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1.
Epileptic Disord ; 2024 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-38949266

RESUMO

OBJECTIVE: Epileptic spasms (ES) can be caused by a variety of etiologies. However, in almost half of cases, the etiology is unidentified. With the advent of next-generation sequencing (NGS), the recognition of genetic etiologies has increased. METHODS: We retrospectively reviewed the medical records of patients with ES who were evaluated in the comprehensive epilepsy program at King Fahad Specialist Hospital Dammam between 2009 and 2022. RESULTS: Our data show that in 57.7% of patients with ES, the etiology was unidentified after a standard clinical evaluation and neuroimaging. Of these patients, n = 25 (35.2%) received a genetic diagnosis after some form of genetic testing, and 3.1% of patients from specialized metabolic work indicated the need for genetic testing to confirm the diagnosis. Karyotyping led to a diagnosis in 3.6% of patients, and chromosomal microarray led to a diagnosis in 7.1%. An NGS epilepsy gene panel (EP) was done for 45 patients, leading to a diagnosis in 24.4% (n = 11). Exome sequencing was done for 27 patients, including n = 14 with non-diagnostic panel testing; it led to a diagnosis in 37.3% (n = 10). Exome sequencing led to a diagnosis in 61.5% of patients without a previous panel test and in only two patients who had previously had a negative panel testing. SIGNIFICANCE: In this article, we present the diagnostic evaluations of ES for a cohort of 123 patients and discuss the yield and priority of NGS for evaluating ES. Our findings suggest that exome sequencing has a higher diagnostic yield for determining the etiology of ES in patients for whom the etiology is still unclear after an appropriate clinical assessment and a brain MRI.

2.
RSC Adv ; 14(27): 19612-19618, 2024 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-38903417

RESUMO

In this study, an acid-base reaction-based dispersive solid-phase extraction method was developed for the extraction of favipiravir from deionized water, plasma and urine samples prior to its determination using a capillary electrophoresis-diode array detector. The target analyte was extracted from the samples using biotin as a green adsorbent. To reach this goal, the pH of the solution was first adjusted to 9.0 (using borate buffer), and the ionic strength of the solution was enhanced by adding sodium chloride (2.5%, w/v). Thereafter, an appropriate amount of biotin was dissolved in the solution and a homogenous phase was obtained. By adding hydrochloric acid to the solution, an acid-base reaction occurs via protonation of biotin, which decreases its solubility. During this procedure, the analyte was adsorbed onto the tiny particles of the produced adsorbent dispersed into the solution. The resulting mixture was sonicated to facilitate the adsorption of the analyte onto the adsorbent surface. After the collection of biotin particles through centrifugation, the analyte was eluted using acetonitrile and then used in the determination stage. Under the optimal extraction conditions, the calibration curve was linear from 250 to 3000 ng mL-1 with a coefficient of determination of 0.9968. Low limit of detection, and quantification, good repeatability on the same day and different days (relative standard deviation ≤ 8.2%), and acceptable extraction recovery were accessed. The applicability of the method was examined by performing it on spiked plasma and urine samples, and its performance was verified.

3.
Diabetol Metab Syndr ; 16(1): 82, 2024 Apr 04.
Artigo em Inglês | MEDLINE | ID: mdl-38576015

RESUMO

BACKGROUND: In the present systematic review and meta-analysis, the association of maternal exposure to the endocrine disrupting chemicals (EDCs) with cardio-metabolic risk factors in children during childhood for the first time. METHOD: The PubMed, Scopus, EMBASE, and Web of Science databases were systematically searched, up to Feb 2023. In total 30 cohort studies had our inclusion criteria. A random-effects model was used for the variables that had considerable heterogeneity between studies. The Newcastle-Ottawa Scale (NOS) tool was used to classify the quality score of studies. All statistical analyses were conducted using Stata 14 and P-value < 0.05 considered as a significant level. RESULTS: In the meta-analysis, maternal exposure to the EDCs was weakly associated with higher SBP (Fisher_Z: 0.06, CI: 0.04, 0.08), BMI (Fisher_Z: 0.07, CI: 0.06, 0.08), and WC (Fisher_Z: 0.06, CI: 0.03, 0.08) z-scores in children. A significant linear association was found between maternal exposure to the bisphenol-A and pesticides with BMI and WC z-score in children (p < 0.001). Subgroup analysis showed significant linear association of BPA and pesticides, in the urine samples of mothers at the first trimester of pregnancy, with BMI and WC z-score in children from 2-8 years (p < 0.05). CONCLUSION: Prenatal exposure to the EDCs in the uterine period could increase the risk of obesity in children. Maternal exposure to bisphenol-A and pesticides showed the strongest association with the obesity, especially visceral form, in the next generation.

