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1.
J Sep Sci ; 47(1): e2300620, 2024 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-38066235

RESUMEN

Herein, a magnetic borate-functionalized MXene composite with multiple boronic affinity sites was fabricated by embedding Fe3 O4 nanoparticles with 4-formylphenylboronic acid functionalized Ti3 C2 Tx nanosheets and served as sorbent for the simultaneous extraction of catecholamines (CAs) in urine samples. The morphology and structure of the magnetic materials were investigated using scanning microscopy, vibrating sample magnetometer, X-ray photoelectron spectrometer, and X-ray diffraction. The introduction of polyethyleneimine can amplify the bonded boronic acid groups, thereby effectively improving the adsorption capacities for CAs based on the multiple interactions of boronic affinity, hydrogen bonding, and metal coordination. The adsorption performance was investigated using the kinetics and isotherms models, and the main parameters that influence the extraction efficiency were optimized. Under the most favorable magnetic solid-phase extraction condition, a sensitive method for the analysis of CAs in urine samples was developed by combining magnetic solid-phase extraction conditions with high-performance liquid chromatography detection. The findings illustrated that the proposed approach possessed a wide linearity range of 0.05-250 ng/mL with an acceptable correlation coefficient (R2  ≥ 0.9984) and detection limits of 0.010-0.015 ng/mL for the target CAs. The research not only provides a notable composite with multiple boronic affinity sites but also offers an effective and feasible measure for the detection of CAs in biological samples.


Asunto(s)
Catecolaminas , Nanopartículas de Magnetita , Nitritos , Elementos de Transición , Polietileneimina/química , Adsorción , Ácidos Borónicos/química , Cromatografía Líquida de Alta Presión , Extracción en Fase Sólida , Nanopartículas de Magnetita/química , Fenómenos Magnéticos
2.
Public Health Nutr ; 27(1): e117, 2024 Apr 11.
Artículo en Inglés | MEDLINE | ID: mdl-38602104

RESUMEN

OBJECTIVE: Monitoring time trends in salt consumption is important for evaluating the impact of salt reduction initiatives on public health outcomes. There has so far not been available data to indicate if salt consumption in Norway has changed during the previous decade. We aimed to assess whether average 24-h salt intake estimated from spot urine samples in the adult population of mid-Norway changed from 2006-2008 to 2017-2019 and to describe variations by sex, age and educational level. DESIGN: Repeated cross-sectional studies. SETTING: The population-based Trøndelag Health Study (HUNT). PARTICIPANTS: In each of two consecutive waves (HUNT3: 2006-2008 and HUNT4: 2017-2019), spot urine samples were collected from 500 men and women aged 25-64 years, in addition to 250 men and women aged 70-79 years in HUNT4. Based on spot urine concentrations of Na, K and creatinine and age, sex and BMI, we estimated 24-h Na intake using the International Cooperative Study on Salt and Blood Pressure (INTERSALT) equation for the Northern European region. RESULTS: Mean (95 % CI) estimated 24-h salt intakes in men were 11·1 (95 % CI 10·8, 11·3) g in HUNT3 and 10·9 (95 % CI 10·6, 11·1) g in HUNT4, P = 0·25. Corresponding values in women were 7·7 (95 % CI 7·5, 7·9) g and 7·7 (95 % CI 7·5, 7·9) g, P = 0·88. Mean estimated salt intake in HUNT4 decreased with increasing age in women, but not in men, and it did not differ significantly across educational level in either sex. CONCLUSIONS: Estimated 24-h salt intake in adult men and women in mid-Norway did not change from 2006-2008 to 2017-2019.


Asunto(s)
Cloruro de Sodio Dietético , Humanos , Masculino , Noruega , Femenino , Persona de Mediana Edad , Adulto , Estudios Transversales , Anciano , Cloruro de Sodio Dietético/administración & dosificación , Cloruro de Sodio Dietético/orina , Sodio/orina , Sodio en la Dieta/orina , Sodio en la Dieta/administración & dosificación , Potasio/orina , Creatinina/orina
3.
Mikrochim Acta ; 191(5): 236, 2024 Apr 03.
Artículo en Inglés | MEDLINE | ID: mdl-38570402

