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1.
J Chromatogr A ; 1627: 461395, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823100

RESUMO

Nowadays, enantioseparation of racemic pharmaceuticals in preparations is a prime concern by drug authorities across the globe. In the present work, it was attempted to develop novel enantioselective extraction method for five clinically used drugs (atenolol, propranolol, metoprolol, racecadotril, and raceanisodamine in their tablets) as racemates. The enantioselective solid-liquid extraction of these racemic drugs was carried out successfully by the use of chiral ionic liquid (CIL) in combination with a metal organic framework (MOF) for the first time. The composite CIL@MOF was synthesized from tropine based chiral ionic liquids with L-proline anion ([CnTr][L-Pro], n=3-6) and HKUST-1 type MOF, which was comprehensively characterized before being used as sorbent for enantioselective dispersive solid-liquid extraction. Preliminary selection of appropriate CIL was carried out on thin layer chromatography (TLC); under the joint participation of copper ion in the developing reagent, [C3Tr][L-Pro] ionic liquid showed better resolution performance with ΔRf value of 0.35 between the enantiomers was obtained for racemic atenolol. Moreover, the effect of copper salt dosage, amount of CIL, soli-liquid ratio and extraction time were investigated. The optimal conditions were obtained after thorough investigations; i.e. sample solution: ethanol, elution solvent: methanol, solid-liquid ratio: 12.5 mg:50 mL, amount of copper salt: 8 mg L-1, amount of impregnated CIL: 30% and extraction time of 30 min. As a result, enantiomeric excess values are 90.4%, 95%, 92%, 81.6% and 83.2% for atenolol, propranolol, metoprolol, racecadotril and raceanisodamine, respectively. The developed enantioselective method was validated following ICH guidelines and it was proved to be simple, effective and enantioselective way for separation of racemic pharmaceuticals with similar behaviors.


Assuntos
Líquidos Iônicos/química , Estruturas Metalorgânicas/química , Preparações Farmacêuticas/isolamento & purificação , Extração em Fase Sólida/métodos , Antagonistas Adrenérgicos beta/análise , Antagonistas Adrenérgicos beta/isolamento & purificação , Atenolol/análise , Atenolol/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Cobre/química , Metoprolol/análise , Metoprolol/isolamento & purificação , Preparações Farmacêuticas/análise , Propranolol/análise , Propranolol/isolamento & purificação , Solventes/química , Estereoisomerismo
2.
J Chromatogr A ; 1627: 461420, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823115

RESUMO

Monitoring preparative protein chromatographic steps by in-line spectroscopic tools or fraction analytics results in medium or large sized data matrices. Multivariate Curve Resolution (MCR) serve to compute or to estimate the concentration values of the pure components only from these data matrices. However, MCR methods often suffer from an inherent solution ambiguity which underlies the factorization problem. The typical unimodality of the chromatographic profiles of pure components can support the chemometric analysis. Here we present the pure components estimation process within the framework of the area of feasible solutions, which is a systematic approach to represent the range of all possible solutions. The unimodality constraint in combination with Pareto optimization is shown to be an effective method for the pure component calculation. Applications are presented for chromatograms on a model protein mixture containing ribonuclease A, cytochrome c and lysozyme and on a two-dimensional chromatographic separation of a monoclonal antibody from its aggregate species. The root mean squared errors of the first case study are 0.0373, 0.0529 and 0.0380 g/L compared to traditional off-line analytics. The second case study illustrates the potential of recovering hidden components with MCR from off-line reference analytics.


Assuntos
Produtos Biológicos/análise , Cromatografia/métodos , Preparações Farmacêuticas/análise , Anticorpos Monoclonais/isolamento & purificação , Estudos de Viabilidade , Análise dos Mínimos Quadrados , Análise Multivariada , Proteínas/isolamento & purificação , Reprodutibilidade dos Testes
3.
J Chromatogr A ; 1625: 461277, 2020 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-32709329

RESUMO

The influence of impregnation the chromatographic plate adsorbent layer, silica, with hen's egg white albumin (OVA) or bovine serum albumin (BSA) on the retention of some popular medicines (paracetamol, aminophenazone, theophylline, caffeine, acetanilide, ciprofloxacin, tramadol, acetylsalicylic acid, acebutolol) is investigated. The effect of composition and buffer pH of the mobile phase on solute separation selectivity is also studied. The chromatographic systems with and without above mentioned albumins and their influence on investigated drug retention are compared. In general, it has been turned out that retention of tested medicines in systems with the sorbent impregnated with albumin significantly increase relative to those with non-impregnated.