4.
Artigo em Inglês | MEDLINE | ID: mdl-38564965

RESUMO

In the present work, a new microextraction procedure combined with gas chromatography-mass spectrometry has been developed for the analysis of several aliphatic amines from urine sample. The sample preparation method was a continuous homogenous liquid phase microextraction that was based on in-situ preparation of 4-chlorophenol: choline chloride deep eutectic solvent. The deep eutectic solvent was prepared by passing the mixture of related compounds through a syringe barrel filled with exothermic salts (calcium chloride and potassium bromide). The released heat by dissolving the salts and increasing the solution ionic strength assists the formation of the deep eutectic solvent. The influence of various factors on the efficiency of the proposed procedure including salts amount, flow rate, pH, salting-out effect, and extraction solvent volume was studied. The calibration curves were linear broadly over the concentration range of 1.2-250 ng mL-1 with coefficient of determinations ≥0.996. The enrichment factors were in the range of 188-246 and the limits of detection and quantification were 0.16-0.37 and 0.56-1.2 ng mL-1, respectively. Based on the results, the offered method was sensitive, rapid, eco-friendly, and efficient for extracting and determining aliphatic amines in urine samples.


Assuntos
Microextração em Fase Líquida , Solventes/química , Microextração em Fase Líquida/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Solventes Eutéticos Profundos , Sais , Colina , Limite de Detecção
5.
Artigo em Inglês | MEDLINE | ID: mdl-38636134

RESUMO

Herein, a simple, sensitive, and reliable dispersive solid phase extraction was reported for the efficient extraction of sunitinib from biological samples. To facilitate the extraction of the desired analyte from urine and plasma samples, magnetic MIL-101Cr (NH2) @SiO2 @ NiFe2O4 was synthesized by a hydrothermal method and applied as an effective sorbent during the extraction process. After adsorption of the drug using 10 mg of MIL-101Cr (NH2) @ SiO2 @ NiFe2O4 nanoparticles through vortexing (1 min), the sorbent was separatedfrom the sample solution using a magnet. To eluate the drug, the sorbent containing the sunitinib was contacted with 100 µL dimethylformamide. The eluent was analyzed by high performance liquid chromatography-tandem mass spectrometry. Reasonable validation data consisting of low limits of detection (0.14, 0.35, and 0.70 ng mL-1 in deionized water, plasma, and urine) and quantification (0.48, 1.2, and 2.4 ng mL-1 in deionized water, plasma, and urine, respectively), a wide linear range of the calibration curve (0.48-200, 1.2-200, and 2.4-100 ng mL-1 in deionized water, plasma, and urine, respectively) good extraction recovery (76 %), and low relative standard deviations for inter- and intra-day precisions (6.9 %) were obtained by the method. Eventually, the proposed procedure was effectively implemented on both plasma and urine samples, yielding successful outcomes.


Assuntos
Limite de Detecção , Estruturas Metalorgânicas , Extração em Fase Sólida , Sunitinibe , Espectrometria de Massas em Tandem , Espectrometria de Massas em Tandem/métodos , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Sunitinibe/sangue , Sunitinibe/urina , Sunitinibe/análise , Sunitinibe/química , Sunitinibe/isolamento & purificação , Humanos , Estruturas Metalorgânicas/química , Reprodutibilidade dos Testes , Modelos Lineares , Nanopartículas de Magnetita/química
6.
ACS Omega ; 9(8): 9185-9201, 2024 Feb 27.
Artigo em Inglês | MEDLINE | ID: mdl-38434905

