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1.
Antioxidants (Basel) ; 11(8)2022 Jul 28.
Artigo em Inglês | MEDLINE | ID: mdl-36009193

RESUMO

Common bean (Phaseolus vulgaris) represents one of the most famous foods with antiobesity activity showing a significant efficacy against fat accumulation, insulin resistance and dyslipidaemia. In this work, two Italian varieties of common bean, i.e., Tondino del Tavo and Cannellino Bio, from the centre of Italy were studied to characterise their phenolic profile by HPLC-PDA in relation to different fractions after a straightforward extraction procedure. Antioxidant property and enzymatic inhibition power were also evaluated in order to delineate a possible biological profile. Results show a considerable phenolic content (0.79 and 1.1 µg/mg of 3-hydroxybenzoic acid for hexane extract of Tondino del Tavo and Cannellino Bio, respectively; 0.30 µg/mg p-coumaric acid for n-hexane extract of Tondino del Tavo) for both varieties, and a strong antioxidant activity according to the major phenolic concentration of the extracts. The anti-inflammatory activity of the decoction extracts was also investigated through a zymosan-induced edema formation assay, revealing a moderate ability for both of them. These preliminary data prompt us to further explore the nutrient components of these two varieties in the future.

2.
Front Physiol ; 13: 886149, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-35694403

RESUMO

Human postmortem skeletal muscles are a unique source of satellite cells for skeletal muscle regenerative studies. Presomite and somite satellite cells obtained by postmortem muscles have been established as populations of human skeletal muscle precursor cells able to proliferate and differentiate in vitro. It is extremely interesting to have access to a large amount of postmortem human skeletal muscle precursor cells, especially from craniofacial as well as limb skeletal muscles in order to evaluate their potential application not only for the fundamental understanding of muscle physiology and diseases but also for drug testing in a challenging 3D-shaping muscles like skeletal muscle microphysiological systems.

3.
Molecules ; 27(6)2022 Mar 21.
Artigo em Inglês | MEDLINE | ID: mdl-35335375

RESUMO

A new 5,7-dihydroxy-3'-methoxy-4'-acetoxyflavone-8-C-ß-d-arabinopyranoside-2″-O-(4‴-acetoxy)-glucoside (6) and three known flavone C-glycosides-5,7,3',4'-tetrahydroxyflavone-6-C-xyloside-8-C-ß-d-glucoside (lucenin-1) (7), 5,7,3'-trihydroxyflavone-6-C-glucoside-8-C-ß-d-glucoside (vicenin-2) (8), and 5,7,4'-trihydroxy-3'-methoxyflavone-6-C-ß-d-glucopyranoside-8-C-α-arabinopyranoside (chrysoeriol-6-C-ß-d-glucopyranoside-8-C-α-arabinopyranoside) (9)-were isolated from aerial parts of Scleranthus perennis L. (Caryophyllaceae). Their structures were determined through the use of comprehensive spectroscopic and spectrometric methods, and a method for the quantification of the major constituents of S. perennis and S. annuus L. was developed. Furthermore, the anti-collagenase and antioxidant activities of all isolated compounds obtained from extracts and fractions from both Scleranthus species were evaluated. The highest percentage of collagenase inhibition (at 400 µg/mL) was distinguished for methanolic extracts (22.06%, 32.04%) and ethyl acetate fractions (16.59%, 14.40%) from S. annuus and S. perennis. Compounds 6-9 displayed moderate inhibitory activity, with IC50 values ranging from 39.59-73.86 µM.