Assuntos
Cromatografia em Camada Delgada/métodos , Clara de Ovo/química , Preparações Farmacêuticas/análise , Soroalbumina Bovina/química , Sílica Gel/química , Adsorção , Animais , Bovinos , Galinhas , Feminino , Concentração de Íons de Hidrogênio , Metanol/química , Compostos Orgânicos/química , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier , Tolueno/química
4.
Artigo em Inglês | MEDLINE | ID: mdl-32640873

RESUMO

Each year, large amounts of plastic waste are generated and must be appropriately disposed. In this work, we studied the feasibility of using plastics as wetland substrates as an alternative plastic waste disposal method and the ability of the constructed wetland to remove pharmaceuticals and personal care products (PPCPs) from contaminated water. Wetland microcosms were constructed using polycarbonate, polyethylene terephthalate, quartz sand, and ceramsite substrates. Lake water spiked with methyl-paraben, ibuprofen, triclosan, 4-methybenzylidene camphor, carbamazepine, and 17α-ethinyl estradiol at 5 µg L-1 was continuously loaded to the microcosms with a hydraulic retention time of approximately 11 days. After 70 days, methyl-paraben, triclosan, and 4-methybenzylidene camphor were effectively removed regardless of the substrate. However, ibuprofen, carbamazepine, and 17α-ethinyl estradiol were partially removed, and the removal efficiency was the best in wetlands with ceramsite substrate. Carbamazepine was the most persistent among the tested compounds. Phospholipid fatty acid (PLFA) analysis revealed that ceramsite supported the highest microbial biomass per bulk volume of substrate followed by quartz sand, polycarbonate, and polyethylene terephthalate, which might be related to the PPCP removal potential of the wetland microcosms.


Assuntos
Cosméticos/análise , Preparações Farmacêuticas/análise , Plásticos/química , Resíduos Sólidos , Poluentes Químicos da Água/análise , Purificação da Água/métodos , Áreas Alagadas , China , Estudos de Viabilidade , Água Doce/microbiologia
5.
J Chromatogr A ; 1624: 461218, 2020 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-32540066

RESUMO

In this study, amylose- and cellulose-phenylcarbamate-based chiral columns with different chiral-selector (CS) chemistries were compared to each other for the separation of enantiomers of basic chiral analytes in acetonitrile and aqueous-acetonitrile mobile phases in HPLC. For two chemistries the amylose-based columns with coated and immobilized CSs were also compared. The comparison of CSs containing only electron-donating or electron-withdrawing substituents with those containing both electron-donating and electron-withdrawing substituents showed opposite results for the studied set of chiral analytes in the case of amylose and cellulose derivatives. Along with the chemistry of CS the focus was on the behavior of polysaccharide phenylcarbamates in acetonitrile versus aqueous acetonitrile as eluents. In agreement with earlier results, it was found that in contrast to the commonly accepted view, polysaccharide phenylcarbamates do not behave as typical reversed-phase materials for basic analytes either. In the range of water content in the mobile phase of up to 20-30% v/v the behavior of these CSs is similar to hydrophilic interaction liquid chromatography (HILIC)-type adsorbents. This means that with increasing water content in the mobile phase up to 20-30% v/v, the retention of analytes mostly decreases. The important finding of this study is that the separation efficiency improves for most analytes when switching from pure acetonitrile to aqueous acetonitrile. Therefore, in spite of reduced retention, the separation of enantiomers improves and thus, the HILIC-range of mobile phase composition, offering shorter analysis time and better peak resolution, is advantageous over pure polar-organic solvent mode. Interesting examples of enantiomer elution order (EEO) reversal were observed for some analytes based on the content of water in the mobile phase on Lux Cellulose-1 and Lux Amylose-2 columns.