RESUMEN

Three different types of Zr-based MOFs derived from benzene dicarboxylic acid (BDC) and naphthalene dicarboxylic acid as organic linkers (ZrBDC, 2,6-ZrNDC, and 1,4-ZrNDC) were synthesized. They were characterized using X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), Fourier-transform IR spectroscopy (FT-IR), and Transmission electron microscopy (TEM). Their hydrophilic/hydrophobic nature was investigated via contact angle measurements; ZrBDC MOF was hydrophilic and the other two (ZrNDC) MOFs were hydrophobic. The three MOFs were combined with MWCNTs as electrode modifiers for the determination of a hydrophobic analyte, flibanserin (FLB), as a proof-of-concept analyte. Under the optimized experimental conditions, a significant enhancement in the oxidation peak current of FLB was observed when utilizing 2,6-ZrNDC and 1,4-ZrNDC, being the highest when using 1,4-ZrNDC. Furthermore, a thorough investigation of the complex oxidation pathway of FLB was performed by carrying out simultaneous spectroelectrochemical measurements. Based on the obtained results, it was verified that the piperazine moiety of FLB is the primary site for electrochemical oxidation. The fabricated sensor based on 1,4-ZrNDC/MW/CPE showed an oxidation peak of FLB at 0.8 V vs Ag/AgCl. Moreover, it showed excellent linearity for the determination of FLB in the range 0.05 to 0.80 µmol L-1 with a correlation coefficient (r) = 0.9973 and limit of detection of 3.0 nmol L-1. The applicability of the developed approach was demonstrated by determination of FLB in pharmaceutical tablets and human urine samples with acceptable repeatability (% RSD values were below 1.9% and 2.1%, respectively) and reasonable recovery values (ranged between 97 and 103% for pharmaceutical tablets and between 96 and 102% for human urine samples). The outcomes of the suggested methodology can be utilized for the determination of other hydrophobic compounds of pharmaceutical or biological interest with the aim of achieving low detection limits of these compounds in various matrices.

4.
J Clin Microbiol ; 61(1): e0136522, 2023 01 26.
Artículo en Inglés | MEDLINE | ID: mdl-36598196

RESUMEN

Monkeypox infection is a zoonosis first described in humans in 1970 in Congo. While previously manifesting in small, confined outbreaks, the disease is rapidly spreading globally. The aim of this study was to investigate microbiological samples (skin, rectal, and oropharyngeal swab samples and plasma and urine samples) that can help in adequate diagnostic, therapeutic, and prognostic management. We present 30 laboratory-confirmed monkeypox patients with peculiar clinical and virological features admitted to the Sexually Transmitted Diseases Centre of Sant' Orsola Hospital, University of Bologna, in the period between 20 June and 10 August 2022. Demographic, anamnestic, and clinical data were obtained, and microbiological samples were collected and analyzed by real-time PCR to detect the presence of monkeypox virus (MPXV) DNA. All monkeypox patients were adult men who have sex with men (MSM) (mean age, 37.5 years). Nonskin samples were collected from 29 patients during the acute phase of the infection. The detection rates of MPXV DNA in plasma, urine, and oropharyngeal swab samples (82.3%, 64.7%, and 75.0%, respectively) were highest in samples collected 4 to 6 days after symptom onset. The presence of MPXV in plasma and urine samples was analyzed 11 to 38 days after symptom onset to monitor viral shedding duration. Interestingly, MPXV DNA was detected in a urine sample collected on day 21 in one patient. Prolonged positivity in urine after the clinical recovery suggests a potential source of infection by contamination of wastewater and sewage and transmission to possible animal reservoirs and highlights the need for further investigations on nonskin samples to extend and more adequately standardize the patient isolation period.


Asunto(s)
Brotes de Enfermedades , Mpox , Adulto , Animales , Humanos , Masculino , ADN , Hospitales/estadística & datos numéricos , Mpox/diagnóstico , Mpox/epidemiología , Minorías Sexuales y de Género/estadística & datos numéricos
5.
Ecotoxicol Environ Saf ; 249: 114414, 2023 Jan 01.
Artículo en Inglés | MEDLINE | ID: mdl-36516626

RESUMEN

BACKGROUND: Based on self-report questionnaires, two previous epidemiological studies investigated the association between the exposure of women to antibiotics and their fertility. However, biomonitoring studies on low-dose antibiotic exposure, mainly from food and water, and its relation to the risk of infertility are missing. METHODS: Based on a case-control study design, 302 women with infertility (144 primary infertility, 158 secondary infertility) and 302 women with normal fertility, all aged 20-49 years, were recruited from Anhui Province, China, in 2020 and 2021. A total of 41 common antibiotics and two antibiotic metabolites in urine samples were determined by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS). RESULTS: Twenty-eight antibiotics with detection rates from 10% to 100% in both cases (median concentration: ∼2.294 ng/mL) and controls (∼1.596 ng/mL) were included in the analysis. Logistic regression analysis revealed that after controlling for confounding factors, high concentrations of eight individual antibiotics (sulfamethoxazole, sulfaclozine, sulfamonomethoxine, penicillin G, chlorotetracycline, ofloxacin, norfloxacin, and cyadox) and four antibiotic classes (sulfonamides, tetracyclines, quinoxalines, and veterinary antibiotics) were related to a high risk of female infertility, with odds ratios (ORs) ranging from 1.30 to 2.86, except for chlorotetracycline (OR = 6.34), while another nine individual antibiotics (sulfamethazine, azithromycin, cefaclor, amoxicillin, oxytetracycline, pefloxacin, sarafloxacin, enrofloxacin, and florfenicol) and classes of chloramphenicol analogs and human antibiotics were related to a reduced risk of infertility, with ORs ranging from 0.70 to 0.20. Based on restricted cubic spline models after controlling for confounding factors, we observed that the relationship between all of the above protective antibiotics and infertility was nonlinear: A certain concentration could reduce the risk of female infertility while exceeding a safe dose could increase the risk of infertility. CONCLUSION: These results provide preliminary evidence that the effects of antibiotics on female fertility vary based on the active ingredient and usage and imply the importance of exposure dose. Future studies are needed to verify these results by controlling for multiple confounding factors.