Assuntos
Antioxidantes , Caryophyllaceae , Antioxidantes/farmacologia , Colagenases , Flavonoides/química , Flavonoides/farmacologia , Glicosídeos/química
4.
J Med Case Rep ; 16(1): 72, 2022 Feb 09.
Artigo em Inglês | MEDLINE | ID: mdl-35139890

RESUMO

BACKGROUND: Since the beginning of the worldwide spread of severe acute respiratory syndrome coronavirus 2 to date, important knowledge has been obtained about the virus behavior in living subjects and on inanimate surfaces; however, there is still a lack of data on virus persistency on dead bodies and the risk of contagion from cadavers. CASE PRESENTATION: The present case shows the persistency of the severe acute respiratory syndrome coronavirus 2 viral genome in nasopharyngeal swabs performed on a drowned Caucasian man, aged 41 years old, who was completely asymptomatic when he was alive, up to 41 days after death. Specific real-time reverse transcriptase-polymerase chain reaction (TaqMan 2019-nCoV Assay Kit v2; Thermo Fisher Scientific, Italy and Realquality RQ-SARS-CoV-2, AB Analytical) was used to evaluate the swabs. CONCLUSIONS: This data reflect the importance of postmortem swabs in all autopsy cases, and not only in potential severe acute respiratory syndrome coronavirus 2-related death, and also highlight the necessity to evaluate virus positivity a long time after the moment of death, even if a low initial viral load was assessed.


Assuntos
COVID-19 , SARS-CoV-2 , Adulto , Cadáver , Humanos , Masculino , Reação em Cadeia da Polimerase em Tempo Real , Manejo de Espécimes
5.
Artigo em Inglês | MEDLINE | ID: mdl-34920289

RESUMO

In the present work, a new sensitive and selective high-performance liquid chromatography-fluorimetric detection (HPLC-FLD) method was developed and validated to quantify febuxostat (FBX) and montelukast (MON) in human plasma. The developed procedure was successfully applied to a study aimed at evaluating the pharmacokinetic profiles of febuxostat and montelukast in human plasma. A sol-gel poly (caprolactone)-block-poly(dimethylsiloxane)-block-poly(caprolactone) (sol-gel PCAP-PDMS-PCAP) extraction sorbent coated fabric phase sorptive extraction membrane was used in the extraction process. The entire chromatographic analysis was performed with isocratic elution of the composition of the mobile phase (acetonitrile:water, 60:40, v:v, 0.032% glacial acetic acid) on the C18 column. The flow rate is varied during the analysis, particularly from 0.5 mL min-1 at the start and linearly increased to 1.5 mL min-1 in 7 min. The detection and quantification of the analytes was carried out by means of a fluorimetric detector at 320 nm and 350 nm as absorption wavelengths and at 380 and 400 nm as emission wavelengths for FBX and MON, respectively. The calibration curves demonstrated linearity in the range 0.3-10 ng mL-1 and 5-100 ng mL-1 for FBX and MON, respectively, while the LOD and LOQ values were 0.1 and 0.3 ng mL-1 for FBX and 1.5 and 5 ng mL-1 for MON. Intraday and interday RSD% values were found lower than 5.79%. As reported, the method was applied to real plasma samples obtained from a volunteer who was co-administered both the drugs. Pharmacokinetic data reveal that the concentration of both the drugs reaches the plateau approximately at the same time, but exhibits an elimination phase at different rates. This study demonstrated the usefulness of the new method and its applicability in therapeutic drug monitoring (TDM).


Assuntos
Acetatos/sangue , Cromatografia Líquida de Alta Pressão/métodos , Ciclopropanos/sangue , Febuxostat/sangue , Quinolinas/sangue , Sulfetos/sangue , Acetatos/química , Acetatos/farmacocinética , Adsorção , Adulto , Fibra de Algodão , Ciclopropanos/química , Ciclopropanos/farmacocinética , Febuxostat/química , Febuxostat/farmacocinética , Humanos , Limite de Detecção , Modelos Lineares , Quinolinas/química , Quinolinas/farmacocinética , Reprodutibilidade dos Testes , Sulfetos/química , Sulfetos/farmacocinética , Adulto Jovem
6.
Anal Chem ; 93(49): 16308-16313, 2021 12 14.
Artigo em Inglês | MEDLINE | ID: mdl-34843645