RESUMO

The streamlined water-leaching preconcentration method is introduced as a novel preconcentration method in this study. The approach has many benefits including low consumption of organic solvent and deionized water and operation time, energy-saving, no need for dispersion or evaporation, and implementation of more efficient preconcentration. Also, a methodological study was done on the synthesis of (Fe/Co) bimetallic-organic framework that eased the synthesis procedure, decreased its time, and enhanced its analytical performance by increasing its surface area, total pore volume, and average pore diameter parameters. To perform the extraction, bi-MOF particles were added into the solution of interest enriched with sodium sulfate. After vortexing to adsorb the analytes, centrifugation isolated the sorbent particles. A microliter-volume of acetonitrile and 1,2-dibromoethane mixture was used for desorption aim via vortexing. After the separation of the organic phase and transferring it into a conical bottom glass test tube, a milliliter volume of sodium chloride solution was applied to leach the organic phase. A gas chromatograph equipped with a flame ionization detector was applied for the injection of the extracted phase. The method was applied for the extraction and preconcentration of some pesticides from juice samples. Wide linear ranges (5.44-1600 µg L-1), low relative standard deviations (3.1-4.5% for intra- (n = 6) and 3.5-5.2% for interday (n = 4) precisions), high extraction recoveries (61-95%), enrichment factors (305-475), and low limits of detection (0.67-1.65 µg L-1) and quantification (2.21-5.44 µg L-1) were obtained for the developed method.

7.
NPJ Digit Med ; 7(1): 73, 2024 Mar 18.
Artigo em Inglês | MEDLINE | ID: mdl-38499608

RESUMO

Severe hypercholesterolemia/possible familial hypercholesterolemia (FH) is relatively common but underdiagnosed and undertreated. We investigated whether implementing clinical decision support (CDS) was associated with lower low-density lipoprotein cholesterol (LDL-C) in patients with severe hypercholesterolemia/possible FH (LDL-C ≥ 190 mg/dL). As part of a pre-post implementation study, a CDS alert was deployed in the electronic health record (EHR) in a large health system comprising 3 main sites, 16 hospitals and 53 clinics. Data were collected for 3 months before ('silent mode') and after ('active mode') its implementation. Clinicians were only able to view the alert in the EHR during active mode. We matched individuals 1:1 in both modes, based on age, sex, and baseline lipid lowering therapy (LLT). The primary outcome was difference in LDL-C between the two groups and the secondary outcome was initiation/intensification of LLT after alert trigger. We identified 800 matched patients in each mode (mean ± SD age 56.1 ± 11.8 y vs. 55.9 ± 11.8 y; 36.0% male in both groups; mean ± SD initial LDL-C 211.3 ± 27.4 mg/dL vs. 209.8 ± 23.9 mg/dL; 11.2% on LLT at baseline in each group). LDL-C levels were 6.6 mg/dL lower (95% CI, -10.7 to -2.5; P = 0.002) in active vs. silent mode. The odds of high-intensity statin use (OR, 1.78; 95% CI, 1.41-2.23; P < 0.001) and LLT initiation/intensification (OR, 1.30, 95% CI, 1.06-1.58, P = 0.01) were higher in active vs. silent mode. Implementation of a CDS was associated with lowering of LDL-C levels in patients with severe hypercholesterolemia/possible FH, likely due to higher rates of clinician led LLT initiation/intensification.

8.
Artigo em Inglês | MEDLINE | ID: mdl-38547699

RESUMO

In this research, a method known as a hollow fiber-liquid-phase microextraction was employed to extract and concentrate free metoprolol from plasma samples. The extracted analyte was subsequently determined using high-performance liquid chromatography coupled with a diode-array detector. Several parameters, including hollow fiber length, sonication time, extraction temperature, and salt addition, were investigated and optimized to enhance extraction efficiency. After extracting the analyte under optimum conditions from plasma samples, the enrichment factor and extraction recovery were 50 and 86 %, respectively. Moreover, the method exhibited detection and quantification limits of 0.41 and 1.30 ng mL-1, respectively. The analysis of real samples demonstrated satisfactory relative recoveries in the range of 91-99 %.


