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1.
Anal Chem ; 96(26): 10586-10593, 2024 Jul 02.
Artículo en Inglés | MEDLINE | ID: mdl-38887018

RESUMEN

This study investigated the added value of combining both near-infrared (NIR) and Raman spectroscopy into a single NIRaman Combi Fiber Probe for in-line blend potency determination in the feed frame of a rotary tablet press. A five-component platform formulation was used, containing acetylsalicylic acid as the Active Pharmaceutical Ingredient (API). Calibration models for the determination of 1 and 5%w/w label claim tablets were developed using NIR and Raman spectra of powder blends ranging from 0.75 to 1.25%w/w and 3.75 to 6.25%w/w API, respectively. Step-change experiments with deliberate 10% deviation steps from the label claims were performed, from which the collected spectra were used for model validation. For model development and validation, low-level data fusion was explored through concatenation of preprocessed NIR and Raman spectra. Mid-level data fusion was also evaluated, based on extracted features of the preprocessed data. Herewith, score vectors were extracted by transforming preprocessed spectra through Principal Component Analysis, followed by critical feature selection through Elastic Net Regression. Partial Least Squares regression was applied to regress singular, low-level or mid-level fused data versus blend potency. It could be concluded that irrespective of the data fusion technique, an increase in Step-Change Sensitivity (SCS) and decrease in Root Mean Squared Error (RMSE) was observed when predicting the 5%w/w step-change experiment. For the prediction of the 1%w/w step-change experiment, no added benefit with regard to SCS and RMSE was observed due to the addition of the noisy NIR spectra.


Asunto(s)
Aspirina , Espectroscopía Infrarroja Corta , Espectrometría Raman , Comprimidos , Espectrometría Raman/métodos , Comprimidos/química , Espectroscopía Infrarroja Corta/métodos , Aspirina/análisis , Análisis de Componente Principal , Calibración
2.
Sensors (Basel) ; 24(10)2024 May 11.
Artículo en Inglés | MEDLINE | ID: mdl-38793913

RESUMEN

The purpose of this paper is to demonstrate a new discovery regarding the interaction between materials and very low radio frequencies. Specifically, we observed a feedback response on an inertia active sensor when specific frequencies (around 2-4 kHz) are used to irradiate targeted pharmaceutical samples like aspirin or paracetamol drugs. The characteristics of this phenomenon, such as excitation and relaxation time, the relation between deceleration and a material's quantity, and signal amplitude, are presented and analyzed. Although the underlying physics of this phenomenon is not yet known, we have shown that it has potential applications in remote identification of compounds, detection, and location sensing, as well as identifying substances that exist in plants without the need for any processing. This method is fast, accurate, low-cost, non-destructive, and non-invasive, making it a valuable area for further research that could yield spectacular results in the future.


Asunto(s)
Acetaminofén , Acetaminofén/análisis , Acetaminofén/química , Fenómenos Electromagnéticos , Aspirina/química , Aspirina/análisis , Preparaciones Farmacéuticas/química , Preparaciones Farmacéuticas/análisis , Ondas de Radio
3.
Biomed Chromatogr ; 37(4): e5585, 2023 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-36692333

RESUMEN

Analytical techniques must be sensitive, specific, and accurate to assess the active pharmaceutical ingredients in pharmaceutical dosage forms. The quality-by-design (QbD) application has proven to be a practical method for magnifying HPLC operations. This article discusses the successfully developed QbD-based stability-indicative LC method for evaluating acetaminophen, caffeine, and aspirin (ASP) in tablet dosage form. To achieve the necessary chromatographic separation, Milli-Q water, methanol, and glacial acetic acid were employed in the following ratios: 63:35:2 (v/v/v) for mobile phase A and 18:80:2 (v/v/v) for mobile phase B. The flow rate, column temperature, and detecting wavelength were 1.0 ml/min, 40°C, and 275 nm, respectively, and an InertSustain C18 analytical column (150 × 4.6 mm, 3 µm) was used. Linearity was between 10.0 and 150.0 µg/ml for ASP and acetaminophen and between 2.6 and 39.0 µg/ml for caffeine. The accuracy findings were more than 97%, and the correlation coefficient for all three components was found to be greater than 0.999. The validated HPLC method yielded reliable and accurate results. ASP was shown to be vulnerable to both acid and alkaline hydrolysis in the forced degradation study. The described method is capable of separating the degradants produced during stress testing and is regarded as stability indicating. The proposed method can be used for a wider range of other formulations with an appropriate diluent selection and sample preparation procedure optimization.