Assuntos
Amilose/química , Celulose/química , Cromatografia Líquida de Alta Pressão/métodos , Preparações Farmacêuticas/isolamento & purificação , Fenilcarbamatos/química , Acetonitrilos/química , Elétrons , Etanolaminas/análise , Etanolaminas/isolamento & purificação , Preparações Farmacêuticas/análise , Propanolaminas/análise , Propanolaminas/isolamento & purificação , Propranolol/análise , Propranolol/isolamento & purificação , Estereoisomerismo , Água/química
6.
Artigo em Inglês | MEDLINE | ID: mdl-32517338

RESUMO

Pharmaceuticals are emerging contaminants in the aquatic environments. Their presence poses toxicological effects in humans and animals even at trace concentrations. This study investigated the presence of antibiotics, anti-epilepsy and anti-inflammatory drugs in river water of selected rivers in the Eastern Cape Province in South Africa. Enzyme-linked immunosorbent assay was used for screening of sulfamethoxazole and fluoroquinolones antibiotics. The samples were collected in upper-stream, middle-stream and lower-stream regions of the rivers and effluent of selected wastewater treatment plants. Pre-concentration of the samples was conducted using lyophilisation and extraction was conducted using solid phase extraction (SPE) on Waters Oasis hydrophilic-lipophilic-balanced cartridge. The percentage recovery after sample clean-up on SPE was 103% ± 6.9%. This was followed by ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry. The detected analytes were sulfamethoxazole, erythromycin, clarithromycin and carbamazepine. Carbamazepine and erythromycin were detected in high concentrations ranging from 81.8 to 36,576.2 ng/L and 11.2 to 11,800 ng/L respectively, while clarithromycin and sulfamethoxazole were detected at moderate concentrations ranging from 4.8 to 3280.4 ng/L and 6.6 to 6968 ng/L, respectively. High concentrations of pharmaceuticals were detected on the lower-stream sites as compared to upper-stream sites.


Assuntos
Preparações Farmacêuticas , Poluentes Químicos da Água , Animais , Cromatografia Líquida , Monitoramento Ambiental , Humanos , Preparações Farmacêuticas/análise , Rios , Extração em Fase Sólida , África do Sul , Poluentes Químicos da Água/análise
7.
J Chromatogr A ; 1623: 461171, 2020 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-32505277

RESUMO

A novel disposable styrene based solid-phase microextraction (SPME) fiber was synthesized for the detection of lipid-lowering and antihypertensive drugs in real aquatic environment. Styrene and poly(ethylene glycol) diacrylate were co-polymerized on quartz fibers by thermal polymerization in capillary molds. The polymeric fiber possessed a homogeneous, dense as well as porous surface, showing excellent chemical and mechanical stability. The performance of the fiber was evaluated through the extraction of seven pharmaceuticals by coupling SPME with high performance liquid chromatography-tandem mass spectrometry under the optimized extraction conditions. The extraction efficiency of the fiber was up to 278 times of PDMS fiber and the enrichment factors ranged from 55 to 1183. The limits of detection were in the range from 1.7 ng L-1 to 11.7 ng L-1, with good reproducibility. Moreover, the fiber was used in the real water samples of the Pearl River Delta. The recoveries of the target analytes from river water and sea water samples at different spiked concentrations were in the range from 84.1% to 133.4% and from 81.5% to 105.5%, respectively.


Assuntos
Preparações Farmacêuticas/análise , Microextração em Fase Sólida/métodos , Poluentes Químicos da Água/análise , Cromatografia Líquida de Alta Pressão , Preparações Farmacêuticas/isolamento & purificação , Polietilenoglicóis/química , Polimerização , Reprodutibilidade dos Testes , Rios/química , Água do Mar/química , Estireno/química , Espectrometria de Massas em Tandem , Poluentes Químicos da Água/isolamento & purificação
8.
Chemosphere ; 258: 127273, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32554005

RESUMO

This work describes the design, optimization and validation of an analytical method for the simultaneous determination of 14 pharmaceuticals and personal care products (PPCPs) in sewage sludge. A thorough optimization of the sample pre-treatment was carried out. As a result, microwave-assisted extraction (MAE) was combined with an in-situ clean-up stage and a filtration step. A combination of MilliQ® water/MeOH 95:5 (v/v) adjusted to pH 9 turned out to be the optimal solvent mixture for extraction. The instrumental part of the method presents a significant novelty based on a fully automated sample preparation for the analysis of PPCPs. It consisted of a direct immersion solid phase microextraction followed by on-fiber derivatization, online coupled to gas chromatography - mass spectrometry (DI-SPME-On-fiber derivatization - GC-MS). An isotope dilution approach was used for quantifying, which conferred high reliability to the method. This methodology was validated for 10 compounds with good analytical performance, limit of detection below 20 ng g-1 and absolute recovery in the range of 30-70% for most of the compounds. It supposes an ecological analytical alternative for many routine analysis laboratories around the world. The developed method was applied to different real samples generated in both a pilot-scale thermal hydrolysis treatment plant and an anaerobic digester operated in mesophilic conditions. Salicylic acid and naproxen were found at concentrations above 1000 ng g-1.