RESUMO

Narcotic and psychotropic substances are natural, synthetic, or semisynthetic compounds that are present in both solid and liquid illicit products. The alterations effects on the central nervous system related to their use can be psycholeptic, psychoanaleptic, or psychodiseptic and are able to generate tolerance, addiction, or dependence phenomena, creating social and public order problems. In this scenario, the analytical evaluations that aim to determine these analytes in seized nonbiological samples, and which assume the character of judicial evidence, must meet high analytical requirements of reliability, transparency, and procedures uniformity at a national level. For the first time in the literature, the herein validated method is able to provide the simultaneous quantitative determination of 37 of the most common narcotic substances as well as the most commonly used excipients/adulterants found in seized illicit material. Additionally, the validated method can process both solid and liquid samples maintaining the precision and trueness levels (intraday and interday) in accordance with the U.S. Food and Drug Administration and European Medicines Agency international guidelines (<14.31 and <13.41%, respectively). Furthermore, it provides a simple and fast procedure for sample preparation using the dilute and shoot approach, exploiting the sensitivity and selectivity of the LC-MS/MS instrument configuration used and the signal acquisition in multiple reaction monitoring (MRM) mode (both positive and negative polarization modes).


Assuntos
Manejo de Espécimes , Espectrometria de Massas em Tandem , Cromatografia Líquida , Reprodutibilidade dos Testes , Estados Unidos
7.
Pharmaceuticals (Basel) ; 14(7)2021 Jun 29.
Artigo em Inglês | MEDLINE | ID: mdl-34209566

RESUMO

Therapeutic drug monitoring (TDM) of antiseizure medications (ASMs) represents a valuable tool to establish an appropriate patient therapy, to collect important information about drugs' interactions and to evaluate patient's metabolic capabilities. In recent years, a new volumetric absorptive microsampling technique using VAMS® technology and Mitra® devices, consisting of a sampling technique for the collection of fixed-volume capillary blood, was developed. These new devices provide a new home-sampling technique for whole blood that has been spread out to simplify sample collection from finger-pricks. This review is aimed to compare published articles concerning the application of VAMS® in epilepsy and to identify the strengths and improvement points for the TDM of antiseizure medications. VAMS® allowed a minimally invasive blood sampling even in the absence of trained personnel. Good stability data have indicated that storage and delivery can be facilitated only for specific ASMs. Trueness and precision parameters have been evaluated, and the hematocrit (HCT) effect was minimized.

8.
Food Chem Toxicol ; 155: 112404, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34246708

RESUMO

Capparis spinose L. also known as Caper is of great significance as a traditional medicinal food plant. The present work was targeted on the determination of chemical composition, pharmacological properties, and in-vitro toxicity of methanol and dichloromethane (DCM) extracts of different parts of C. spinosa. Chemical composition was established by determining total bioactive contents and via UHPLC-MS secondary metabolites profiling. For determination of biological activities, antioxidant capacity was determined through DPPH, ABTS, CUPRAC, FRAP, phosphomolybdenum, and metal chelating assays while enzyme inhibition against cholinesterase, tyrosinase, α-amylase and α-glucosidase were also tested. All the extracts were also tested for toxicity against two breast cell lines. The methanolic extracts were found to contain highest total phenolic and flavonoids which is correlated with their significant radical scavenging, cholinesterase, tyrosinase and glucosidase inhibition potential. Whereas DCM extracts showed significant activity for reducing power, phosphomolybdenum, metal chelation, tyrosinase, and α-amylase inhibition activities. The secondary metabolites profiling of both methanolic extracts exposed the presence of 21 different secondary metabolites belonging to glucosinolate, alkaloid, flavonoid, phenol, triterpene, and alkaloid derivatives. The present results tend to validate folklore uses of C. spinose and indicate this plant to be used as a potent source of designing novel bioactive compounds.