Asunto(s)
Acetaminofén , Cafeína , Acetaminofén/análisis , Cafeína/análisis , Comprimidos/química , Cromatografía Líquida de Alta Presión/métodos , Aspirina/análisis
4.
Fetal Diagn Ther ; 50(6): 406-414, 2023.
Artículo en Inglés | MEDLINE | ID: mdl-37487469

RESUMEN

INTRODUCTION: The Fetal Medicine Foundation (FMF) London developed a first trimester combined screening algorithm for preterm preeclampsia (pPE) that allows a significantly higher detection of pregnancies at risk compared to conventional screening by maternal risk factors only. The aim of this trial is to validate this screening model in the Swiss population in order to implement this screening into routine first trimester ultrasound and to prescribe low-dose aspirin 150 mg (LDA) in patients at risk for pPE. Therefore, a multicentre registry study collecting and screening pregnancy outcome data was initiated in 2020; these are the preliminary results. METHODS: Between June 1, 2020, and May 31, 2021, we included all singleton pregnancies with pPE screening at the hospitals of Basel, Lucerne, and Bern. Multiple of medians of uterine artery pulsatility index (UtA-PI), mean arterial pressure (MAP), placental growth factor (PlGF), and pregnancy-associated plasma protein A (PAPP-A) as well as risks were analysed as calculated by each centre's software and recalculated on the FMF online calculator for comparative reasons. Statistical analyses were performed by GraphPad Version 9.1. RESULTS: During the study period, 1,027 patients with singleton pregnancies were included. 174 (16.9%) had a risk >1:100 at first trimester combined screening. Combining the background risk, MAP, UtA-PI, and PlGF only, the cut-off to obtain a screen positive rate (SPR) of 11% is ≥1:75. Outcomes were available for 968/1,027 (94.3%) of all patients; 951 resulted in live birth. Fifteen (1.58%) developed classical preeclampsia (PE), 23 (2.42%) developed PE according to the International Society for the Study of Hypertension in Pregnancy (ISSHP) definition. CONCLUSION: First trimester combined screening for PE and prevention with LDA results in a low prevalence of PE. The screening algorithm performs according to expectations; however, the cut-off of >1:100 results in a SPR above the accepted range and a cut-off of ≥1:75 should be considered for screening. More data are needed to evaluate, if these results are representative for the general Swiss population.


Asunto(s)
Preeclampsia , Recién Nacido , Embarazo , Humanos , Femenino , Preeclampsia/diagnóstico por imagen , Preeclampsia/epidemiología , Suiza/epidemiología , Factor de Crecimiento Placentario , Primer Trimestre del Embarazo , Resultado del Embarazo , Aspirina/análisis , Arteria Uterina/diagnóstico por imagen , Flujo Pulsátil , Biomarcadores
5.
Biomed Chromatogr ; 35(2): e4986, 2021 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-33118207

RESUMEN

Two green, simple, and accurate chromatographic methods were developed and validated for the simultaneous determination of omeprazole and aspirin mixture in the presence of salicylic acid, a major impurity of aspirin. Method A is a reversed-phase ultra-high-performance liquid chromatography; the separation was performed on a C18 column, with a mobile phase composed of ethanol:0.1% aqueous solution of triethylamine acidified with orthophosphoric acid (pH 3) (30:70, v/v) at 0.15 mL/min flow rate and 230 nm. Omeprazole, aspirin, and aspirin impurity retention times were 7.47, 4.40, and 5.13 min, respectively. Good linearity was achieved in the concentration ranges of 5-80, 5-85, and 3-50 µg/mL for the three mentioned components, respectively. Method B is thin-layer chromatography (TLC) where silica gel TLC F254 plates were utilized to achieve separation using ethanol:ethyl acetate (2:8, v/v) as a developing system at 240 nm. The resulted Rf values were 0.83, 0.65, and 0.23 for omeprazole, aspirin, and impurity, respectively. The concentration ranges of 0.1-3 µg/band for the three drugs showed good linearity. The proposed methods are eco-friendly and greener when compared to the already reported method (Microchemical Journal, 152, 104350). This is the first use of TLC method for the determination of the three drugs. International Council for Harmonization (ICH) guidelines were followed to ensure the validity of developed methods.


