voltammetry and controlled potential electrolysis in acetonitrile. They are shown to be able to catalyze the electroreduction of protons into hydrogen in acidic organic media, with good Faradaic yields (75–95%) and good acti ...
... Sulfonamides are widely used in human and veterinary medicine. The presence of sulfonamides residues in food is an issue of great concern. Throughout the present work, a method for the targeted analysis of 16 sulfonamides and metabolites residue in liver of several species has been developed and validated. Extraction and clean-up has been statistically optimized using central composite design expe ...
... The aim of the current study was to optimise and validate the methodology for determination of γ‐hydroxybutyric acid (GHB) in saliva by CE combined with a contactless conductivity detector (C⁴D) and indirect UV absorbance detection (λABS = 210 nm). The optimized BGE, consisting of 8.5 mM maleic acid, 17 mM arginine, 255 μM cetyltrimethylammonium bromide (CTAB), and 15% acetonitrile, was evaluated ...
Rosa Maria De Carlo; Maria Concetta Bruzzoniti, et al. ; Luca Rivoira; Lorenzo Ciofi; Claudia Ancillotti; Leonardo Checchini; Massimo Del Bubba; Show all 7 Authors
... Seven quick, easy, cheap, effective, rugged and safe (QuEChERS)-based procedures, differing in both the extraction and clean-up steps, were investigated for the recovery of bentazone (BTZ), atrazine (ATZ), carbamazepine (CBZ), phenytoin (PNT) and its metabolite 5-(p-hydroxyphenyl-),5-phenylhydantoin (HPPH) from soil. Target analytes were chosen for their extensive use and/or occurrence in soil, as ...
Moreno-Bondi Maria C., et al. ; Benito-Peña Elena; Navarro-Villoslada Fernando; Carrasco Sergio; Jockusch Steffen; Ottaviani M. Francesca; Show all 6 Authors
... The effect of the cross-linker on the shape and size of molecular imprinted polymer (MIP) beads prepared by precipitation polymerization has been evaluated using a chemometric approach. Molecularly imprinted microspheres for the selective recognition of fluoroquinolone antimicrobials were prepared in a one-step precipitation polymerization procedure using enrofloxacin (ENR) as the template molecul ...
absorption; acetonitrile; detection limit; fish fillets; high performance liquid chromatography; liquid-liquid extraction; mackerel; malondialdehyde; pH; system optimization
Abstract:
... A rapid, specific and simple procedure is proposed for the determination of free malonaldehyde (MA) contained in fish tissue. The method is the optimization of the reaction of MA with 2,3-diaminonaphthalene to afford a naphtodiazepinium ion that present a UV absorption at 311nm, useful for MA determination by HPLC with UV detection. The reaction proceeds in the presence of 25% acetonitrile at 37°C ...
Maria Ochsenkühn-Petropoulou, et al. ; Fotios Tsopelas; Niki Malaki; Theodosia Vallianatou; Marios Chrysanthakopoulos; Demetris Vrakas; Anna Tsantili-Kakoulidou; Show all 7 Authors
... The retention behavior of sixty structurally diverse drugs on two immobilized artificial membrane (IAM) columns, IAM.PC.MG and IAM.PC.DD2 types, at two pH values, 7.4 and 5.5, was established. Extrapolated to pure aqueous phase retention factors, logkw(IAM), were determined and the role of acetonitrile as organic modifier was explored, considering the relationships with the slopes, S, of the extra ...
... Molybdenum precipitates preferentially under reducing conditions; therefore, its occurrence in sediment records is used as an indicator of paleoredox conditions. Although thiomolybdates (MoO₄–ₓSₓ²– with x = 1–4) supposedly are necessary intermediates in the process of molybdenum precipitation under anoxic conditions, there is no information about their abundance in natural environments, because of ...
... This paper describes the synthesis of novel molecularly imprinted polymers (MIPs), prepared by a noncovalent imprinting approach, for cleanup and preconcentration of curcumin (CUR) and bisdemethoxycurcumin (BDMC) from medicinal herbal extracts and further analysis by high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Two molecular mimics, a mixture of reduced BDMCs and ...
... In this study, the zeta potentials of a silica hydride stationary phase (Diamond Hydride™) in the presence of different water–acetonitrile mixtures (from 0–80% (v/v) acetonitrile) of different ionic strengths (from 0–40mM) and pH values (from pH 3.0–7.0) have been investigated. Debye–Hückel theory was applied to explain the effect of changes in the pH and ionic strength of these aqueous media on t ...