Assuntos
Capparis/química , Inibidores Enzimáticos/farmacologia , Sequestradores de Radicais Livres/farmacologia , Compostos Fitoquímicos/farmacologia , Extratos Vegetais/farmacologia , Plantas Medicinais/química , Capparis/toxicidade , Linhagem Celular Tumoral , Inibidores Enzimáticos/química , Inibidores Enzimáticos/toxicidade , Sequestradores de Radicais Livres/química , Sequestradores de Radicais Livres/toxicidade , Humanos , Compostos Fitoquímicos/química , Compostos Fitoquímicos/toxicidade , Componentes Aéreos da Planta/química , Componentes Aéreos da Planta/toxicidade , Extratos Vegetais/química , Extratos Vegetais/toxicidade , Raízes de Plantas/química , Raízes de Plantas/toxicidade , Plantas Medicinais/toxicidade
9.
Molecules ; 26(11)2021 May 28.
Artigo em Inglês | MEDLINE | ID: mdl-34071519

RESUMO

Currently, forensic research is multidisciplinary with new methods and parameters useful to define the cause and time of death as well as survival/agony times. The identification of biochemical markers able to estimate agonal period has been studied by many forensic researchers. It is known that the estimation of agonal time in different types of death is not always easy, hence our interest in literature's data. The studies analyzed in this review confirm the important role of thanatobiochemistry for the estimation of survival times. Regardless of the death cause, the survival/agony time between the primary event and death influences markers concentrations in biological samples (e.g., blood, urine, cerebrospinal fluid). Different biomarkers can be used for qualitative evaluations in deaths with short and long agony (e.g., C-reactive protein, ferritin, GFAP, etc.). Instead, the quantitative interpretation showed limits due to the lack of reference cut-offs. Thanatobiochemistry is a useful tool to confirm what emerged from autopsies findings (macroscopic and histological analysis), but further studies are desirable to confirm the evidence emerging from our review of the literature.


Assuntos
Autopsia/métodos , Morte , Medicina Legal/métodos , Mudanças Depois da Morte , 8-Hidroxi-2'-Desoxiguanosina/sangue , Animais , Biomarcadores/sangue , Proteína C-Reativa/biossíntese , Proteínas de Transporte/sangue , Catecolaminas/metabolismo , Eletroquímica , Proteínas de Ligação a Ácido Graxo/sangue , Ferritinas/sangue , Proteína Glial Fibrilar Ácida/sangue , Humanos , Camundongos , Modelos Químicos , Subunidade beta da Proteína Ligante de Cálcio S100/sangue , Tireoglobulina/química , Hormônios Tireóideos/sangue
10.
J Chromatogr A ; 1648: 462215, 2021 Jul 05.
Artigo em Inglês | MEDLINE | ID: mdl-34000593

RESUMO

A new analyte separation and preconcentration method for the trace determination of antidepressant drugs, Fluoxetine (FLU) and Citalopram (CIT) in urine and wastewaters, was developed based on HPLC-DAD analysis after magnetic solid phase extraction (MSPE). In the proposed method, FLU and CIT were retained on the newly synthetized magnetic sorbent (Fe3O4@PPy-GO) in the presence of buffer (pH 10.0) and then were desorbed into a lower volume of acetonitrile prior to the chromatographic determinations. Before HPLC analysis, all samples were filtered through a 0.45 µm PTFE filter. Experimental parameters such as interaction time, desorption solvent and volume, and pH were studied and optimized in order to establish the detection limit, linearity, enrichment factor and other analytical figures of merit under optimum operation conditions. In the developed method, FLU and CIT were analyzed by diode array detector at the corresponding maximum wavelengths of 227 and 238 nm, respectively, by using an isocratic elution of 60% pH 3.0 buffer, 30% acetonitrile, and 10% methanol. By using the optimum conditions, limit of detections for FLU and CIT were 1.58 and 1.43 ng mL-1, respectively, while the limit of quantifications was 4.82 and 4.71 ng mL-1, respectively. Relative standard deviations (RSD%) for triplicate analyses of model solutions containing 100 ng mL-1 target molecules were found to be less than 5.0 %. Finally, the method was successfully applied to urine (both simulated and real healthy human) and wastewater samples, and quantitative results were obtained in recovery experiments.