Asunto(s)
Clortetraciclina , Infertilidad Femenina , Humanos , Femenino , Antibacterianos/análisis , Espectrometría de Masas en Tándem/métodos , Clortetraciclina/análisis , Infertilidad Femenina/inducido químicamente , Infertilidad Femenina/epidemiología , Estudios de Casos y Controles , China/epidemiología
6.
Medicina (Kaunas) ; 59(3)2023 Feb 23.
Artículo en Inglés | MEDLINE | ID: mdl-36984441

RESUMEN

Background and Objectives: This study presents the development and validation of the 96-microwell-based spectrofluorimetric (MW-SFL) and high performance liquid chromatography (HPLC) with fluorescence detection (HPLC-FD) methods for the quantitation of alectinib (ALC) in its bulk powder form and in urine samples. Materials and Methods: The MW-SFL was based on the enhancement of the native fluorescence of ALC by the formation of micelles with the surfactant cremophor RH 40 (Cr RH 40) in aqueous media. The MW-SFL was executed in a 96-microwell plate and the relative fluorescence intensity (RFI) was recorded by utilizing a fluorescence plate reader at 450 nm after excitation at 280 nm. The HPLC-FD involved the chromatographic separation of ALC and ponatinib (PTB), as an internal standard (IS), on a C18 column and a mobile phase composed of methanol:potassium dihydrogen phosphate pH 7 (80:20, v/v) at a flow rate of 2 mL min-1. The eluted ALC and PTB were detected by utilizing a fluorescence detector set at 365 nm for excitation and 450 nm for emission. Results: Validation of the MW-SFL and HPLC-FD analytical methods was carried out in accordance with the recommendations issued by the International Council for Harmonization (ICH) for the process of validating analytical procedures. Both methods were efficaciously applied for ALC quantitation in its bulk form as well as in spiked urine; the mean recovery values were ≥86.90 and 95.45% for the MW-SFL and HPLC-FD methods, respectively. Conclusions: Both methodologies are valuable for routine use in quality control (QC) laboratories for determination of ALC in pure powder form and in human urine samples.


Asunto(s)
Carbazoles , Piperidinas , Humanos , Cromatografía Líquida de Alta Presión/métodos , Polvos
7.
Electrophoresis ; 43(9-10): 978-989, 2022 05.
Artículo en Inglés | MEDLINE | ID: mdl-34624141

RESUMEN

In this study, a new analytical method was developed and validated for the simultaneous analysis of antibiotic drugs (amoxicillin, cefotaxime, ciprofloxacin, clindamycin, linezolid, metronidazole) and their metabolites (amoxycilloic acid, amoxicillin diketopiperazine, 3-desacetyl cefotaxime lactone, clindamycin sulfoxide, ciprofloxacin piperazinyl-N4-sulfate, linezolid N-oxide, metronidazole-OH) in human urine. Capillary electrophoresis (CE) along with the tandem mass spectrometry (MS/MS) was used to determine and identify all analytes. Appropriate conditions for MS/MS measurements along with the use of the central composite design were optimized. The effects of different analytical conditions (the composition, the concentration, and the pH value of the background electrolyte, the time and pressure of the injection, the capillary temperature and influence of the organic modifier) on the migration and separation of antibiotic drugs and metabolites were examined using the CE-DAD. The analytical procedure was linear for concentrations ranging from 20 to 1000 ng/mL, with determination coefficients higher than 0.99 for all the analytes. The validated analytical procedure was then applied to the measurement of antibiotic drugs and their metabolites in human urine samples.