... The first CE procedure for the quantitative determination of pharmacologically relevant secoiridoids in olive oil, oleocanthal and oleacein, is described. Together with their precursors tyrosol and hydroxytyrosol they could be baseline separated in less than 15min using a borax buffer with pH 9.5, at 25kV and 30°C. Method validation confirmed that the procedure is selective, accurate (recovery rat ...
Sandra Maria Pinto, et al. ; Elisângela do Carmo Domingo; Aline Auxiliadora Tireli; Cleiton Antonio Nunes; Alexandre Vieira Batista; Mário César Guerreiro; Show all 6 Authors
... A combination of a simple pretreatment for melamine extraction and direct analysis in electrospray ionization tandem mass spectrometry (ESI–MS/MS) is proposed. Three pretreatments were evaluated. The first was based on suppressing interference using acetonitrile. The second used sulphuric acid and trichloroacetic acid to suppress interference and for melamine extraction, respectively. The third us ...
... Terephthalate-substituted thiophene derivatives are promising redox-active components for anode materials in lithium-ion batteries. In this study, we present the synthesis of substituted 2-(thiophen-3-yl)terephthalate derivatives (TTDs) as suitable monomers for thiophene-based conducting redox polymers, along with their characterization by electrochemical and spectroscopic techniques. Density func ...
Quintana Maria, et al. ; Haynes Keith M.; Perry Collin M.; Rivas Marlene; Golden Teresa D.; Bazan Antony; Nesterov Vladimir N.; Berhe Seare A.; Rodríguez Juan; Estrada Walter; Youngblood W. Justin; Show all 11 Authors
... Cuprous oxide (Cu₂O) nanorod arrays have been prepared via a novel templated electrodeposition process and were characterized for their photocatalytic behavior in nonaqueous photoelectrochemical cells. Zinc oxide (ZnO) nanorod films serve as sacrificial templates for the in situ formation of polymer nanopore membranes on transparent conductive oxide substrates. Nitrocellulose and poly(lactic acid) ...
... In the present work, a new stationary phase for disposable pipette extraction (DPX) based on composites of polyaniline and a styrene–divinylbenzene (SD) copolymer was applied to the analysis of fluoxetine and norfluoxetine in plasma samples using liquid chromatography and fluorescence detector (LC–FD).The DPX variables, such as number of draw/eject cycles, sample pH, type and volume of the desorpt ...
... The photoinduced processes of pristine and Mg²⁺-doped anatase nanopowders with the exposed {001} facets synthesized by a solvothermal method, using HF as the capping agent, were investigated by EPR spectroscopy. The adsorbed fluoride ions on the {001} facets of the as-prepared anatase samples have been removed by NaOH washing (washed samples) or calcination at 600°C (calcined samples). EPR spectra ...
Calhorda Maria José, et al. ; Cachatra Vasco; Almeida Andreia; Sardinha João; Lucas Susana D.; Gomes Ana; Vaz Pedro D.; Florêncio M. Helena; Nunes Rafael; Vila-Viçosa Diogo; Rauter Amélia P.; Show all 11 Authors
... 2-O-Acyl protected-d-ribo-3-uloses reacted with [(ethoxycarbonyl)methylene]triphenylphosphorane in acetonitrile to afford regio- and stereoselectively 2-(Z)-alkenes in 10–60 min under microwave irradiation. This domino reaction is proposed to proceed via tautomerization of 3-ulose to enol, acyl migration, tautomerization to the 3-O-acyl-2-ulose, and Wittig reaction. Alternatively, in chloroform, r ...
Maria Beatriz A. Gloria, et al. ; Letícia Rocha Guidi; Flávio Alves Santos; Ana Cláudia S.R. Ribeiro; Christian Fernandes; Luiza H.M. Silva; Show all 6 Authors
acetonitrile; aminoglycosides; aquaculture; beta-lactams; detection limit; enrofloxacin; fish; guidelines; ionization; macrolides; monitoring; screening; sulfonamides; tandem mass spectrometry; tetracyclines; trichloroacetic acid
Abstract:
... The objective of this study was to develop and validate a fast, sensitive and simple liquid chromatography–electrospray ionization-tandem mass spectrometry (LC–ESI-MS/MS) method for the screening of six classes of antibiotics (aminoglycosides, beta-lactams, macrolides, quinolones, sulfonamides and tetracyclines) in fish. Samples were extracted with trichloroacetic acid. LC separation was achieved ...