Assuntos
Microextração em Fase Líquida , Metoprolol , Microextração em Fase Líquida/métodos , Cromatografia Líquida de Alta Pressão/métodos , Cloreto de Sódio , Sonicação
10.
Anal Methods ; 16(11): 1593-1602, 2024 Mar 14.
Artigo em Inglês | MEDLINE | ID: mdl-38404220

RESUMO

In this study, a sample preparation procedure based on salt-induced homogeneous liquid-liquid extraction performed in a narrow-bore tube was used for the preconcentration and extraction of Zn(II), Cu(II), and Cd(II) ions from honey samples. To perform the procedure, a mixture of working solution containing sodium chloride, acetonitrile, and a synthesized deep eutectic solvent (as an extraction solvent) was transferred into a narrow tube filled with solid sodium chloride up to a specific level. As the solution flowed through the tube, tiny droplets of the extraction solvent were formed at the boundary between the solution and salt layer. The droplets moved upwards in the tube and eventually collected as a distinct layer on the top of the solution. The separated phase was removed and dispersed into ionized water. After centrifugation, tiny droplets of the extraction solvent containing the analytes were sedimented at the bottom of the tube. The concentrated analytes were measured using flame atomic absorption spectrophotometry. The linear ranges and extraction recoveries were obtained in the ranges of 1.5-100 µg kg-1 and 89.6-94.8%, respectively. The detection limits ranged from 0.35 to 0.48 µg kg-1. Low relative standard deviations (C = 10 µg L-1, n = 6) of 3.1, 2.8, and 3.4% for Zn(II), Cu(II), and Cd(II), respectively, were obtained. Finally, the optimized method was successfully used in determination of concentration of the selected heavy metal ions in various honey samples.


Assuntos
Mel , Microextração em Fase Líquida , Solventes , Cloreto de Sódio , Cádmio , Solventes Eutéticos Profundos , Microextração em Fase Líquida/métodos , Extração Líquido-Líquido/métodos , Cloreto de Sódio na Dieta , Zinco
11.
Artigo em Inglês | MEDLINE | ID: mdl-38211390

RESUMO

Tacrolimus is a potent immunosuppressive drug used in the prevention of tissue rejection. It has a narrow therapeutic index. Therefore, the determination of its concentration in biological fluids like plasma and urine is a very crucial issue. In this research, tacrolimus concentrations in plasma and urine samples were determined with a dispersive solid phase extraction procedure coupled to high-performance liquid chromatography-tandem mass spectrometry. For this purpose, a curcumin modified metal-organic framework was synthesized and used in extraction procedure. Tacrolimus was adsorbed onto the sorbent surface with aid of vortexing. Then, the adsorbed tacrolimus was eluted by a suitable solvent. Important parameters in extraction procedure were optimized by "one-variable-at-a-time" approach and reported as below: sorbent amount, 10 mg; sample solution pH, 2; agitation mode, vortexing; adsorption and desorption times, 1 min, and eluent (volume), methanol (200 µL). Under the optimized conditions and according to the International Council for Harmonization guidelines, the validation of the method was performed, and the results showed acceptable accuracy and precision (relative standard deviations ≤14 %), good linearity in a wide range (4-200 ng mL-1), and low limits of detection (1.2 ng mL-1 in plasma and 0.34 ng mL-1 in urine) and quantification (4.7 ng mL-1 in plasma and 1.12 ng mL-1 in urine). Finally, the validated method was successfully applied for the determination of tacrolimus in the plasma samples of the patients.


Assuntos
Curcumina , Estruturas Metalorgânicas , Nanocompostos , Humanos , Estruturas Metalorgânicas/química , Tacrolimo , Espectrometria de Massas em Tandem/métodos , Espectrometria de Massa com Cromatografia Líquida , Cromatografia Líquida , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodos
13.
Anal Chim Acta ; 1287: 342062, 2024 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-38182369

RESUMO

BACKGROUND: Herein, a new extraction procedure based on in-situ formation of carbon dioxide-incorporated solid sorbent was introduced for dispersive solid phase extraction of phenolic compounds from aqueous samples. In this study, incorporation of carbon dioxide into the structure of a diamine led to the formation of a solid compound in the sample solution that adsorbed the analytes. RESULTS: The sample solution was mixed with isophorone diamine and placed under carbon dioxide stream. By doing so, isophorone diamine reacted with carbon dioxide and produced a carbamic acid analogue. It was dispersed into the sample solution as tiny particles that adsorbed the analytes. The adsorbed analytes were eluted by a volatile organic solvent and concentrated more by the vaporization of the eluate. The extraction procedure was done at low temperature to limit the releasing carbon dioxide from the produced compound. To obtain the reliable results, the method was validated and the obtained limits of detection and quantification were in the ranges of 0.29-41 and 0.96-1.3 ng/mL, respectively. Acceptable relative standard deviation (≤7.3%) and coefficient of determination (≥0.994) values confirmed the method repeatability and linearity. High enrichment factors (410-435) and extraction recoveries (82-87%) were attained with the introduced method. SIGNIFICANCE AND NOVELTY: In this work, a chemical reaction was done between isophorone diamine and carbon dioxide in solution. The produced product (sorbent) was insoluble in solution and dispersed in whole parts of the solution as tiny particles. A high contact area between the sorbent and analytes provided high extraction efficiency for the analytes. The method was successful utilized in determining target analytes in real samples and the matrix effect of the samples had no important effect on the obtained results.