Assuntos
Cosméticos/análise , Micro-Ondas , Preparações Farmacêuticas/análise , Esgotos/química , Solventes/química , Poluentes Químicos da Água/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Metanol/química , Reprodutibilidade dos Testes , Microextração em Fase Sólida/métodos , Água/química
9.
An Acad Bras Cienc ; 92(1): e20181021, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32401841

RESUMO

Fosamprenavir calcium is an amprenavir prodrug of the protease inhibitors class used in the treatment of patients with acquired immunodeficiency syndrome (AIDS). Different solid forms of this drug are described in patents, in this sense studies on the physico-chemical characterization and stability are relevant for the selection of a solid form with adequate features for pharmaceutical purposes. In the present work form I (commercial) and amorphous of fosamprenavir calcium were characterized by the techniques of Differential Scanning Calorimetry (DSC), Thermogravimetry (TGA), Powder X-ray Diffraction (PXRD), Fourier-Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). Furthermore, the chemical and polymorphic stability of the commercial form were evaluated by DSC, PXRD, FTIR and High-Performance Liquid Chromatography (HPLC). In the studies of characterization, thermal analyses allied to spectroscopic methods (PXRD and FTIR) demonstrated that the presence of water in the crystalline structure of Form I is fundamental for maintaining its crystallinity. In studies of accelerated stability the techniques of DSC, PXRD and FTIR showed that Form I does not suffer phase change when submitted to controlled conditions of temperature and humidity. Moreover, HPLC and FTIR proved the chemical stability of this solid form of fosamprenavir, thus demonstrating its suitability for pharmaceutical purposes.


Assuntos
Carbamatos/química , Organofosfatos/química , Preparações Farmacêuticas/análise , Sulfonamidas/química , Tecnologia Farmacêutica/métodos , Umidade , Microscopia Eletrônica de Varredura , Análise Espectral/métodos , Temperatura , Termodinâmica
10.
Aquat Toxicol ; 224: 105499, 2020 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-32416570

RESUMO

Pharmaceutical substances are ubiquitous in the aquatic environment and their concentration levels typically range from ng/L up to several µg/L. Furthermore, as those compounds are designed to be highly biologically active, assessing their impacts on non-target organisms is important. Here, we conducted a mesocosm experiment testing a mixture of five pharmaceuticals (diclofenac, carbamazepine, irbesartan, acetaminophen and naproxen) on fish, three-spined stickleback (Gasterosteus aculeatus). The mixture concentration levels were chosen on the basis of the contamination of the Meuse river in Belgium which had been measured previously during a monitoring campaign undertaken in 2015 and 2016. Three nominal mixture concentration levels were tested: the lowest concentration level mixture was composed by environmentally-relevant concentrations that approximate average realistic values for each pharmaceuticals (Mx1); the two other levels were 10 and 100 times these concentrations. Although no impact on stickleback prey was observed, the mixture significantly impaired the survival of female fish introduced in the mesocosms at the highest treatment level without causing other major differences on fish population structure. Impacts on condition factors of adults and juveniles were also observed at both individual and population levels. Using a modelling approach with an individual-based model coupled to a bioenergetic model (DEB-IBM), we concluded that chronic exposure to environmentally-relevant concentrations of five pharmaceuticals often detected in the rivers did not appear to strongly affect the three-spined stickleback populations. Mechanisms of population regulation may have counteracted the mixture impacts in the mesocosms.