Asunto(s)
Metronidazol , Espectrometría de Masas en Tándem , Amoxicilina , Antibacterianos/análisis , Cefotaxima , Ciprofloxacina , Clindamicina , Electroforesis Capilar/métodos , Humanos , Linezolid , Espectrometría de Masas en Tándem/métodos
8.
Anal Bioanal Chem ; 414(22): 6681-6694, 2022 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-35879427

RESUMEN

The presence of endocrine-disrupting chemicals in our daily life is increasing every day and, by extension, human exposure and the consequences thereof. Among these substances are bisphenols and parabens. Urine is used to analyze the exposure. The determination of 12 bisphenol homologues and 6 parabens is proposed. A procedure based on a method previously developed by our research group in 2014 is improved. The extraction yield is higher, because the new protocol is 5 times more efficient. Also, a comparison between calibration with pure standards and matrix calibration, to calculate the matrix effect, was also made. A high grade of matrix effect for all analytes was observed. In terms of validation, the limits of detection (LOD) were between 0.03 and 0.3 ng mL-1 and limits of quantification (LOQ) 0.1 to 1.0 ng mL-1, respectively, and the recovery is higher than 86.4% and lower than 113.6%, with a RSD lower than 13.5% in all cases. A methodology for accurate and sensitive quantification of bisphenol homologues together with parabens in human urine using UHPLC-MS/MS was developed. The method was successfully applied to 30 urine samples from children.


Asunto(s)
Disruptores Endocrinos , Espectrometría de Masas en Tándem , Niño , Cromatografía Líquida de Alta Presión/métodos , Disruptores Endocrinos/análisis , Humanos , Límite de Detección , Parabenos/análisis , Espectrometría de Masas en Tándem/métodos
9.
Anal Bioanal Chem ; 414(1): 451-463, 2022 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-33751162

RESUMEN

Oxazepam, one of the most frequently prescribed anxiolytic drugs, is not completely removed from wastewater with conventional treatment processes. It can thus be found at trace levels in environmental water, with human urine constituting the major source of contamination. This study focused on the development and characterization of molecularly imprinted polymers (MIPs) for the selective solid-phase extraction of oxazepam at trace levels from environmental water and human urine samples. Two MIPs were synthesized, and their selectivity in pure organic and aqueous media were assayed. After optimizing the extraction procedure adapted to a large sample volume to reach a high enrichment factor, the most promising MIP was applied to the selective extraction of oxazepam from environmental water. Extraction recoveries of 83 ± 12, 92 ± 4 and 89 ± 10% were obtained using the MIP for tap, mineral and river water, respectively, while a recovery close to 40% was obtained on the corresponding non-imprinted polymer (NIP). Thanks to the high enrichment factors, a limit of quantification (LOQ) of 4.5 ng L-1 was obtained for river water. A selective extraction procedure was also developed for urine samples and gave rise to extraction recoveries close to 95% for the MIP and only 23% for the NIP. Using the MIP, a LOQ of 357 ng L-1 was obtained for oxazepam in urine. The use of the MIP also helped to limit the matrix effects encountered for the quantification of oxazepam in environmental samples and in human urine samples after extraction on an Oasis HLB sorbent.


Asunto(s)
Impresión Molecular , Cromatografía Líquida de Alta Presión , Humanos , Impresión Molecular/métodos , Polímeros Impresos Molecularmente , Oxazepam , Polímeros , Extracción en Fase Sólida/métodos
10.
Environ Res ; 212(Pt E): 113636, 2022 09.
Artículo en Inglés | MEDLINE | ID: mdl-35679907

RESUMEN

Antibiotics are essential medications for human and animal health, as they are used to battle urinary infections and bacterial diseases. Therefore, the rapid determination of antibiotic drugs in biological samples is necessary to address the current clinical challenge. Here, we developed a heterojunction ternary composite of BiOCl/BiVO4 nanosheets enriched with graphene oxide (BiOCl/BiVO4@GO) for accurate and minimal-level detection of an antihistamine (promethazine hydrochloride, PMZ) in urine samples. The BiOCl/BiVO4 nanosheets were prepared by a wet chemical approach using a deep eutectic green solvent. The spectroscopic and analytical methods verified the formation and interaction of the BiOCl/BiVO4@GO composite. Our results showed that the thoroughly exfoliated BiOCl/BiVO4@GO composite retained good electrical conductivity and fast charge transfer toward the electrode-electrolyte interface in neutral aqueous media. In addition, the experimental conditions were accurately optimized, and the BiOCl/BiVO4@GO composite showed excellent electrocatalytic activity toward the oxidation of PMZ. Indeed, the BiOCl/BiVO4@GO composite demonstrated a good linear response range (0.01-124.7 µM) and a detection level of 3.3 nM with a sensitivity of 1.586 µA µM-1 cm-2. In addition, the BiOCl/BiVO4@GO composite had excellent storage stability, good reproducibility, and reliable selectivity. Finally, the BiOCl/BiVO4@GO displayed a desirable recovery level of PMZ in urine samples for real-time monitoring.