Isabela Maria Campos Tavares, et al. ; Mariane Gonçalves Santos; Adriano Francisco Barbosa; Jefferson Bettini; Eduardo Costa Figueiredo; Show all 5 Authors
... The use of a new class of hybrid materials, called restricted access molecularly imprinted polymers (RAMIPs) seems to present a good strategy for the sample preparation of complex matrices, since these materials combine good protein elimination capacity with high degree selectivity. Mass spectrometers (MS) have been successfully used for polar drug identification and quantification. In order to co ...
acetonitrile; detection limit; drugs; humans; liquid chromatography; metabolites; rivers; sediments; solid phase extraction; solvents; statistical analysis; tandem mass spectrometry
Abstract:
... An analytical method based on a modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction procedure followed by ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) was developed for the analysis of psychiatric drugs in sediments. An optimized approach was applied in sample preparation by using basic acetonitrile as extraction solvent. Extraction ...
... A reliable and simple method for the detection and quantification of residues of 14 non-steroidal anti-inflammatory drugs and a metamizole metabolite in swine muscle was developed using liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The samples were extracted with acetonitrile (ACN) in solid–liquid extraction followed by a low-temperature partitioning (LLE-L ...
... A conducting redox polymer (CPR) based on pyrrole with a hydroquinone pendant group was synthesized through electropolymerization of the corresponding monomer. The formal potential (E⁰′) in aqueous solution at different pH as well as in MeCN containing equal amounts of pyridinium-triflates and the corresponding free pyridine with different pKₐ was investigated. E⁰′ could be completely recovered in ...
Maria Angela de Almeida Meireles, et al. ; J. Felipe Osorio-Tobón; Pedro I.N. Carvalho; Gerardo Fernández Barbero; Gislaine Chrystina Nogueira; Mauricio Ariel Rostagno; Show all 6 Authors
... The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast method for the analysis of main curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) present in extracts of turmeric (Curcuma longa L.). A step-by-step strategy was used to optimize temperature (40–55°C), flo ...
Maria D. Rodriguez, et al. ; Laura Fernandez-Lopez; Nazzoly Rueda; Rocio Bartolome-Cabrero; Tiago L. Albuquerque; Jose C.S. dos Santos; Oveimar Barbosa; Roberto Fernandez-Lafuente; Show all 8 Authors
... A strategy to stabilize octyl (OC)-Rhizomucor miehei lipase (RML) and OC-Candida rugosa lipase (CRL) at pH 10 is necessary to take full advantage of the immobilization of these enzymes on OC-glyoxyl (OCGLX) supports. CaCl2 and MnCl2 have been reported to stabilize OC-RM and OC-CRL at pH 5.0 and 7.0. After screening different buffers, 5mM CaCl2 was found to be fully soluble in Gly at pH 10. OC-RML ...
... In this work the development and in house validation of the HMF direct determination in corn and cane syrups by HPLC–UV was carried out for the first time. The separation was done with isocratic elution of a mobile phase comprising water (with 0.5% formic acid) and acetonitrile (90:10, v/v) on Phenomenex C18 column (5.0μm, 4.6×150mm), at 30°C, flow rate of 0.8mLmin−1 and detection at 285nm. The va ...
Maria A. Chiacchio, et al. ; Ugo Chiacchio; Gianluigi Broggini; Roberto Romeo; Silvia Gazzola; Salvatore V. Giofrè; Bartolo Gabriele; Raffaella Mancuso; Giuseppe Floresta; Chiara Zagni; Show all 10 Authors
... A palladium-catalyzed diamination domino process of sulfamates arising from glycine allylamides is reported. The reaction leads to the formation of [1,2,5]thiadiazolo-fused piperazinones. The essential feature of the synthetic route is the use of PdCl₂(MeCN)₂/CuBr₂, as a catalytic system which promotes the second amination process, leading to the bicycle ring-fused compounds in good yields. ...