Assuntos
Preparações Farmacêuticas/análise , Rios/química , Smegmamorpha/crescimento & desenvolvimento , Poluentes Químicos da Água/toxicidade , Acetaminofen/análise , Acetaminofen/toxicidade , Animais , Bélgica , Carbamazepina/análise , Carbamazepina/toxicidade , Diclofenaco/análise , Diclofenaco/toxicidade , Feminino , Modelos Teóricos , Naproxeno/análise , Naproxeno/toxicidade , Dinâmica Populacional , Smegmamorpha/fisiologia , Poluentes Químicos da Água/análise
11.
Chemosphere ; 256: 127002, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32445997

RESUMO

Pharmaceuticals and personal care products (PPCPs) has been of concerns for their potential threats to ecosystems and human's health for decades. PPCPs have been detected in water environments worldwide and have been identified in water sources and finished water. To elucidate the potential exposure of PPCPs in drinking water, this study assessed the occurrences and treatment efficiencies of PPCPs in the drinking water of Taiwan. Raw and finished water samples collected from five main drinking water treatment plants (DWTPs) in February, June, and November 2018 were analyzed. Furthermore, laboratory-scale water treatment processes were conducted to evaluate the treatment efficiencies of these chemicals. Most of the water samples from the DWTPs had a low concentration (<30 ng/L) of PPCPs. Only samples from a DWTP was observed to have higher concentration of ibuprofen (55.6 ng/L), benzophenone (92.5 ng/L), caffeine (390.5 ng/L), and diethyltoluamide (DEET) (434.9 ng/L) in raw water than others. The results of laboratory simulations indicated that the pre-chlorination process was the key step responsible for the removal of PPCPs in conventional water treatment processes, which can remove most of the hormone treatment products, parabens, oxybenzone, and acetaminophen in water sources. However, the filtration process with anthracite as a medium could remove some of the parabens (approximately 11.9%-41.2%), hormones (approximately 18.2%-44.8%), suntan lotions (37.5%-68.8%), and naproxen (30.1%) from Milli-Q water. The removal efficiencies of the aforementioned chemicals were marginally lower in raw water. However, analgesics, caffeine, and DEET cannot be removed effectively through conventional drinking water treatment.


Assuntos
Cosméticos/análise , Água Potável/química , Monitoramento Ambiental , Poluentes Químicos da Água/análise , Benzofenonas , Ecossistema , Humanos , Preparações Farmacêuticas/análise , Taiwan , Purificação da Água/métodos
12.
BMC Bioinformatics ; 21(1): 183, 2020 May 11.
Artigo em Inglês | MEDLINE | ID: mdl-32393166

RESUMO

BACKGROUND: Even though R is one of the most commonly used statistical computing environments, it lacks a graphical user interface (GUI) that appeals to students, researchers, lecturers, and practitioners in medicine and pharmacy for conducting standard data analytics. Current GUIs built on top of R, such as EZR and R-Commander, aim to facilitate R coding and visualization, but most of the functionalities are still accessed through a command-line interface (CLI). To assist practitioners of medicine and pharmacy and researchers to run most routines in fundamental statistical analysis, we developed an interactive GUI; i.e., MEPHAS, to support various web-based systems that are accessible from laptops, workstations, or tablets, under Windows, macOS (and IOS), or Linux. In addition to fundamental statistical analysis, advanced statistics such as the extended Cox regression and dimensional analyses including partial least squares regression (PLS-R) and sparse partial least squares regression (SPLS-R), are also available in MEPHAS. RESULTS: MEPHAS is a web-based GUI (https://alain003.phs.osaka-u.ac.jp/mephas/) that is based on a shiny framework. We also created the corresponding R package mephas (https://mephas.github.io/). Thus far, MEPHAS has supported four categories of statistics, including probability, hypothesis testing, regression models, and dimensional analyses. Instructions and help menus were accessible during the entire analytical process via the web-based GUI, particularly advanced dimensional data analysis that required much explanation. The GUI was designed to be intuitive for non-technical users to perform various statistical functions, e.g., managing data, customizing plots, setting parameters, and monitoring real-time results, without any R coding from users. All generated graphs can be saved to local machines, and tables can be downloaded as CSV files. CONCLUSION: MEPHAS is a free and open-source web-interactive GUI that was designed to support statistical data analyses and prediction for medical and pharmaceutical practitioners and researchers. It enables various medical and pharmaceutical statistical analyses through interactive parameter settings and dynamic visualization of the results.