Asunto(s)
Aspirina/análisis , Cromatografía Líquida de Alta Presión/métodos , Cromatografía en Capa Delgada/métodos , Contaminación de Medicamentos , Omeprazol/análisis , Tecnología Química Verde , Límite de Detección , Modelos Lineales , Reproducibilidad de los Resultados , Ácido Salicílico/análisis
6.
Mikrochim Acta ; 188(5): 179, 2021 04 29.
Artículo en Inglés | MEDLINE | ID: mdl-33914148

RESUMEN

A core-shell material (UiO@TapbTp) has been developed as an adsorbent and matrix to detect nonsteroidal anti-inflammatory drugs (NSAIDS) by matrix laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) in complex samples. The hybrid material is prepared by growing covalent organic framework (COF, TapbTp) layers in situ on an amino-modified metal-organic framework (MOF, UiO-66-NH2). The combination of the MOF and COF overcomes their individual shortcomings and integrates both of their advantages. Compared with the bare COF and MOF, the core-shell composite exhibits improved enrichment ability and matrix performance. With the help of pre-enrichment under optimized conditions, the limits of detection (LODs) for ketoprofen, naproxen, and aspirin are reduced by nearly 1000 times, with values of 0.001 mg L-1, 0.010 mg L-1, and 0.001 mg L-1, respectively, and the relative standard deviations (RSDs) are all below 12.35%. The good recoveries (84.8-118%) in (spiked) saliva and environmental water sample further verify the applicability of the method in complex samples.


Asunto(s)
Antiinflamatorios no Esteroideos/análisis , Aspirina/análisis , Cetoprofeno/análisis , Estructuras Metalorgánicas/química , Naproxeno/análisis , Adsorción , Antiinflamatorios no Esteroideos/química , Aspirina/química , Agua Potable/análisis , Cetoprofeno/química , Lagos/análisis , Límite de Detección , Naproxeno/química , Saliva/química , Espectrometría de Masa por Láser de Matriz Asistida de Ionización Desorción/métodos , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/química
7.
Int J Mol Sci ; 22(17)2021 Sep 04.
Artículo en Inglés | MEDLINE | ID: mdl-34502520

RESUMEN

In our previous study, we introduced the platelet endothelial cell adhesion molecule 1 (PECAM-1)/thrombus ratio, which is a parameter indicating the proportion of PECAM-1 in laser-induced thrombi in mice. Because PECAM-1 is an antithrombotic molecule, the higher the PECAM-1/thrombus ratio, the less activated the platelets. In this study, we used an extracorporeal model of thrombosis (flow chamber model) to verify its usefulness in the assessment of the PECAM-1/thrombus ratio in animal and human studies. Using the lipopolysaccharide (LPS)-induced inflammation model, we also evaluated whether the PECAM-1/thrombus ratio determined in the flow chamber (without endothelium) differed from that calculated in laser-induced thrombosis (with endothelium). We observed that acetylsalicylic acid (ASA) decreased the area of the thrombus while increasing the PECAM-1/thrombus ratio in healthy mice and humans in a dose-dependent manner. In LPS-treated mice, the PECAM-1/thrombus ratio decreased as the dose of ASA increased in both thrombosis models, but the direction of change in the thrombus area was inconsistent. Our study demonstrates that the PECAM-1/thrombus ratio can more accurately describe the platelet activation status than commonly used parameters such as the thrombus area, and, hence, it can be used in both human and animal studies.