Maria T. Matyska, et al. ; Chadin Kulsing; Yuanzhong Yang; Roshanak Sepehrifar; Michael Lim; Joshua Toppete; Joseph J. Pesek; Reinhard I. Boysen; Milton T.W. Hearn; Show all 9 Authors
... In this study, the surface charge properties of perfluorinated C8 (PerfluoroC8) and undecanoic acid (UDA) modified silica hydride stationary phases have been investigated. The zeta potential values of these stationary phases were measured in aqueous/acetonitrile mobile phases of different pH, buffer concentrations and acetonitrile contents. The retention behaviour of several basic, acidic and neut ...
acetonitrile; drugs; gases; heterocyclic amines; ionization; ions; levamisole; methanol; monitoring; solvents; spectrometers; tandem mass spectrometry
Abstract:
... Nowadays most LC-MS methods rely on tandem mass spectrometry not only for quantitation and confirmation of compounds by multiple reaction monitoring (MRM), but also for the identification of unknowns from their product ion spectra. However, gas-phase reactions between charged and neutral species inside the mass analyzer can occur, yielding product ions at m/z values higher than that of the precurs ...
... The effect of ionic liquid electrolytes on back electron-transfer rates for dye-sensitized TiO₂ thin films was investigated using microsecond–millisecond transient absorption. For D35/TiO₂ and [Ru(dcb)₃]²⁺/TiO₂ in electrolytes based on 1-alkyl-3-methyl-imidazolium hexafluorophosphate, significantly slower back electron-transfer rates, compared to those observed in neat acetonitrile (CH₃CN) and LiC ...
Anny Talita Maria da Silva, et al. ; Hanna Leijoto de Oliveira; Sara da Silva Anacleto; Arnaldo César Pereira; Warley de Souza Borges; Eduardo Costa Figueiredo; Keyller Bastos Borges; Show all 7 Authors
... A simple method using HPLC-DAD was developed for the determination of fluoroquinolones in human urine including ciprofloxacin (CIPRO), enrofloxacino (ENRO), marbofloxacino (MARBO) and norfloxacin (NOR). In addition, it was studied the extraction of fluoroquinolones in human urine samples using pipette tip-based molecularly imprinted polymers solid phase extraction (PT-MIPs-SPE). With the goal of f ...
... A simple and reliable high‐performance liquid chromatography method was developed and validated for the simultaneous determination of lipophilic antioxidants in tomato fruits using C₃₀ column operated at 15°C and a gradient mobile phase based on acetonitrile/methanol/dichloromethane in a total run time of 30 min. Diode array and fluorescence detectors were used respectively for the detection of ca ...
... A simple, sensitive and accurate analytical method was optimized and developed for the determination of deoxynivalenol and aflatoxins in cereals intended for human consumption using high‐performance liquid chromatography with diode array and fluorescence detection and a photochemical reactor for enhanced detection. A response surface methodology, using a fractional central composite design, was ca ...
absorption; acetonitrile; catalytic activity; color; electron transfer; electrons; energy; ligands; moieties; oxygen; paraquat; photolysis; ruthenium; singlet oxygen; spectroscopy; triethylamine
Abstract:
... The [Ru(II) (phen)₂(pPDIp)]²⁺ complex, where pPDIp is the symmetric bridging ligand phenanthroline–perylene–phenanthroline, shows strong electronic absorption bands attributed to the pPDIp and {Ru(phen)₂}²⁺ moieties in acetonitrile. The charge-separated intermediate {Ru(III) (phen)₂(pPDIp–•)} was detected by transient absorption spectroscopy upon electronic excitation in either the pPDIp or the co ...
... Sophorolipids (SLs) were produced by Starmerella bombicola. The separation and purification of SLs are a complex process, since they are produced as a mixture of compounds with few structural differences. Solvent extraction is commonly used in downstream processing. In this work, an environmental friendly approach was developed for SLs recovery and purification, based on neutral polymeric sorbents ...
acetonitrile; ammonium acetate; cannabidiol; drugs; forensic sciences; guidelines; humans; ionization; liquid chromatography; metabolites; methanol; monitoring; tandem mass spectrometry; toxicology; urine
Abstract:
... A comprehensive cannabinoid urine quantification method may improve clinical and forensic result interpretation and is necessary to support our clinical research. A liquid chromatography tandem mass spectrometry quantification method for ∆⁹-tetrahydrocannabinol (THC), 11-hydroxy-THC (11-OH-THC), 11-nor-9-carboxy-THC (THCCOOH), ∆⁹-tetrahydrocannabinolic acid (THCAA), cannabinol (CBN), cannabidiol ( ...