Assuntos
Antidepressivos/análise , Cromatografia Líquida/métodos , Citalopram/análise , Fluoxetina/análise , Espectrofotometria Ultravioleta/métodos , Águas Residuárias/química , Poluentes Químicos da Água/análise , Antidepressivos/urina , Citalopram/urina , Fluoxetina/urina , Humanos , Limite de Detecção , Extração em Fase Sólida/métodos , Solventes/química , Poluentes Químicos da Água/urina
11.
Talanta ; 230: 122307, 2021 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-33934773

RESUMO

A magnetic solid phase extraction (MSPE) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) methodology was developed for the determination of chloramphenicol (CP) and tetracycline (TET) antibiotic residues in milk samples. As a solid phase sorbent, C-nanofiber coated magnetic nanoparticles were synthesized and extensively characterized using Field Emission Scanning Electron Microscopy (FE-SEM), Raman Spectroscopy and X-ray Powder Diffraction (XRD) analysis. Experimental variables of MSPE method for both antibiotic analytes were investigated and optimized systematically. After MSPE, the linear range for both the analytes (r2 > 0.9954) were obtained in a range 10.0-600.0 ng mL-1. The limit of detections (LODs) for CP and TET were 3.02 and 3.52 ng mL-1, respectively while RSDs % were below than 4.0%. Finally, the developed method based on MPSE-HPLC-DAD was applied to real milk samples to quantify the antibiotic residues. Recovery values for each antibiotic compound were found in the range of 94.6-105.4% (n = 3) by using spiked model solution.


Assuntos
Cloranfenicol , Nanofibras , Animais , Antibacterianos , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Fenômenos Magnéticos , Leite , Extração em Fase Sólida
12.
Anal Chem ; 93(4): 1957-1961, 2021 02 02.
Artigo em Inglês | MEDLINE | ID: mdl-33470800

RESUMO

This study introduces an innovative device for the noninvasive sampling and chromatographic analysis of different compounds present in exhaled breath aerosol (EBA). The new sampling device, especially in light of the recent COVID-19 pandemic that forced many countries to impose mandatory facemasks, allows an easy monitoring of the subject's exposure to different compounds they may come in contact with, actively or passively. The project combines the advantages of a fabric-phase sorptive membrane (FPSM) as an in vivo sampling device with a validated LC-MS/MS screening procedure able to monitor more than 739 chemicals with an overall analysis time of 18 min. The project involves the noninvasive in vivo sampling of the EBA using an FPSM array inserted inside an FFP2 mask. The study involved 15 healthy volunteers, and no restrictions were imposed during or prior to the sampling process regarding the consumption of drinks, food, or drugs. The FPSM array-LC-MS/MS approach allowed us to effectively exploit the advantages of the two complementary procedures (the convenient sampling by an FPSM array and the rapid analysis by LC-MS/MS), obtaining a powerful and green tool to carry out rapid screening analyses for human exposure to different compounds. The flexible fabric substrate, the sponge-like porous architecture of the high-efficiency sol-gel sorbent coating, the availability of a large cache of sorbent coatings, including polar, nonpolar, mixed mode, and zwitterionic phases, the easy installation into the facemask, and the possibility of sampling without interrupting regular activities provide FPSMs unparalleled advantages over other sampling techniques, and their applications are expected to expand to many other clinical or toxicological studies.


Assuntos
Exposição Ambiental , Membranas Artificiais , Têxteis , COVID-19/epidemiologia , COVID-19/virologia , Cromatografia Líquida de Alta Pressão/métodos , Humanos , Máscaras , Pandemias , Reprodutibilidade dos Testes , SARS-CoV-2/isolamento & purificação , Espectrometria de Massas em Tandem/métodos
13.
Artigo em Inglês | MEDLINE | ID: mdl-33429126

