Prezentovaná práca sa zameriava na vývoj a validáciu analytickej metódy na báze kapilárnej zónovej elektroforézy v spojení s UV detekciou pre simultánne stanovenie tramadolu a paracetamolu vo farmaceutických a biologických vzorkách. Základný elektrolyt bol tvorený 50 mM uhličitanom amónnym, ktorý predstavuje pomerne atypický elektrolytový systém. Vyvinutá metóda disponuje vhodnými validačnými parametrami ako linearita (koeficient determinácie r2 ≥ 0,995), selektivita alebo medza dôkazu na úrovni 0,25 – 0,5 μg/ml. Metóda bola charakterizovaná adekvátnymi hodnotami presnosti a správnosti, ktoré boli v súlade s kritériami validačných smerníc, či už pre matrice farmaceutického alebo biologického charakteru. Detekcia bola uskutočnená pri vlnovej dĺžke 200 nm. Daná metóda bola úspešne použitá pre potreby stanovenia tramadolu a paracetamolu v rozličných liekových formách a v biologickej matrici moču. Dosiahnuté výsledky indikujú potenciál začlenenia metódy do procesov kontroly kvality liečiv a/alebo bioanalýzy.
The aim of the present study is the development and validation of a simple method based on capillary zone electrophoresis coupled with UV detection for simultaneous determination of tramadol and paracetamol in pharmaceutical and biological samples. The background electrolyte was composed of 50 mM ammonium carbonate, which is a type of a non-conventional electrolyte system. The developed method was characterized by suitable validation parameters, such as linearity (coefficient of determination r2 ≥ 0,995), selectivity or the limit of detection at the level of 0.25 – 0.5 μg/ml. Acceptable values of accuracy and precision were obtained, which were in good agreement with the recommended validation guidelines for analysis of pharmaceutical and biological samples. Detection was performed at a wavelength of 200 nm. The developed method was successfully applied to determine tramadol and paracetamol in various dosage forms and in urine biological samples. Achieved results indicate a potential of the method to be integrated in the common quality control processes of drugs and/or in bioanalysis.
The analytical performance of the clay paste electrode and graphene paste electrode was compared using square wave voltammetry (SWV) and cyclic voltammetry (CV). The comparison was made on the basis of a paracetamol (PA) determination on both working electrodes. The influence of pH and SWV parameters was investigated. The linear concentration ranges were found to be 6.0 × 10-7-3.0 × 10-5 and 2.0 × 10-6-8.0 × 10-5 mol L-1 for clay paste electrode (ClPE) and graphene paste electrode (GrPE), respectively. The detection and quantification limits were calculated as 1.4 × 10-7 and 4.7 ×10-7 mol L-1 for ClPE and 3.7 × 10-7 and 1.2 × 10-6 mol L-1 for GrPE, respectively. Developed methods were successfully applied to pharmaceutical formulations analyses. Scanning electron microscopy and energy-dispersive X-ray spectroscopy were used to characterize ClPE and GrPE surfaces. Clay composition was examined with wavelength dispersive X-ray (WDXRF).
Early stages of ontogenesis determining subsequent growth, development, and productivity of crops can be affected by wastewater and sludge contaminated with pharmaceuticals. Diclofenac (DCF) and paracetamol (PCT; both 0.0001 to 10 mg/L) did not affect seed germination and primary root length of onion, lettuce, pea, and tomato. Conversely, 20-day-old pea and maize plants exhibited decrease in biomass production, leaf area (by approx. 40% in pea and 70% in maize under 10 mg/L DCF), or content of photosynthetic pigments (by 10% and 60% under 10 mg/L PCT). Quantum yields of photosystem II were reduced only in maize (FV/FM and ΦII by more than 40% under 10 mg/L of both pharmaceuticals). Contents of H2O2 and superoxide increased in roots of both species (more than four times under 10 mg/L PCT in pea). Activities of antioxidant enzymes were elevated in pea under DCF treatments, but decreased in maize under both pharmaceuticals. Oxidative injury of root cells expressed as lowered oxidoreductase activity (MTT assay, by 40% in pea and 80% in maize) and increase in malondialdehyde content (by 60% and 100%) together with the membrane integrity disruption (higher Evans Blue accumulation, by 100% in pea and 300% in maize) confirmed higher sensitivity of maize as a C4 monocot plant to both pharmaceuticals.