... A series of phenyl‐bonded stationary phases with incorporated polar functional groups was subjected to an adsorption investigation. Measurement of acetonitrile and methanol adsorption was obtained using the minor disturbance method. It was observed that adsorption of organic solvent strongly depends on the presence of polar functional groups in the bonded phases that influence the hydrophobicity a ...
Maria Grazia Di Milia, et al. ; Elisabetta Bertol; Jennifer Pascali; Diego Palumbo; Valeria Catalani; Alessia Fioravanti; Francesco Mari; Fabio Vaiano; Show all 8 Authors
... 3-MeO-PCP or 3-methoxyphencyclidine is a derivative of phencyclidine. It acts as a dissociative anesthetic and it has allegedly hallucinogenic and sedative effects. There are almost no documented intoxication cases and references about its pharmacology and toxicity in literature. This study presents two concomitant intoxication cases due to consumption of 3-MeO-PCP and alcohol. A 19 (A) and a 21 y ...
European Union; HT-2 toxin; acetonitrile; aflatoxins; deoxynivalenol; detection limit; fumonisins; grains; laws and regulations; monitoring; nuts; ochratoxin A; tandem mass spectrometry; ultra-performance liquid chromatography; zearalenone; Cyprus
Abstract:
... The validation of a rapid, reliable and sensitive method for the simultaneous determination of Aflatoxins, Ochratoxin A, Zearalenone, Deoxynivalenol, Fumonisins, T-2 and HT-2 toxins, in nuts and cereals is reported. This method is based on a single extraction step using an acetonitrile/water mixture followed by the analysis of the diluted crude extract using ultra high-performance liquid chromatog ...
Luca Maria Chiesa, et al. ; Giuseppe Federico Labella; Sara Panseri; Domenico Britti; Fabrizio Galbiati; Roberto Villa; Francesco Arioli; Show all 7 Authors
European Union; acetonitrile; guidelines; honey; honey bee colonies; mass spectrometry; multiresidue analysis; pesticide residues; pesticides; solvents
Abstract:
... The worldwide loss of honeybee colonies may be due to their exposure to several contaminants (i.e., pesticides); such contamination may also have impacts on consumers’ health. Therefore, it is essential to develop quick and new methods to detect several pesticide residues in honey samples. In this study, the effectiveness of accelerated solvent extraction (ASE) was compared with QuEChERS methods f ...
Angela Maria Palacio-Cortés, et al. ; Aurora L. Carreño Otero; Mario Antonio Navarro-Silva; Vladimir V. Kouznetsov; Jonny E. Duque L.; Show all 5 Authors
... Because mosquito control depend on the use of commercial insecticides and resistance has been described in some of them, there is a need to explore new molecules no resistant. In vivo effects of girgensohnine analog 2-(3,4-dimethoxyphenyl)-2-(piperidin-1-yl)acetonitrile DPPA and Cymbopogon flexuosus essential oil CFEO, on the detoxifying enzymes acetylcholinesterase (AChE), glutathione-S-transfera ...
Maria Heloísa Paulino de Moraes, et al. ; André Victor Sartori; Rosana Pereira dos Santos; Yuri Pereira Souza; Armi Wanderley da Nóbrega; Show all 5 Authors
acetonitrile; aflatoxins; deoxynivalenol; formic acid; fumonisins; laws and regulations; liquid chromatography; ochratoxin A; solvents; sonication; statistical analysis; sterigmatocystin; tandem mass spectrometry; zearalenone; Brazil
Abstract:
... An analytical method applying ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the determination of aflatoxins M2, M1, G2, G1, B2, B1, deoxynivalenol, ochratoxin A, fumonisins B1 and B2, hydrolyzed fumonisins B1 and B2, zearalenone and sterigmatocystin in cereal-based porridge destined for infant consumption was developed and validated. The mycotoxins were ex ...
Anna Maria Sulej-Suchomska, et al. ; Agnieszka Klupczynska; Hanna Piotrowska-Kempisty; Marcin Wierzchowski; Jadwiga Jodynis-Liebert; Zenon J. Kokot; Show all 6 Authors
... The synthetic resveratrol analogue DMU-212 (3,4,4′,5-tetramethoxystilbene) has been shown to possess stronger anticancer activity than resveratrol in a variety of tumour cells. To date, there has been no appropriate procedure that would ensure a reliable data about levels of metabolic products of DMU-212 in cancer cell lines. The purpose of this study was to develop a new procedure for determinati ...