Asunto(s)
Grafito , Antibacterianos , Electrodos , Grafito/química , Antagonistas de los Receptores Histamínicos , Reproducibilidad de los Resultados
11.
Urol Int ; 106(3): 227-234, 2022.
Artículo en Inglés | MEDLINE | ID: mdl-33744905

RESUMEN

The purpose of this study in a small group of non-stone-forming Chinese persons was to measure the levels of supersaturation with calcium oxalate and calcium phosphate and pH with the aim of confirming if any of the different short-term urine samples were better for risk evaluation than a 24-h sample. Nine normal men and 1 woman collected urine during 4 periods of the day. Period 1 between 08 and 12 h, Period 2 between 12 and 18 h, Period 3 between 18 and 22 h, and Period 4 between 22 and 08 h. Each sample was analysed for calcium, oxalate, citrate, magnesium and phosphate, and estimates of supersaturation with calcium oxalate (CaOx) and calcium phosphate (CaP) were expressed in terms of AP(CaOx) and AP(CaP) index. An estimate of the solute load of CaOx was also calculated. Urine composition for 24-h urine (Period 24) was obtained mathematically from the analysed variables. Urine composition corresponding to 14-h urine portions 22-12 h (Period 14N) and 08-22 h (Period 14 D) were calculated. The lowest pH levels were recorded in Period 1 urine. The highest level of AP(CaOx) index was recorded during Period 1, and the product AP(CaOx) index × 107 × hydrogen ion concentration was significantly higher in Period 1 urine than in 24-h urine (p = 0.02). Also, the product SL(CaOx) × 107 × hydrogen ion concentration was significantly higher in Period 1 urine (p = 0.02). Low AP (CaP) index levels were recorded in Period 4, but also in all periods following dietary loads of calcium and phosphate. With the important reservation that the analytical results were obtained from non-stone-forming persons, the conclusion is that analysis of urine samples collected between 08 and 12 h might be an alternative to 24-h urine. The risk evaluation might advantageously be expressed either in terms of the product AP(CaOx) index × 107 × hydrogen ion concentration or the product SL(CaOx) × 107 × hydrogen ion concentration.


Asunto(s)
Cálculos Urinarios , Oxalato de Calcio , China , Ácido Cítrico/orina , Cristalización , Femenino , Humanos , Masculino
12.
Sensors (Basel) ; 22(4)2022 Feb 18.
Artículo en Inglés | MEDLINE | ID: mdl-35214527

RESUMEN

Mephedrone, also known as 4-methylmethcathinone, is growing into a prominent recreational drug for young people. When it came to detecting mephedrone, limited efforts were made using electrochemical sensors. As a result, this application depicts the fabrication of a new, sensitive, selective, and economical electrochemical sensor capable of detecting mephedrone by using silver nanoparticles capped with saffron produced through electropolymerization to modify carbon paste electrodes (CPEs). Silver nanoparticles (AgNPs) were capped with saffron (AgNPs@Sa) using a green method. AgNPs@Sa were studied using electron scanning microscopy (SEM) and UV-vis spectroscopy. The sensor was evaluated under the optimum condition to determine its analytical features. The results showed that this procedure had a wide linear range, low detection limit and sufficient reproducibility. Furthermore, the sensor posed sufficient stability. Moreover, it was applied in the determination of mephedrone in urine samples, showing the potential applicability of this electrochemical sensor in real sample analysis.


Asunto(s)
Crocus , Nanopartículas del Metal , Adolescente , Carbono/química , Técnicas Electroquímicas/métodos , Electrodos , Humanos , Límite de Detección , Nanopartículas del Metal/química , Metanfetamina/análogos & derivados , Reproducibilidad de los Resultados , Plata/química
13.
Int J Mol Sci ; 23(4)2022 Feb 20.
Artículo en Inglés | MEDLINE | ID: mdl-35216460

RESUMEN

Acute decompensated heart failure (ADHF) is a life-threatening clinical syndrome involving multi-organ function deterioration. ADHF results from multifaceted, dysregulated pathways that remain poorly understood. Better characterization of proteins associated with heart failure decompensation is needed to gain understanding of the disease pathophysiology and support a more accurate disease phenotyping. In this study, we used an untargeted mass spectrometry (MS) proteomic approach to identify the differential urine protein signature in ADHF patients and examine its pathophysiological link to disease evolution. Urine samples were collected at hospital admission and compared with a group of healthy subjects by two-dimensional electrophoresis coupled to MALDI-TOF/TOF mass spectrometry. A differential pattern of 26 proteins (>1.5-fold change, p < 0.005), mostly of hepatic origin, was identified. The top four biological pathways (p < 0.0001; in silico analysis) were associated to the differential ADHF proteome including retinol metabolism and transport, immune response/inflammation, extracellular matrix organization, and platelet degranulation. Transthyretin (TTR) was the protein most widely represented among them. Quantitative analysis by ELISA of TTR and its binding protein, retinol-binding protein 4 (RBP4), validated the proteomic results. ROC analysis evidenced that combining RBP4 and TTR urine levels highly discriminated ADHF patients with renal dysfunction (AUC: 0.826, p < 0.001) and significantly predicted poor disease evolution over 18-month follow-up. In conclusion, the MS proteomic approach enabled identification of a specific urine protein signature in ADHF at hospitalization, highlighting changes in hepatic proteins such as TTR and RBP4.