RESUMO

Following the convenient, yet very powerful pathway to create designer extraction sorbent using sol-gel chemistry, a novel sol-gel phenyl/methyl/poly(dimethylsiloxane) sorbent coating was created on polyester fabric substrate for fabric phase sorptive extraction (FPSE) and was subsequently applied to monitor human exposure to selected polycyclic aromatic hydrocarbons (PAHs) including pyrene, chrysene, and benzo[a]pyrene in plasma samples obtained from tobacco smoker volunteers using high performance liquid chromatography-fluorescence detector (HPLC-FLD). A rapid FPSE-HPLC-FLD method was developed that adequately resolved the PAHs chromatographically, after their successful extraction from human plasma using fabric phase absorption extraction (FPSE) and subsequently analysed in the liquid chromatographic system by means of an analytical column (InterSustain C-18 column 150 × 4.6 mm, 5 µm) using acetonitrile (ACN) and water as mobile phases in gradient elution mode. With the optimized conditions, the retention times were found to be 6.168, 7.214, and 10.404 min for pyrene, chrysene, and benzo[a]pyrene, respectively. The total chromatographic runtime was limited to 12.5 min. The method, validated through the calculation of all the analytical parameters according to the International Guidelines, was applied to the analysis of real samples collected from informed volunteers. The proposed approach which included the use of sol-gel phenyl/methyl/poly(dimethylsiloxane) immobilized on hydrophobic polyester substrate and C18 stationary phase used in HPLC, has shown a high potential as a rapid tool for future clinical, forensic and toxicological applications, also in the light of the LOD and LOQ values comparable to those normally obtainable with more sophisticated, and expensive instruments that often require highly trained personnel. The results reported here further consolidate the application of FPSE in the analysis of biological samples for both diagnostic and analytical-clinical purposes.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Exposição Ambiental/análise , Hidrocarbonetos Policíclicos Aromáticos/sangue , Dimetilpolisiloxanos/química , Humanos , Limite de Detecção , Modelos Lineares , Hidrocarbonetos Policíclicos Aromáticos/química , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Reprodutibilidade dos Testes , Espectrometria de Fluorescência
14.
Molecules ; 25(23)2020 Dec 07.
Artigo em Inglês | MEDLINE | ID: mdl-33297520

RESUMO

The increased risk of illness and disability is related to the age inevitable biological changes. Oxidative stress is a proposed mechanism for many age-related diseases. The crucial importance of polyphenol pharmacophore for aging process is largely described thanks to its effects on concentrations of reactive oxygen species. Resveratrol (3,5,4'-trihydroxy-trans-stilbene, RSV) plays a critical role in slowing the aging process but has a poor bioavailabity after oral intake. In this present work, a series of RSV derivatives was designed, synthesized, and evaluated as potential antioxidant agents. These derivatives contain substituents with different electronic and steric properties in different positions of aromatic rings. This kind of substituents affects the activity and the bioavailability of these compounds compared with RSV used as reference compound. Studies of Log P values demonstrated that the introduction of halogens gives the optimum lipophilicity to be considered promising active agents. Among them, compound 6 showed the higher antioxidant activity than RSV. The presence of trifluoromethyl group together with a chlorine atom increased the antioxidant activity compared to RSV.


Assuntos
Técnicas de Química Sintética , Estilbenos/síntese química , Estilbenos/farmacologia , Animais , Linhagem Celular , Halogenação , Humanos , Camundongos , Modelos Teóricos , Estrutura Molecular , Estilbenos/química
15.
Forensic Sci Int ; 312: 110330, 2020 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-32480284

RESUMO

A new liquid chromatography-tandem mass spectrometry (LC-MS/MS) confirmation method for the direct analysis of 17 drugs starting from 200µL of diluted oral fluid (OF), in a single chromatographic run, was developed and validated. Cocaine, benzoylecgonine (BEG), cocaethylene, Δ-9-tetrahydrocannabinol (Δ-9-THC), buprenorphine, 6-acetylmorphine (6AM), morphine, codeine, methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), 3,4-Methylenedioxy-N-ethylamphetamine (MDE), ketamine, N-methyl-1-(1,3-benzodioxol-5-yl)-2-butanamine (MBDB) were determined in a chromatographic run of 12min only with no sample pre-treatment, after the addition of 15 different internal standards (ISs). The method met all requirements in terms of linearity, accuracy (precision and trueness), recovery, and stability requested by FDA guidelines. Carry-over and interferences were negligible, as well as the matrix effects. LLOQs are below the limits defined by European guidelines and Italian national laws. The original oral fluid collections are stable at least six months at -20°C and one week at +4°C.