14.
Artigo em Inglês | MEDLINE | ID: mdl-38252747

RESUMO

A magnetic dispersive solid phase extraction method combined with solidification of floating organic droplet-based dispersive liquid-liquid microextraction has been validated for the extraction of polycyclic aromatic hydrocarbons from honey samples. For this purpose, a carbonised cellulose-ferromagnetic nanocomposite was used as a sorbent through the magnetic dispersive solid phase extraction. For preparation of the sorbent, first, carbonised cellulose nanoparticles were created by treating cellulose filter paper with concentrated solution of sulfuric acid. Then, the prepared nanoparticles were loaded onto Fe3O4 nanoparticles through coprecipitation. In the extraction process, first, a few mg of the sorbent was added to the diluted honey solution and dispersed in it using vortex agitation. The particles were then separated and the adsorbed analytes were eluted with an organic solvent. The eluent was taken and after mixing with a water-immiscible extraction solvent was used in the following solidification of floating organic droplet-based dispersive liquid-liquid microextraction procedure. By performing the extraction process under the obtained optimum conditions, low limits of detection (0.08-0.17 ng g-1) and quantification (0.27-0.57 ng g-1), satisfactory precision (relative standard deviations ≤ 5.0%), and wide linear range (0.57-500 ng g-1) with great coefficients of determination (r2≥ 0.9986) were obtained.


Assuntos
Mel , Microextração em Fase Líquida , Hidrocarbonetos Policíclicos Aromáticos , Cromatografia Gasosa-Espectrometria de Massas , Microextração em Fase Líquida/métodos , Hidrocarbonetos Policíclicos Aromáticos/análise , Extração em Fase Sólida/métodos , Solventes , Celulose , Fenômenos Magnéticos
15.
CNS Neurol Disord Drug Targets ; 23(4): 463-467, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-37026496

RESUMO

Epilepsy is one of the most common and devastating neurological disorders that causes unprovoked, recurrent seizures arising from excessive synchronized neuronal discharging. Although antiepileptic drugs (AEDs) reduce the frequency of epilepsy seizures, drug-refractory epileptic patients exert resistance to AEDs, resulting in treatment difficulty. Moreover, pharmacological treatments do not show satisfactory results in response to photosensitive epilepsy. In the recent era, light therapy emerged as a potential non-pharmacological approach for treating various diseases, including depression, seasonal affective disorders, migraine, pain, and others. Several studies have also shown the potential of light therapy in treating epilepsy. In addition, Red light evokes epilepsy seizures. Blue lenses filter the red light and significantly suppress the frequency of epilepsy seizures. However, the effects of green light on the frequency of epileptic seizures are not studied yet. In addition, light-activated gene therapy or optogenetics also emerged as a possible option for epilepsy treatment. Animal models have shown the therapeutic possibilities of optogenetics and light therapy; however, human studies addressing this possibility are still vague. This review provides the beneficial effects of light in reducing seizure frequency in epilepsy patients. A limited number of studies have been reported so far; therefore, light therapy for treating epilepsy requires more studies on animal models to provide precise results of light effects on seizures.


Assuntos
Epilepsia Generalizada , Epilepsia , Transtornos de Enxaqueca , Animais , Humanos , Epilepsia/tratamento farmacológico , Convulsões/tratamento farmacológico , Anticonvulsivantes/uso terapêutico , Anticonvulsivantes/efeitos adversos , Epilepsia Generalizada/tratamento farmacológico , Transtornos de Enxaqueca/tratamento farmacológico
16.
Childs Nerv Syst ; 40(3): 957-960, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-37943342