Asunto(s)
Activación Plaquetaria/fisiología , Molécula-1 de Adhesión Celular Endotelial de Plaqueta/metabolismo , Molécula-1 de Adhesión Celular Endotelial de Plaqueta/fisiología , Animales , Aspirina/análisis , Plaquetas/metabolismo , Plaquetas/fisiología , Adhesión Celular , Células Endoteliales/metabolismo , Células Endoteliales/fisiología , Endotelio Vascular/citología , Femenino , Voluntarios Sanos , Humanos , Inflamación , Lipopolisacáridos/efectos adversos , Lipopolisacáridos/farmacología , Masculino , Ratones , Ratones Endogámicos C57BL , Trombosis/metabolismo
8.
Clin Chem Lab Med ; 59(2): 383-392, 2020 08 31.
Artículo en Inglés | MEDLINE | ID: mdl-32866112

RESUMEN

Objectives: Dual platelet inhibition is commonly used for prevention of cardiovascular events in patients undergoing neuroendovascular procedures. Non-responsiveness to platelet inhibitors may be associated with adverse outcomes. The aim of this study was to evaluate the reliability of the platelet function analyzer PFA-100® in comparison to light transmittance aggregometry (LTA) for monitoring clopidogrel and acetylsalicylic acid (ASA) non-responsiveness in a cohort of patients treated for intracranial aneurysm or cranial artery stenosis. Methods: Non-responsiveness to clopidogrel and ASA was assessed by LTA using adenosine diphosphate (ADP) and arachidonic acid and by PFA-100® with the ADP/prostaglandin E1 (PGE1) and collagen/epinephrine cartridges, respectively. Results: A total of 203 patients (145 females; median age, 57 years) were analyzed. Agreement between the two tests was poor for clopidogrel non-responsiveness (ƙ=0.19) and not better than chance for ASA non-responsiveness (ƙ=0.01). Clopidogrel non-responsiveness by LTA and PFA-100® was associated with higher von Willebrand factor antigen and activity levels. ADP-induced platelet disaggregation was lower in patients with clopidogrel non-responsiveness as assessed by PFA-100®. Clopidogrel non-responsiveness by LTA was associated with a higher prevalence of diabetes and a higher body mass index (BMI). Adverse outcomes (death, thromboembolism, or in-stent thrombosis) occurred in 13% (n=26) of all patients independently of ASA and clopidogrel non-responsiveness as assessed by both devices. Conclusions: Our results show that LTA and PFA-100® are not interchangeable in the assessment of ASA and clopidogrel non-responsiveness in patients undergoing neuroendovascular interventions.


Asunto(s)
Aspirina/análisis , Pruebas de Coagulación Sanguínea/métodos , Clopidogrel/análisis , Inhibidores de Agregación Plaquetaria/análisis , Adenosina Difosfato/metabolismo , Anciano , Alprostadil/metabolismo , Plaquetas/metabolismo , Colágeno/metabolismo , Epinefrina/metabolismo , Femenino , Humanos , Masculino , Persona de Mediana Edad , Agregación Plaquetaria , Valores de Referencia , Reproducibilidad de los Resultados , Stents , Evaluación de la Tecnología Biomédica , Trombosis/metabolismo , Factores de Tiempo
9.
Magn Reson Chem ; 58(11): 1018-1025, 2020 11.
Artículo en Inglés | MEDLINE | ID: mdl-31900955

RESUMEN

A combined experimental and computational approach was used to distinguish between different polymorphs of the pharmaceutical drug aspirin. This method involves the use of ab initio random structure searching (AIRSS), a density functional theory (DFT)-based crystal structure prediction method for the high-accuracy prediction of polymorphic structures, with DFT calculations of nuclear magnetic resonance (NMR) parameters and solid-state NMR experiments at natural abundance. AIRSS was used to predict the crystal structures of form-I and form-II of aspirin. The root-mean-square deviation between experimental and calculated 1 H chemical shifts was used to identify form-I as the polymorph present in the experimental sample, the selection being successful despite the large similarities between the molecular environments in the crystals of the two polymorphs.