Asunto(s)
Insuficiencia Cardíaca , Proteoma , Enfermedad Aguda , Insuficiencia Cardíaca/orina , Humanos , Proteómica/métodos , Curva ROC , Proteínas Plasmáticas de Unión al Retinol , Urinálisis
14.
Artículo en Inglés | MEDLINE | ID: mdl-35705305

RESUMEN

BACKGROUND: Pyrethroid (PYR) insecticides are widely used for controlling various pests. There are two types that differ in terms of usage: agricultural-purpose PYR (agriculture-PYR) and hygiene purpose PYR (hygiene-PYRs). Few studies exist on the exposure to these chemicals in small children. In this study, we conducted biomonitoring of urinary pyrethroid metabolites in 1.5-year-old children throughout the year. METHODS: Study subjects were 1075 children participating in an Aichi regional sub-cohort of the Japan Environment and Children's Study as of 18-month health check-up. The concentrations of four specific hygiene-PYR metabolites including 2,3,5,6-tetrafluoro-1,4-benzenedimethanol (HOCH2-FB-Al), and five common metabolites of hygiene- and agriculture-PYRs including 3-phenoxybenzoic acid (3PBA) and cis- and trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (DCCA), were measured in urine samples extracted from soiled diapers using a triple quadrupole gas chromatograph-mass spectrometer. RESULTS: The highest detection frequencies were for 3PBA, followed by DCCA, 1R-trans-chrysanthemum dicarboxylic acid, and HOCH2-FB-Al. Among the six metabolites, urinary concentrations were seasonally varied. However, this variation was not observed in the most studied PYR metabolite, 3PBA. Spearman's correlation analysis demonstrated a significant positive correlation between FB-Al and DCCA (r = 0.56) and HOCH2-FB-Al and 4-methoxymethyl-2,3,5,6-tetrafluorobenzyl alcohol (r = 0.60). CONCLUSIONS: This biomonitoring survey found widespread and seasonally specific exposure to multiple hygiene- and agriculture-PYRs in 1.5-year-old Japanese children.


Asunto(s)
Insecticidas , Piretrinas , Agricultura , Preescolar , Exposición a Riesgos Ambientales/análisis , Humanos , Lactante , Japón , Espectrometría de Masas , Piretrinas/orina
15.
Ecotoxicol Environ Saf ; 219: 112319, 2021 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-33993090

RESUMEN

Herein, we synthesized a kind of magnetic covalent organic framework nanohybrids (NiFe2O4@COF), and integrated it with polydimethyl siloxane and silicone rubber curing agent for solid phase microextraction (SPME) fiber coating. The fiber coating demonstrated a porous and uniform surface with the BET specific surface of 169.7 m2 g-1. As for seven environmental analytes, the NiFe2O4@COF-based SPME fiber coating gave the higher extraction recoveries for triclosan (TCS) and methyltriclosn (MTCS) than those of fenpropathrin, bifenthrin, permethrin, fenvalerate and deltamethrin. Several operational parameters were rigorously optimized, such as extraction temperature, extraction time, thermal desorption time, solution pH and salt effect. Combined with the GC-ECD detection, the newly developed microextraction method supplied the wide linear range of 0.1-1000 µg L-1 with the correlation coefficients of > 0.9995. The limits of detection (LODs) and limits of quantitation (LOQs) reached as low as 1-7 ng L-1 and 3.3-23 ng L-1, respectively. The intra-day and inter-day precisions in six replicates (n = 6 ) were < 3.55% and < 5.06%, respectively, and the fiber-to-fiber reproducibility (n = 3) was < 7.64%. To evaluate its feasibility in real samples, the fortified recoveries for TCS and MTCS, at low (0.2 µg L-1), middle (2.0 µg L-1) and high (20.0 µg L-1) levels, varied between 81.9% and 119.1% in tap, river and barreled waters as well as male, female and children urine samples. Especially, it is worth mentioning that the NiFe2O4@COF-based SPME coating fiber can be recycled for at least 150 times with nearly unchanged extraction efficiency. Moreover, the extraction recoveries by the as-fabricated fiber coating were much higher than those by three commercial fibers (PDMS, PDMS/DVB and PDMS/DVB/CAR). Overall, the NiFe2O4@COF-based SPME is a convenient, sensitive, efficient and "green" pretreatment method, thereby possessing important application prospects in trace monitoring of TCS-like pollutants in complex liquid matrices.