Assuntos
Cromatografia Líquida/métodos , Drogas Ilícitas/análise , Saliva/química , Espectrometria de Massas em Tandem/métodos , Toxicologia Forense/métodos , Humanos , Manejo de Espécimes , Detecção do Abuso de Substâncias/métodos , Temperatura
16.
Molecules ; 25(12)2020 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-32545471

RESUMO

Ethanol (ethylic alcohol) represents the most commonly used drug worldwide and is often involved in clinical and forensic toxicology. Based on several reports, excessive alcohol consumption is the main contributing factor in traffic accidents, drownings, suicides, and other crimes. For these reasons, it becomes essential to analyze the alcohol concentration during autopsy. Although blood is usually used for alcohol analysis in post-mortem cases, it could suffer alterations, putrefaction, and microbial contaminations. As an alternative to whole blood, vitreous humor has been successfully used in medico-legal studies. In this work, post-mortem specimens were analyzed for ethanol determination. The analysis of blood and vitreous humor were carried-out using gas chromatography-flame ionized detector (GC-FID) with a total run time of 6 min. The method was validated in terms of limit of detection, limit of quantification, dynamic range, sensibility, recovery, precision and trueness. A linear regression analysis indicated a coefficient of determination (R2) of 0.9981. The study confirmed no statistically differences between alcohol concentration in blood and vitreous humor, leading vitreous humor as an excellent matrix that could be used as an alternative to whole blood in toxicological analysis in cases where blood is not available.


Assuntos
Autopsia/métodos , Etanol/análise , Corpo Vítreo/química , Líquidos Corporais/química , Cromatografia Gasosa/métodos , Etanol/sangue , Toxicologia Forense/métodos , Humanos , Mudanças Depois da Morte
17.
Phytochem Anal ; 31(6): 687-699, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32291862

RESUMO

INTRODUCTION: The analysis of plant and herbal samples is a challenging task for analytical chemists due to the complexity of the matrix combined with the low concentration of analytes. In recent years different liquid-phase microextraction (LPME) techniques coupled with a variety of analytical equipment have been developed for the determination of both organic and inorganic analytes. OBJECTIVE: Over the past few years, the number of research papers in this field has shown a markedly growing tendency. Therefore, the purpose of this review paper is to summarise and critically evaluate research articles focused on the application of LPME techniques for the analysis of plant and herbal samples. RESULTS: Due to the complex nature of the samples, the direct application of LPME techniques to the analysis of plants has not often been done. LPME techniques as well as their modalities have been commonly applied in combination with other pretreatment techniques, including a solid-liquid extraction technique supported by mechanical agitation or auxiliary energies for plant analysis. Applications and the most important parameters are summarised in the tables. CONCLUSION: This review summarises the application of the LPME procedure and shows the major benefits of LPME, such as the low volume of solvents used, high enrichment factor, simplicity of operation and wide selection of applicable detection techniques. We can expect further development of microextraction analytical methods that focus on direct sample analysis with the application of green extraction solvents while fully automating procedures for the analysis of plant materials.


Assuntos
Microextração em Fase Líquida , Plantas , Solventes
18.
Molecules ; 25(5)2020 Mar 06.
Artigo em Inglês | MEDLINE | ID: mdl-32155959

RESUMO

Phenolic compounds are secondary metabolites that are found ubiquitously in plants, fruits, and vegetables. Many studies have shown that regular consumption of these compounds could have a positive effect on our health. The aim of this study was to compare the phytochemical contents of the water extracts from three different plants used as folk remedies in Turkey: Aesculus hippocastanum, Olea europaea, and Hypericum perforatum. A liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) analysis was performed to explore the phenolic profiles. The biological activities of these extracts were also evaluated in terms of their antioxidant activities (2,2-diphenyl-1-picrylhydrazyl DPPH, 2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid ABTS, Ferric Reducing Antioxidant Power Assay FRAP, cupric ion reducing antioxidant capacity CUPRAC, ß-carotene, phosphomolybdenum, and metal chelating) and enzyme inhibitory properties (against acetylcholinesterase, butyrylcholinesterase, and tyrosinase). The aqueous extract of H. perforatum showed the highest levels of total phenolic, flavonoid, and saponin contents. Protocatechuic acid, vanillic acid, verbascoside, hesperidin, hyperoside, apigenin 7-hexosides, and quercetin were the most common compounds found in this species. The results confirm that A. hippocastanum, O. europaea, and H. perforatum represent a potential source of natural-derived molecules with positive properties that could be used as valid starting point for new food supplements, and drugs in the pharmaceutical, cosmetic, and food industries.