Assuntos
Preparações Farmacêuticas/análise , Software , Estatística como Assunto , Interface Usuário-Computador , Ciclo Celular , Bases de Dados como Assunto , Humanos , Probabilidade , Saccharomyces cerevisiae/citologia
13.
Food Chem ; 322: 126765, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32311620

RESUMO

An efficient and sensitive analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated for the simultaneous determination of 42 pharmaceuticals belonging to different therapeutic classes (i.e. antibiotics, analgesics, anti-inflammatories, cardiovascular agents, anxiolytics and human indicators) in seafood samples. The very simple sample preparation included analytes extraction with acidified methanol, concentration by evaporation and filtration of the final extract prior to LC-MS/MS analysis. Analytical performances were evaluated in muscles of four commercial species (hake, red mullet, sole and shrimp) and showed good recoveries at two spiked concentration levels, with relative standard deviations below 45%. Limits of quantification ranged from 0.1 to 40.2 ng/g. This procedure has been successfully applied to the determination of the target analytes in seafood collected from the Bay of Biscay (Southern France) and 4 of these 42 pharmaceuticals were detected at low ng/g levels, suggesting a very limited contamination.


Assuntos
Cromatografia Líquida/métodos , Contaminação de Alimentos/análise , Preparações Farmacêuticas/análise , Alimentos Marinhos/análise , Espectrometria de Massas em Tandem/métodos , Fracionamento Químico/métodos , Análise de Alimentos/métodos , França , Músculos/química , Solventes , Poluentes Químicos da Água/análise
14.
Mar Pollut Bull ; 153: 111014, 2020 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-32275560

RESUMO

The detection rates of pharmaceuticals (Ps), personal care products (PCPs), current-use pesticides (CUPs) and a food additive (FA) in Brisbane River estuary (Queensland), Sydney estuary (New South Wales) and the Yarra River estuary (Melbourne, Victoria) were: Ps: 16/25, 7/25 and 12/25, respectively, CUPs; 28/53, 5/53 and 23/53, respectively, PCPs: 1/3, 0/3 and, 1/3, respectively and FA; 1/1, 1/1 and 1/1, respectively. Diuron was measured in all estuarine samples, simazine, MCPA and 2,4 D were also commonly measured. Pharmaceuticals: carbamazepine, iopromide paracetamol tramadol and venlafaxine were also commonly measured across the estuaries. Generally, analytes were prominent in Brisbane River estuary, followed by Yarra River/Sydney estuary. Inputs of Ps are likely from leakages or effluents of WWTPs; CUPs are potentially from agricultural and parklands via surface run-off in Brisbane River estuary, while for Sydney and Yarra estuaries, which have separate stormwater and sewer systems, sources are likely to be ingression and leakage.


Assuntos
Cosméticos , Monitoramento Ambiental , Praguicidas , Preparações Farmacêuticas/análise , Poluentes Químicos da Água , Austrália , Estuários , Aditivos Alimentares , New South Wales , Queensland , Rios
15.
J Chromatogr A ; 1621: 461053, 2020 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-32276857

RESUMO

The chromatographic properties of a new coated amylose tris(3-chloro-5-methylphenylcarbamate) were evaluated in supercritical fluid chromatography for the separation of enantiomers of chiral 1-aryl-5-aryl-pyrrolidin-2-one derivatives, potential anticancer agents, and some commercial drugs. The mobile phase consisted of CO2-modifier mixtures with 30% of either methanol or ethanol, the flow rate was 3 mL/min. The column oven temperature was 40 °C and the outlet pressure was 15 MPa, in order to limit the compressibility of the CO2, thus limiting density variation along the column. The obtained results were then compared to those observed toward 3 other stationary phases: the coated amylose tris(3,5-dimethylphenylcarbamate), the immobilized amylose tris(3,5-dimethylphenylcarbamate) and the coated amylose tris(5-chloro-2-methylphenylcarbamate). It was shown that the new coated amylose tris(3-chloro-5-methylphenylcarbamate) was the most retentive column whatever the studied compounds, particularly for thalidomide and omeprazole with retention factors up to 73.3 and 29.5for the second enantiomer, respectively. Concerning the enantioselectivity, even most of the compounds are separated on all the four columns, the coated amylose tris(3-chloro-5-methylphenylcarbamate) allows the best resolution for most of the ten studied analytes (except omeprazole for which the resolution values are equal to 7.8 and 9.7 on the coated amylose tris(3-chloro-5-methylphenylcarbamate) and amylose tris(3,5-dimethylphenylcarbamate), respectively). Acting in complementary ways, the two chlorinated stationary phases permitted the complete separation of enantiomers of nine compounds out of the ten.