RESUMO

Malformations of cortical development such as polymicrogyria can cause medically refractory epilepsy. Epilepsy surgery (hemispherotomy) can be a good treatment option. In recent years, navigated transcranial magnetic stimulation (nTMS), a noninvasive brain mapping technique, has been used to localize the eloquent cortex for presurgical evaluation of patients with epilepsy. In the present case study, neurophysiological markers of the primary motor cortex (M1), including resting motor threshold (rMT), motor evoked potentials (MEPs), and silent period (SP), were assessed in both hands of a right-handed 10-year-old girl with a history of epilepsy and right hemispheric polymicrogyria. Bilateral MEPs with short latencies were elicited from the contralesional side. The average MEP amplitude and the latency for the patient's paretic and non-paretic hands differed significantly. We conclude that nTMS is a safe and tolerable procedure that can be used for presurgical evaluation in children with intractable epilepsy.


Assuntos
Neoplasias Encefálicas , Epilepsia Resistente a Medicamentos , Epilepsias Parciais , Epilepsia , Córtex Motor , Polimicrogiria , Feminino , Criança , Humanos , Estimulação Magnética Transcraniana/métodos , Neoplasias Encefálicas/cirurgia , Potencial Evocado Motor , Córtex Motor/fisiologia , Mapeamento Encefálico/métodos , Epilepsia Resistente a Medicamentos/etiologia , Epilepsia Resistente a Medicamentos/cirurgia
17.
Gene ; 900: 148020, 2024 Mar 30.
Artigo em Inglês | MEDLINE | ID: mdl-38000703

RESUMO

OBJECTIVE: The adipokine Chemerin and the retinoic acid receptor responder 2 (RARRES2) gene have been associated with an increased incidence of obesity, insulin resistance, endothelial dysfunction, type 2 diabetes mellitus, and coronary artery disease. The impact of RARRES2 rs17173608 gene polymorphism on acute myocardial infarction and Chemerin levels has not yet been entirely elucidated. This study aimed to assess the association of RARRES2 rs17173608 gene polymorphism and serum Chemerin with acute myocardial infarction (AMI) and its risk factors in an Iranian population. METHODS: In this case-control study, 134 AMI patients and 100 healthy controls were recruited from tertiary referral hospitals in Zanjan, Iran. Whole blood samples were collected for DNA extraction and Chemerin level determination. An enzyme-linked immunosorbent assay was used to quantify plasma levels of Chemerin. Tetra-primer amplification refractory mutation system-polymerase chain reaction and agarose gel electrophoresis techniques were used to detect gene polymorphism of Chemerin rs17173608 from DNA samples. RESULTS: Serum Chemerin levels were higher in the control group than in the AMI group. However, after adjusting for age, sex, and other risk factors, there was no significant association between serum Chemerin level and AMI occurrence. In the genotype analysis, 21.6% of patients had the TT genotype, and 78.4% had the TG genotype. The GG genotype was not detected in any patient. The genotype distribution of the healthy control group was 19.0% TT genotype, 80.0% TG genotype, and 1.0% GG genotype. Serum Chemerin levels in participants with TG genotype were statistically different between case and control groups. CONCLUSION: Serum Chemerin levels and RARRES2 rs17173608 gene polymorphism were not correlated with AMI occurrence after adjusting for AMI risk factors in Iranian patients. More research with a larger sample size and diverse ethnicities is needed to corroborate our findings.


Assuntos
Diabetes Mellitus Tipo 2 , Infarto do Miocárdio , Humanos , Estudos de Casos e Controles , Diabetes Mellitus Tipo 2/genética , DNA , Genótipo , Irã (Geográfico) , Infarto do Miocárdio/genética , Polimorfismo de Nucleotídeo Único , Fatores de Risco
18.
J Pharm Biomed Anal ; 239: 115874, 2024 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-38029702

RESUMO

In this work, a simple and inexpensive dispersive solid phase extraction method using SiO2 @MCM-41-Co3O4 yolk shell as a sorbent was developed for the extraction of favipiravir from plasma samples. The sorbent was synthesized with a simple and novel method. Optimization of the extraction procedure was performed using one parameter at a time strategy. For selective measurement of favipiravir in real samples, multiple reaction monitoring mode in high-performance liquid chromatography-tandem mass spectrometry was used. The synthesized sorbent presented a high adsorption capacity for favipiravir due to its mesoporous structure and different interactions. After optimization of effective parameters including the amount of sorbent, pH, and adsorption and desorption times, the analytical parameters of the method were evaluated. The developed method exhibited a wide linear range from 0.50 to 1000 µg/L. The detection limit and quantification limit of the method were 0.15 and 0.50 µg/L, respectively. The relative standard deviation of the method was obtained by using intra- and inter-day tests, and in both cases, it was less than 6.0%. Finally, the method was successfully used to measure favipiravir in plasma samples with relative recoveries in the range of 87-105%.