Asunto(s)
Triclosán/química , Contaminantes Químicos del Agua/química , Dimetilpolisiloxanos , Humanos , Límite de Detección , Fenómenos Magnéticos , Estructuras Metalorgánicas , Polivinilos , Reproducibilidad de los Resultados , Ríos , Microextracción en Fase Sólida/métodos , Temperatura , Triclosán/análogos & derivados , Triclosán/orina , Agua , Contaminantes Químicos del Agua/orina
16.
Mikrochim Acta ; 188(4): 122, 2021 03 10.
Artículo en Inglés | MEDLINE | ID: mdl-33694068

RESUMEN

A colorimetric sensing method is described for discrimination of multiple antioxidants based on core-shell Au@Ag nanocubes (NCs). In order to extract data-rich colorimetric responses from the sensor array, three different concentrations of chloroaurate acid (HAuCl4) were employed as sensing elements. Interestingly, Au3+ ions can be reduced to different valence states (i.e., Au(0) and Au(I)) by different antioxidants, and thus effectively inhibit the oxidation etching process of Au@Ag NCs by Au(III) ions to varying extents, generating diverse colorimetric responses (color and absorbance). This enables identification of the six antioxidants at 10 nM via linear discriminant analysis (LDA) with relative standard deviation (RSD) of 2.52% (n = 3). The discrimination ability of the sensor array was further evaluated in antioxidant binary and multicomponent mixtures. Remarkably, identification of these six antioxidants spiked in urine was realized with 100% of accuracy. Schematic presentation of colorimetric assay for antioxidants based on three chloroauric acid/Au-Ag nanocubes.


Asunto(s)
Antioxidantes/análisis , Cloruros/química , Colorimetría/métodos , Compuestos de Oro/química , Nanopartículas del Metal/química , Oro/química , Humanos , Límite de Detección , Orina/química
17.
Mikrochim Acta ; 188(9): 311, 2021 Aug 29.
Artículo en Inglés | MEDLINE | ID: mdl-34455515

RESUMEN

A simple dual-read assay for uric acid (UA) was developed based on a combined ratiometric fluorescent and colorimetric strategy using nitrogen-doped carbon dots (N-CDs). The biosensor relies on the oxidation of UA by uricase to produce H2O2, which was then converted to •OH radicals by I-, resulting in the oxidation of o-phenylenediamine (OPD) to 2,3-diaminophenazine (DAP). In the presence of UA, the colorless biosensor system changed to yellow. Furthermore, the presence of DAP quenched the fluorescence emission of the N-CDs at 427 nm based on the inner filter effect (IFE). With increasing UA concentrations, the fluorescence intensity of the biosensor at 427 nm decreased but increased at 580 nm, demonstrating the ratiometric response. A strong linearity was observed between the fluorescence intensity ratio of DAP to N-CDs (I580/I427) and the corresponding UA concentration over the range 0.5-150 µM, and a limit of detection (S/N ratio of 3) of 0.06 µM was calculated. The dual-read assay was successfully employed in the quantitation of UA in human serum and urine samples, revealing its potential for measuring UA in clinical samples.


Asunto(s)
Colorimetría/métodos , Colorantes Fluorescentes/química , Puntos Cuánticos/química , Espectrometría de Fluorescencia/métodos , Ácido Úrico/sangre , Ácido Úrico/orina , Técnicas Biosensibles/métodos , Carbono/química , Humanos , Peróxido de Hidrógeno/química , Límite de Detección , Nitrógeno/química , Fenilendiaminas/química , Urato Oxidasa/química , Ácido Úrico/química
18.
Anaerobe ; 72: 102461, 2021 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-34626800