Assuntos
Amilose/análogos & derivados , Cromatografia com Fluido Supercrítico/métodos , Amilose/química , Antineoplásicos/análise , Antineoplásicos/isolamento & purificação , Carbamatos/química , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/isolamento & purificação , Fenilcarbamatos/química , Pirrolidinonas/análise , Pirrolidinonas/isolamento & purificação , Dióxido de Silício/química , Estereoisomerismo
16.
Arch Environ Contam Toxicol ; 78(4): 579-588, 2020 May.
Artigo em Inglês | MEDLINE | ID: mdl-32123946

RESUMO

The occurrence and potential sources of pharmaceuticals and personal care products (PPCPs) in surface waters from a large coastal city Qingdao, North China, were investigated. Forty-five compounds were analyzed by high-performance liquid chromatography-tandem mass spectrometry. The results showed that 28 compounds of PPCPs were detected. The most frequently detected compounds were atrazine, clarithromycin, nonylphenol, and bisphenol A with the detection rates > 90%. Paracetamol showed the highest concentration up to 4400 ng/L (mean 152.5 ng/L), followed by ampicillin (max. 2980 ng/L) with the highest mean concentration (229.3 ng/L), iopromide (max. 1744 ng/L, mean 74.5 ng/L), atrazine (max. 1612 ng/L, mean 96.1 ng/L), and bisphenol A (max. 1384 ng/L, mean 78.3 ng/L). The contamination levels and composition profiles of PPCPs along the rivers flowing through rural and urban areas and in seawater showed large spatial variability. Typical source markers and principle component analysis were used to track and differentiate the potential PPCP sources. The emphases of the study were the influence of animal farming in rural areas on PPCP composition profiles and the ecological risk. The results indicated that PPCPs in Qingdao surface water mainly came from three potential sources, i.e., treated wastewater (effluents from WWTPs), untreated wastewater, and nonpoint sources in agricultural areas.


Assuntos
Cosméticos/análise , Monitoramento Ambiental/métodos , Preparações Farmacêuticas/análise , Rios/química , Poluentes Químicos da Água/análise , Agricultura , China , Cidades , Medição de Risco , Água do Mar/química , Águas Residuárias/química
17.
Environ Monit Assess ; 192(4): 204, 2020 Mar 02.
Artigo em Inglês | MEDLINE | ID: mdl-32124056

RESUMO

Pharmaceuticals are chemical compounds employed as medicinal drugs. They have severe physic-chemical properties which make them destructive for non-target species. Consequently, their continuous addition in the environment may pose hazardous effects. Among these, diclofenac (DCF), a non-steroidal anti-inflammatory drug (NSAID), is extensively used in Pakistan which may lead to its accumulation in both terrestrial and aquatic environment. Present study aims to assess the presence and concentration of pharmaceutically active drug (DCF) in surface water and wastewater of twin cities of Pakistan (Rawalpindi and Islamabad). For this purpose, a validated high-performance liquid chromatography (HPLC) method was adopted involving solid-phase extraction procedure. Wastewater samples were collected from various sites of Rawalpindi and Islamabad. Results of HPLC analysis revealed that DCF was extant with considerably high concentration, not only in wastewater but also in surface water samples. Concentrations as high as 216 µg L-1 was detected in Rawat industrial area and low as 8 µg L-1 was detected in dairy farm wastewater samples collected from Taramri. However, maximum DCF levels in residential wastewater and hospital wastewater were detected to be 105 µg L-1 and 34 µg L-1, respectively. Moreover, the highest detected level (116 µg L-1) was found in surface water of Sawan River. Further, results of ecological risk assessment revealed its possible toxic effects of DCF on various aquatic organisms.


Assuntos
Diclofenaco , Preparações Farmacêuticas , Poluentes Químicos da Água , Cidades , Diclofenaco/análise , Ecossistema , Monitoramento Ambiental , Paquistão , Preparações Farmacêuticas/análise , Medição de Risco , Águas Residuárias , Poluentes Químicos da Água/análise
18.
J Chromatogr A ; 1620: 461009, 2020 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-32173027