Assuntos
COVID-19 , Espectrometria de Massas em Tandem , Humanos , Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas em Tandem/métodos , Dióxido de Silício/química , Espectrometria de Massa com Cromatografia Líquida , Limite de Detecção , Extração em Fase Sólida/métodos
19.
J Pharm Biomed Anal ; 240: 115926, 2024 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-38142500

RESUMO

For the first time in this study, a microextraction method was developed to perform follicular fluid safety assessment analysis. The drastic importance of follicular fluid safety on the proper nourishment and development of oocytes caused the development of the present method. Since women are regularly exposed to parabens through cosmetics, healthcare, and hygienic products, the infection of body fluids is probable in long-term exposures. Also, for the first time, MIL-68 (In) was applied in an analytical method. Moreover, a new method called in-situ effervescence-boosted dispersive liquid-liquid microextraction was adopted for the simultaneous derivatization and preconcentration of the target parabens. To perform the method, 25 mg of MIL-68 (In) was dispersed into the solution of follicular fluid by vortexing. Then, 1.0 mL of 2-propanol was used to elute the analytes from the absorbent via vortexing. The analyte-enriched organic phase was mixed with 100 µL of acetic anhydride (derivatization agent) and 27 µL 1,2-dibromoethane (extraction solvent) which was swiftly injected into a sodium carbonate solution. Following the centrifugation, the extraction solvent was sedimented at the bottom of a conical bottom glass test tube and an aliquot of it was injected into a gas chromatograph equipped with a flame ionization detector. Wide linear ranges (120-25000 µg L-1), satisfactory extraction recoveries (31-79%) and enrichment factors (31-79), and appreciable limits of detection (7-36 µg L-1) and quantification (25-120 µg L-1) were recorded. The high surface area of MIL-68 (In) (608.82 m2 g-1) and its significantly low average pore diameter (13.829 A°) provide an ideal platform for the extraction of parabens from the complex matrix of follicular fluid.


Assuntos
Microextração em Fase Líquida , Parabenos , Humanos , Feminino , Parabenos/análise , Microextração em Fase Líquida/métodos , Líquido Folicular/química , Solventes/análise , Extração em Fase Sólida/métodos
20.
Sci Rep ; 13(1): 21304, 2023 12 02.
Artigo em Inglês | MEDLINE | ID: mdl-38042936

RESUMO

This study was the first-ever attempt to apply MIL-68 (Ga) in developing an analytical method. The method extracts and preconcentrates some parabens from mouthwash and hydrating gel samples. The variable extraction parameters were optimized, and the figures of merit were documented. Avogadro software was used besides discussing intermolecular interactions to clarify the absorption process. ComplexGAPI software was also exploited to assess the greenness of the method. After the derivatization of the parabens using acetic anhydride in the presence of sodium carbonate, sodium chloride was added to the solution and vortexed to dissolve. A few milligrams of MIL-68 (Ga) were added into the solution and vortexed. Centrifugation separated the analyte-loaded absorbent, which was treated with mL volume of methanol through vortexing for desorption aim. A few microliters of 1,2-dibromoethane were merged with the methanolic phase and injected into a sodium chloride solution. One microliter of the extracted phase was injected into a gas chromatograph equipped with a flame ionization detector. High enrichment factors (200-330), reasonable extraction recoveries (40-66%), wide linear ranges (265-30,000 µg L-1), and appreciable coefficients of determination (0.996-0.999) were documented. The applicability of dispersive solid phase extraction for extracting polar analytes, imposing no additional step for performing derivatization, the capability of MIL-68 (Ga) for the absorption of both derivatized and non-derivatized parabens, the use of only 10 mg absorbent, and one-pot synthesis besides no high temperature or long reaction time in the sorbent provision are the highlights of the method.


Assuntos
Parabenos , Cloreto de Sódio , Parabenos/análise , Extração em Fase Sólida/métodos , Cromatografia Gasosa/métodos , Metanol
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