Asunto(s)
Aspirina/análisis , Teoría Funcional de la Densidad , Cristalografía por Rayos X , Espectroscopía de Resonancia Magnética , Modelos Moleculares , Protones
10.
Chem Pharm Bull (Tokyo) ; 68(11): 1049-1054, 2020.
Artículo en Inglés | MEDLINE | ID: mdl-33132371

RESUMEN

To accelerate drug development, the pharmaceutical industry is working to shorten and improve studies on stability. The Accelerated Stability Assessment Program (ASAP) incorporating the humidity-corrected Arrhenius equation as an accelerated methodology has been proposed for both drug substances and drug products. In this study, the effect of magnesium stearate (MgSt) content on the chemical stability of acetylsalicylic acid was evaluated as a model system of drug-excipient compatibility studies using ASAP. In the acetylsalicylic acid powder blends, temperature and humidity showed a first-order linear response to the natural logarithm of the reaction rate constant, and MgSt content also showed a first-order linear response. A polynomial model was built in which temperature, humidity, and MgSt content were independent each other. The fitting index of the model, the coefficient of determination, was 0.9567, which was a good fit. In the long-term stability study (25 °C/60% relative humidity, 6 months), there was good agreement in total between measured values and model-predicted values. Using this model, we inferred that the degradation rates were depended on MgSt content at the fixed temperature and humidity because the micro-environmental pH of the excipient was catalytically affected. Applying this model equation can significantly reduce the duration of formulation design and stability studies and save time and costs in drug development.


Asunto(s)
Modelos Teóricos , Preparaciones Farmacéuticas/metabolismo , Ácidos Esteáricos/química , Aspirina/análisis , Aspirina/metabolismo , Estabilidad de Medicamentos , Humedad , Concentración de Iones de Hidrógeno , Cinética , Preparaciones Farmacéuticas/análisis , Polvos/química , Temperatura
11.
Biomed Chromatogr ; 33(10): e4608, 2019 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-31145484

RESUMEN

We developed novel stability-indicating HPLC method for simultaneous estimation of 14 impurities in excedrin tablet, a formulation with a combination of acetaminophen, aspirin, and caffeine. In addition, a new impurity that was generated through degradation of aspirin at high temperatures during the accelerated stability conditions was positively identified and confirmed, using liquid chromatography-mass spectrometry technique. The HPLC method was optimized using the Inertsustain C18 , 250 × 4.6 mm, 5.0 µm column, employing simple gradient method. Forced degradation studies were performed under acidic, basic, oxidative and thermal conditions to prove the scope and stability-indicating the nature of the method. The optimized method was validated as per the International Conference on Harmonization guidelines. The HPLC method showed linearity from LOQ concentration to 21 µg mL-1 . Precision and intermediate precision values were <5% RSD. The validated HPLC method is currently applied for the routine testing of excedrin tablet formulations in quality control laboratories.


Asunto(s)
Acetaminofén/análisis , Acetaminofén/química , Aspirina/análisis , Aspirina/química , Cafeína/análisis , Cafeína/química , Cromatografía Líquida de Alta Presión/métodos , Contaminación de Medicamentos , Combinación de Medicamentos , Límite de Detección , Modelos Lineales , Reproducibilidad de los Resultados
12.
Drug Dev Ind Pharm ; 45(2): 265-272, 2019 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-30307339

RESUMEN

Objective and Significance: Methocarbamol (MET) and aspirin (ASP) are widely used as a muscle relaxant combination. The USP reports guaifenesin (GUA) and salicylic acid (SAL) as related substances and hydrolytic products of MET and ASP, respectively. This work aimed at developing and validating a simple and sensitive RP-HPLC method for the determination of both drugs as well as their related substances (at their pharmacopeial limits) in their bulk powders, laboratory prepared mixtures, and MET-ASP combined tablets. Methods and Results: Chromatographic separation was achieved in less than 9 min with the required resolution, peak symmetry, and accuracy on C18 column using isocratic elution system of diluted acetic acid (pH 3.2): acetonitrile at the ratio of 79: 21, v/v, at a flow rate of 1 mL/min. Detection was achieved with photodiode array at 233 nm for MET, GUA, and SAL and at 273 nm for ASP. The developed method has been validated as per ICH guidelines and the calibration plots were linear over the concentration ranges of 2-150, 0.4-30, 25-450, and 0.2-27 µg/mL for MET, GUA, ASP, and SAL, respectively. Conclusion: The optimized method proved to be specific, robust and precise for the quality control of the studied drugs in pharmaceutical preparations to ascertain that their related substances are not exceeding the permitted pharmacopeial limits.