RESUMO

A fast method for analysis of 47 pharmaceuticals active compounds (PhACs) in fish muscle has been developed and validated addressing the parameters accuracy, precision (intraday and interday), matrix effect at three spiking levels: 5, 25 and 50 ng PhAC g-1 in fish as well as linearity, limit of detection (LOD), limit of quantification (LOQ). Sixteen protocols were performed varying extraction techniques, solvents, sample filtration and clean-up step. The selected method was based on an ultrasound extraction with acidified mixture of acetonitrile and isopropyl alcohol followed by a clean-up step using Z-Sep/C18 sorbents. Quantitative analysis of the PhACs in the extracts was accomplished by UPLC- QTOF-MS using Sequential Window Acquisition of All Theoretical Fragment-Ion, SWATHTM acquisition technology. 90% Of the compounds presented extraction recoveries between 60 and 130% with LOQ between 0.2 and 11 ng g-1. The validated method was applied to the analysis of 32 muscle samples from thirteen different species of fish collected in four European river basins (Adige, Evrotas, Llobregat and Sava). A total of ten compounds were found in fish samples with diltiazem as the most frequently detected one followed by carbamazepine and caffeine. Additionally, by taking advantage of the information-rich mass spectral data from the SWATH mode acquisition, the raw data were reprocessed for the presence of the most prescribed 250 pharmaceuticals, metabolites, and drugs of abuse previously reported to occur in the aquatic environment. By considering the mass errors of the molecular ion (˂± 3 ppm) and one characteristic fragment ion (˂±10 ppm) as well as the Library score and the Formula Finder score of the data processing software six compounds were retrieved, and eventually four of them confirmed with authentic standards: cocaine and its metabolite benzoylecgonine, the stimulant nicotine, and the antibiotic ofloxacin. Two lipid regulators, lovastatin and simvastatin, were determined as a false positive.


Assuntos
Monitoramento Ambiental , Peixes/metabolismo , Miniaturização/métodos , Preparações Farmacêuticas/análise , Rios , Animais , Cromatografia Líquida/métodos , Íons , Limite de Detecção , Reprodutibilidade dos Testes
19.
J Chromatogr A ; 1621: 461031, 2020 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-32201038

RESUMO

An innovative strong hydrophilic organic polymer monolithic column of poly(N-benzylquininium chloride-co-1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine) (poly(NBQ-co-TAT)) has been successfully synthesized through in situ copolymerization for capillary electrochromatography. The amphiphilic monomer NBQ and the strong polar cross-linker TAT are firstly used in hydrophilic electrochromatography by taking advantage of the exhibition of hydrophilicity at lower levels of organic solvent and ease formation of porous structure. The monolithic column poly(NBQ-co-TAT) shows powerful hydrophilic selectivity with mobile phase containing more than 60% organic solvent. The introduction of NBQ and TAT enlarges the sources of functional monomers and cross-linkers for HILIC. Due to the presence of the positively charged group in NBQ, an anodic electroosmotic flow is generated with the change of pH values from 2.0 to 12.0. The monolithic column was used for the separations of thioureas, phenols, xanthines, nucleobases, acidic substances and pharmaceuticals. The highest column efficiency for N, N'-dimethylthiourea is 1.15 × 105 N m-1. The application of the monolithic column for a real sample, cytochrome C digestion indicates its great potential in practical application.


Assuntos
Eletrocromatografia Capilar , Preparações Farmacêuticas/análise , Quinina/análogos & derivados , Eletro-Osmose , Interações Hidrofóbicas e Hidrofílicas , Fenóis/análise , Polimerização , Polímeros/química , Quinina/química , Solventes/química , Xantinas/análise
20.
Virchows Arch ; 477(4): 593-595, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32170449

RESUMO

Microscopic foreign objects are sometimes found in gastrointestinal (GI) tract specimens. Some signify important diagnostic findings, such as parasitic or bacterial organisms and some medication resins. Partially digested fruits and vegetables can also be present, and some have been described in the literature as potential mimickers of clinically important findings. While animal protein appears as skeletal muscle on histologic examination, fruits and vegetables can show a wide variation under the microscope. To our knowledge, a thorough histologic examination of commonly eaten fruits and vegetables has not been published in the pathology literature. Herein, we present key morphologic features of fruits and vegetables that might be found in GI specimens, emphasizing potential mimics of significant pathologic findings.


Assuntos
Digestão , Ingestão de Alimentos , Frutas/citologia , Gastroenteropatias/patologia , Trato Gastrointestinal/patologia , Enteropatias Parasitárias/patologia , Preparações Farmacêuticas/análise , Verduras/citologia , Artefatos , Biópsia , Gastroenteropatias/parasitologia , Trato Gastrointestinal/química , Trato Gastrointestinal/parasitologia , Humanos , Enteropatias Parasitárias/parasitologia , Valor Preditivo dos Testes , Reprodutibilidade dos Testes
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