RESUMEN

Peptostreptococcus anaerobius is a gram-positive anaerobic coccus (GPAC) found in the gastrointestinal and vaginal microbiota. The organism is mainly found in polymicrobial and scarcely in monobacterial infections such as prosthetic and native endocarditis. Anaerobic bacteria have rarely been reported as the cause of urinary tract infection (UTI). Although GPAC are susceptible to most antimicrobials used against anaerobic infections, P. anaerobius has shown to be more resistant. Herein, we report a case of UTI caused by P. anaerobius from a 62-year-old man with a history of urological disease. Surprisingly, the microorganism was directly identified by Matrix-Assisted Laser Desorption-Ionization Time-of-Flight Mass Spectrometry (MALDI-TOF MS) from the urine sample. The isolate was successfully identified by phenotypic methods, MALDI-TOF MS, and 16S rRNA gene sequencing. P. anaerobius showed no ß-lactamase-producing activity, was resistant to penicillin, ampicillin, ciprofloxacin and levofloxacin, and displayed intermediate susceptibility to ampicillin-sulbactam and amoxicillin-clavulanic acid. Successful treatment was achieved with oral amoxicillin-clavulanic acid. Antimicrobial susceptibility testing (AST) should be performed on P. anaerobius isolates due to their unpredictable AST patterns and because empirically administered antimicrobial agents may not be active. This report shows that MALDI-TOF MS, directly used in urine specimens, may be a quick option to diagnose UTI caused by P. anaerobius or other anaerobic bacteria. This review is a compilation of monobacterial infections caused by P. anaerobius published in the literature, their pathogenicity, identification, and data about the antimicrobial susceptibility of P. anaerobius.


Asunto(s)
Infecciones por Bacterias Grampositivas/microbiología , Peptostreptococcus/clasificación , Peptostreptococcus/fisiología , Infecciones Urinarias/microbiología , Antiinfecciosos/farmacología , Antiinfecciosos/uso terapéutico , Técnicas de Tipificación Bacteriana , Susceptibilidad a Enfermedades , Infecciones por Bacterias Grampositivas/diagnóstico , Infecciones por Bacterias Grampositivas/tratamiento farmacológico , Humanos , Masculino , Pruebas de Sensibilidad Microbiana , Persona de Mediana Edad , Tipificación Molecular , Peptostreptococcus/efectos de los fármacos , Peptostreptococcus/aislamiento & purificación , ARN Ribosómico 16S/genética , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción , Resultado del Tratamiento , Infecciones Urinarias/diagnóstico , Infecciones Urinarias/tratamiento farmacológico
19.
Sensors (Basel) ; 21(9)2021 Apr 23.
Artículo en Inglés | MEDLINE | ID: mdl-33922519

RESUMEN

A novel promising carbon paste electrode with excellent potentiometric properties was prepared for the analysis of trihexyphenidyl hydrochloride (THP), the acetylcholine receptor and an anticholinergic drug in real samples. It contains 10.2% trihexyphenidy-tetraphenylborate ionic pair as the electroactive material, with the addition of 3.9% reduced graphene oxide and 0.3% of anionic additive into the paste, which consists of 45.0% dibutylphthalate as the solvent mediator and 40.6% graphite. Under the optimized experimental conditions, the electrode showed a Nernstian slope of 58.9 ± 0.2 mV/decade with a regression coefficient of 0.9992. It exhibited high selectivity and reproducibility as well as a fast and linear dynamic response range from 4.0 × 10-7 to 1.0 × 10-2 M. The electrode remained usable for up to 19 days. Analytical applications showed excellent recoveries ranging from 96.8 to 101.7%, LOD was 2.5 × 10-7 M. The electrode was successfully used for THP analysis of pharmaceutical and biological samples.


Asunto(s)
Grafito , Preparaciones Farmacéuticas , Carbono , Electrodos , Potenciometría , Reproducibilidad de los Resultados , Trihexifenidilo
20.
Molecules ; 26(21)2021 Oct 21.
Artículo en Inglés | MEDLINE | ID: mdl-34770764

RESUMEN

In this work, the design of a microfluidic paper-based analytical device (µPAD) for the quantification of nitrate in urine samples was described. Nitrate monitoring is highly relevant due to its association to some diseases and health conditions. The nitrate determination was achieved by combining the selectivity of the nitrate reductase enzymatic reaction with the colorimetric detection of nitrite by the well-known Griess reagent. For the optimization of the nitrate determination µPAD, several variables associated with the design and construction of the device were studied. Furthermore, the interference of the urine matrix was evaluated, and stability studies were performed, under different conditions. The developed µPAD enabled us to obtain a limit of detection of 0.04 mM, a limit of quantification of 0.14 mM and a dynamic concentration range of 0.14-1.0 mM. The designed µPAD proved to be stable for 24 h when stored at room temperature in air or vacuum atmosphere, and 60 days when stored in vacuum at -20 °C. The accuracy of the nitrate µPAD measurements was confirmed by analyzing four certified samples (prepared in synthetic urine) and performing recovery studies using urine samples.


Asunto(s)
Diseño de Equipo , Microfluídica/instrumentación , Microfluídica/métodos , Nitrato-Reductasa/química , Nitratos/orina , Papel , Urinálisis/instrumentación , Urinálisis/métodos , Humanos , Reproducibilidad de los Resultados , Sensibilidad y Especificidad
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