Asunto(s)
Aspirina/análisis , Metocarbamol/análisis , Ácido Acético , Acetonitrilos , Calibración , Cromatografía Líquida de Alta Presión , Combinación de Medicamentos , Guaifenesina/análisis , Límite de Detección , Polvos , Estándares de Referencia , Reproducibilidad de los Resultados , Ácido Salicílico/análisis , Comprimidos
13.
Molecules ; 23(12)2018 Nov 28.
Artículo en Inglés | MEDLINE | ID: mdl-30487409

RESUMEN

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50⁻9.00 µg/spot and 1.50⁻13.50 µg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.


Asunto(s)
Ácido Ascórbico/análisis , Aspirina/análisis , Densitometría/métodos , Sensibilidad y Especificidad
14.
Magn Reson Chem ; 55(6): 584-588, 2017 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-27930812

RESUMEN

Electrophoretic displacement of charged entity phase modulates the spectrum acquired in electrophoretic NMR experiments, and this modulation can be presented via 2D FT as 2D mobility spectroscopy (MOSY) spectra. We compare in various mixed solutions the chemical selectivity provided by 2D MOSY spectra with that provided by 2D diffusion-ordered spectroscopy (DOSY) spectra and demonstrate, under the conditions explored, a superior performance of the former method. 2D MOSY compares also favourably with closely related LC-NMR methods. The shape of 2D MOSY spectra in complex mixtures is strongly modulated by the pH of the sample, a feature that has potential for areas such as in drug discovery and metabolomics. Copyright © 2016 The Authors. Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.


Asunto(s)
Mezclas Complejas/análisis , Ensayo de Cambio de Movilidad Electroforética/métodos , Espectroscopía de Resonancia Magnética/métodos , Acetaminofén/análisis , Aminoácidos/análisis , Aspirina/análisis , Cafeína/análisis , Difusión , Concentración de Iones de Hidrógeno , Comprimidos
15.
Am J Forensic Med Pathol ; 38(4): 349-352, 2017 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-28795995

RESUMEN

We report the case of an 18-year-old woman with personality disorders who was hospitalized a few hours after suicidal ingestion of acetaminophen, quetiapine, acetylsalicylic acid, and ethanol. Twelve hours after admission, severe liver damage was evident, but the patient was stable and awaiting hepatic transplantation. Electrolytes were successfully controlled. The condition of the liver stabilized. Cardiac biomarkers then deteriorated unexpectedly. Localized ST-segment elevations were noted on electrocardiogram, but angiography ruled out myocardial infarction. A computed tomographic scan ruled out cerebral edema. The patient died of irreversible cardiac arrest 40 hours after admission. Heart failure remained unexplained, and the body underwent forensic autopsy.At autopsy, histologic findings were indicative of acute toxic myocarditis and were concluded to be caused by acetaminophen intoxication. Acetaminophen overdose is common and typically leads to liver failure requiring supportive treatment and emergency liver transplantation. Toxic myocarditis is an extremely rare complication of acetaminophen overdose. It has only been reported 4 times in the literature despite the widespread use and misuse of acetaminophen. Toxic myocarditis remains a possibility in many cases of overdose but can be overlooked in a clinical picture dominated by hepatorenal failure and encephalopathy. Clinicians and forensic pathologists should be aware of this rare potential complication.


Asunto(s)
Acetaminofén/efectos adversos , Analgésicos no Narcóticos/efectos adversos , Insuficiencia Cardíaca/etiología , Miocarditis/inducido químicamente , Suicidio , Acetaminofén/análisis , Adolescente , Analgésicos no Narcóticos/análisis , Antiinflamatorios no Esteroideos/efectos adversos , Antiinflamatorios no Esteroideos/análisis , Antipsicóticos/efectos adversos , Antipsicóticos/análisis , Aspirina/efectos adversos , Aspirina/análisis , Trastorno de Personalidad Limítrofe/psicología , Depresores del Sistema Nervioso Central/efectos adversos , Depresores del Sistema Nervioso Central/análisis , Sobredosis de Droga , Etanol/efectos adversos , Etanol/análisis , Femenino , Cromatografía de Gases y Espectrometría de Masas , Humanos , Fumarato de Quetiapina/efectos adversos , Fumarato de Quetiapina/análisis
16.
Anal Bioanal Chem ; 408(17): 4733-41, 2016 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-27108284