Assuntos
Aesculus/enzimologia , Hypericum/enzimologia , Medicina Tradicional , Olea/enzimologia , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Flavonoides , Fenóis , Compostos Fitoquímicos/química , Compostos Fitoquímicos/farmacologia , Saponinas , Turquia
19.
Molecules ; 24(18)2019 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-31540217

RESUMO

In this work, the synthesis, characterization, and application of novel parabens imprinted polymers as highly selective solid-phase extraction (SPE) sorbents have been reported. The imprinted polymers were created using sol-gel molecular imprinting process. All the seven parabens were considered herein in order to check the phase selectivity. By means of a validated HPLC-photodiode array detector (PDA) method all seven parabens were resolved in a single chromatographic run of 25 min. These SPE sorbents, in-house packed in SPE empty cartridges, were first characterized in terms of extraction capability, breakthrough volume, retention volume, hold-up volume, number of theoretical plates, and retention factor. Finally, the device was applied to a real urine sample to check the method feasibility on a very complex matrix. The new paraben imprinted SPE sorbents, not yet present in the literature, potentially encourage the development of novel molecularly imprinted polymers (MIPs) to enhance the extraction efficiency, and consequently the overall analytical performances, when the trace quantification is required.


Assuntos
Parabenos/química , Polímeros/síntese química , Urina/química , Humanos , Impressão Molecular , Polímeros/química , Extração em Fase Sólida
20.
Biomolecules ; 9(8)2019 08 14.
Artigo em Inglês | MEDLINE | ID: mdl-31416216

RESUMO

The Lamiaceae family comprises many flowering plants classified into about 236 genera. The genus Ziziphora is one of the well-known genera of this family and its species are important in different fields of pharmaceutical, chemical, traditional, and folk medicines. The phytochemicals present in Ziziphora include monoterpenic essential oils, triterpenes, and phenolic substances. The aim of this paper was to study the phytochemical profile of Ziziphora taurica subsp. taurica and compare and evaluate the biological activities of its ethyl acetate (ZTT-EtOAc), methanolic (ZTT-MeOH), and aqueous (ZTT-W) extracts based on their enzyme inhibition and antioxidant capacities. Determination of total phenolic (TPC) and total flavonoid (TFC) contents as well as biological activities were determined using spectrophotometric procedures. Subsequently, the individual phenolic compounds were detected by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). In total, twenty-two different phenolic compounds were identified, including apigenin, ferulic acid, and luteolin which were the most common. ZTT-MeOH extract showed the best antioxidant activity, whereas ZTT-EtOAc extract was the most effective against tyrosinase and α-amylase. Ziziphora taurica subsp. taurica represents a potential source of natural compounds with positive effects on human health.


Assuntos
Antioxidantes/farmacologia , Inibidores Enzimáticos/farmacologia , Flavonoides/farmacologia , Lamiaceae/química , Fenóis/farmacologia , Compostos Fitoquímicos/farmacologia , Antioxidantes/análise , Benzotiazóis/antagonistas & inibidores , Compostos de Bifenilo/antagonistas & inibidores , Inibidores Enzimáticos/análise , Flavonoides/análise , Humanos , Estrutura Molecular , Monofenol Mono-Oxigenase/antagonistas & inibidores , Monofenol Mono-Oxigenase/metabolismo , Fenóis/análise , Compostos Fitoquímicos/análise , Picratos/antagonistas & inibidores , Extratos Vegetais/química , Ácidos Sulfônicos/antagonistas & inibidores , alfa-Amilases/antagonistas & inibidores , alfa-Amilases/metabolismo
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