RESUMEN

In this contribution, the utility of sequential injection analysis in combination with surface-enhanced Raman spectroscopy (SERS) as a detection technique was investigated for simultaneous determination of aspirin and vitamin C in their pharmaceutical dosage forms and in spiked urine samples. The silver substrate was synthesized in situ by laser-induced photochemical procedure. By focusing the laser on a flow cell at 1 ml/min of continuous flow of 0.5 mM silver nitrate and 5 mM sodium citrate mixture, an active silver spot on the inner wall of the flow cell was prepared in a few seconds. The whole setup is fully computer controlled using ATLAS software to combine the two techniques. The system allows sequential determination of aspirin concentrations ranging from 100 to 500 ng/ml and vitamin C concentrations between 10 and 110 ng/ml with good precision of relative standard deviations (RSDs) of 0.85 and 1.7 %, respectively. A comparison of these results with those of the reported procedures showed excellent results compared with t and F values, indicating good accuracy and precision. The detection limits were 32 and 3 ng/ml for aspirin and vitamin C, respectively.


Asunto(s)
Ácido Ascórbico/análisis , Aspirina/análisis , Fotoquímica , Plata/química , Humanos , Límite de Detección , Microscopía Electrónica de Rastreo
17.
Anal Chem ; 87(10): 5263-9, 2015 May 19.
Artículo en Inglés | MEDLINE | ID: mdl-25860874

RESUMEN

We report on self-assembled nanocube-based plasmene nanosheets as new surface-enhanced Raman scattering (SERS) substrates toward direct identification of a trace amount of drugs sitting on topologically complex real-world surfaces. The uniform nanocube arrays (superlattices) led to low spatial SERS signal variances (∼2%). Unlike conventional SERS substrates which are based on rigid nanostructured metals, our plasmene nanosheets are mechanically soft and optically semitransparent, enabling conformal attachment to real-world solid surfaces such as banknotes for direct SERS identification of drugs. Our plasmene nanosheets were able to detect benzocaine overdose down to a parts-per-billion (ppb) level with an excellent linear relationship (R(2) > 0.99) between characteristic peak intensity and concentration. On banknote surfaces, a detection limit of ∼0.9 × 10(-6) g/cm(2) benzocaine could be achieved. Furthermore, a few other drugs could also be identified, even in their binary mixtures with our plasmene nanosheets. Our experimental results clearly show that our plasmene sheets represent a new class of unique SERS substrates, potentially serving as a versatile platform for real-world forensic drug identification.


Asunto(s)
Anestésicos Locales/análisis , Benzocaína/análisis , Oro/química , Nanoestructuras/química , Plata/química , Espectrometría Raman/métodos , Acetaminofén/análisis , Analgésicos no Narcóticos/análisis , Antiinflamatorios no Esteroideos/análisis , Aspirina/análisis , Ibuprofeno/análisis , Límite de Detección , Nanoestructuras/ultraestructura , Espectrometría Raman/instrumentación , Propiedades de Superficie
18.
Anal Bioanal Chem ; 407(19): 5649-59, 2015 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-26025549

RESUMEN

The use of the successive projections algorithm (SPA) for elimination of uninformative variables in interval selection, and unfold partial least squares regression (U-PLS) modeling of excitation-emission matrices (EEM), when under the inner filter effect (IFE) is reported for first time. Post-calibration residual bilinearization (RBL) was employed against events of unknown components in the test samples. The inner filter effect can originate changes in both the shape and intensity of analyte spectra, leading to trilinearity losses in both modes, and thus invalidating most multiway calibration methods. The algorithm presented in this paper was named iSPA-U-PLS/RBL. Both simulated and experimental data sets were used to compare the prediction capability during: (1) simulated EEM; and (2) quantitation of phenylephrine (PHE) in the presence of paracetamol (PAR) (or acetaminophen) in water samples. Test sets containing unexpected components were built in both systems [a single interference was taken into account in the simulated data set, while water samples were added with varying amounts of ibuprofen (IBU), and acetyl salicylic acid (ASA)]. The prediction results and figures of merit obtained with the new algorithm were compared with those obtained with U-PLS/RBL (without intervals selection), and with the well-known parallel factors analysis (PARAFAC). In all cases, U-PLS/RBL displayed better EEM handling capability in the presence of the inner filter effect compared with PARAFAC. In addition, iSPA-U-PLS/RBL improved the results obtained with the full U-PLS/RBL model, in this case demonstrating the potential of variable selection.


Asunto(s)
Algoritmos , Modelos Químicos , Acetaminofén/análisis , Aspirina/análisis , Fluorescencia , Ibuprofeno/análisis , Análisis de los Mínimos Cuadrados , Fenilefrina/análisis
19.
Guang Pu Xue Yu Guang Pu Fen Xi ; 35(5): 1271-5, 2015 May.
Artículo en Zh | MEDLINE | ID: mdl-26415442

RESUMEN

The projection algorithm used in mixture analysis to determine whether there is unknown disturbance existing in grey system can not accurately identify different samples and similar samples at the same time when it is used in the identification of drugs, because of the insufficient criteria. In the present study, one of its criteria for whether the size of measurement error of testing sample is at a limited level is improved for whether the size and distribution of measurement error is equal and similar between testing sample and standard sample. By testing 6 kinds of normal drugs (including BAYER Aspirin Enteric-coated Tablets, TYLENOL Acetaminophen Sustained Release Tablets, BAYER Compound Paracetamol Tablets(II), HUAZHONG Compound Vitamin C, HUAZHONG Vitamin B and MADINGLIN Demperidone Tablets) and 3 kinds of similar drugs of aspirin (including BAYER Aspirin Enteric-coated Tablets, Shanghai SINE Aspirin Enteric-coated Tablets and Bamyl Aspirin Effervescent Tablets), it was found that the un-improved projection algorithm directly used in discrimination of drugs shows poor performance with many problems existing, however, the improved projection algorithm can discriminate different drugs and similar drugs with accuracy up to 100%. The improved projection algorithm can be a universal, accurate and reliable automated pharmaceutical identification algorithm and can provide a reference for the study on identification of substance.


Asunto(s)
Algoritmos , Química Farmacéutica/métodos , Espectrometría Raman , Acetaminofén/análisis , Aspirina/análisis , Comprimidos
20.
Pak J Pharm Sci ; 28(5): 1631-6, 2015 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-26408883

RESUMEN

Norjizak is a new drug abused in the past few years in Iran with symptoms and complications distinct from other common forms of drug and characterized by higher rate of mortality. The present study aims to analyze the chemical components of this substance. Five samples were obtained from abusers referring from different areas of Tehran to a treatment clinic. All samples were 2 ml vials with yellowish fluid. Thin Layer Chromatography (TLC) was performed first to analyze the samples semi-quantitatively and the quantitative levels of components were then explored using high-performance liquid chromatography (HPLC). TLC revealed steroid (in form of betamethasone), heroin, codeine, morphine and thebaine in all five samples. Four samples contained acetaminophen and two samples contained caffeine. None of them contained amphetamine, benzodiazepine, tricyclic antidepressant, aspirin, barbiturates, tramadol and buprenorphine. HPLC revealed that heroin, codeine, morphine and thebaine constituted the narcotic foundation in all samples. In addition, the heroin to acetylcodeine ratio was significantly lower in three samples, which indicates their higher toxicity. The results of the present study on the chemical components of Norjizak showed that this substance is an opiate one similar to heroin and the heroin-based crack prevalent in Iran which contains betamethasone.


Asunto(s)
Aspirina/análisis , Cafeína/análisis , Orfenadrina/análisis , Betametasona/análisis , Cromatografía Líquida de Alta Presión , Cromatografía en Capa Delgada , Codeína/análisis , Combinación de Medicamentos , Heroína/análisis , Irán , Trastornos Relacionados con Sustancias
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