- MeSH
- antioxidancia analýza MeSH
- chemické látky znečišťující vodu toxicita MeSH
- diklofenak analýza toxicita MeSH
- fotosyntéza účinky léků MeSH
- klíčení účinky léků MeSH
- kořeny rostlin účinky léků metabolismus MeSH
- listy rostlin účinky léků MeSH
- malondialdehyd analýza MeSH
- odpadní voda chemie MeSH
- paracetamol analýza toxicita MeSH
- peroxid vodíku analýza metabolismus MeSH
- semena rostlinná účinky léků fyziologie MeSH
- zemědělské plodiny účinky léků růst a vývoj MeSH
- Publikační typ
- časopisecké články MeSH
A new HPLC method for separation and determination of impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fenpiverinium bromide in combined suppository dosage form was developed and validated. The separation of paracetamol and its impurities 4-aminophenol, 4-nitrophenol, 4-chloracetanilid; codeine and its impurities methylcodeine, morphine, codeine dimer and 10-hydroxycodeine; pitophenone and its impurities 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl] benzoic acid, 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl]benzoic acid 2-(1-piperidinyl)-ethyl ester, methyl ester of 2-(4-hydroxybenzoyl) benzoic acid and fenpiverinium was achieved by using ion-pair reversed phase liquid chromatography with UV detection. Validation parameters such as the precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness were verified for all the mentioned impurities of codeine phosphate hemihydrate and 4-aminophenol and 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl] benzoic acid as the main degradation products of paracetamol and pitophenone hydrochloride, respectively. The described method was found to be useful for analysis of the stability samples and therefore suitable for routine purity testing of the drug product.
- MeSH
- benzofenony analýza MeSH
- chromatografie s reverzní fází MeSH
- čípky analýza MeSH
- kodein analýza MeSH
- kontaminace léku statistika a číselné údaje MeSH
- molekulární struktura MeSH
- paracetamol analýza MeSH
- piperidiny analýza MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
- validační studie MeSH
Labor aktuell, ISSN 1214-7672 2015, číslo 47, novinky
16 stran : ilustrace, tabulky ; 30 cm
- MeSH
- balení výrobků MeSH
- Hepadnaviridae MeSH
- hepatitida B - antigeny povrchové analýza imunologie MeSH
- hepatocelulární karcinom MeSH
- imunoanalýza metody přístrojové vybavení MeSH
- jaterní cirhóza MeSH
- paracetamol analýza MeSH
- referenční hodnoty MeSH
- sérum chemie imunologie MeSH
- techniky in vitro MeSH
- Publikační typ
- přehledy MeSH
- Konspekt
- Patologie. Klinická medicína
- NLK Obory
- hepatologie
- infekční lékařství
- diagnostika
A simple, rapid, and environmentally friendly HPLC method was developed and validated for the separation of four compounds (4-aminophenol, caffeine, paracetamol, and propyphenazone) with different chemical properties. A "green" mobile phase, employing water as the major eluent, was proposed and applied to the separation of analytes with different polarity on polyethylene glycol (PEG) stationary phase. The chromatography separation of all compounds and internal standard benzoic acid was performed using isocratic elution with a low-toxicity mobile phase consisting of 0.04% (v/v) triethylamine and water. HPLC separation was carried out using a PEG reversed-phase stationary phase Supelco Discovery HS PEG column (15 × 4 mm; particle size 3 μm) at a temperature of 30 °C and flow rate at 1.0 mL min(-1). The UV detector was set at 210 nm. In this study, a PEG stationary phase was shown to be suitable for the efficient isocratic separation of compounds that differ widely in hydrophobicity and acid-base properties, particularly 4-aminophenol (log P, 0.30), caffeine (log P, -0.25), and propyphenazone (log P, 2.27). A polar PEG stationary phase provided specific selectivity which allowed traditional chromatographic problems related to the separation of analytes with different polarities to be solved. The retention properties of the group of structurally similar substances (aromatic amines, phenolic compounds, and xanthine derivatives) were tested with different mobile phases. The proposed green chromatography method was successfully applied to the analysis of active substances and one degradation impurity (4-aminophenol) in commercial preparation. Under the optimum chromatographic conditions, standard calibration was carried out with good linearity correlation coefficients for all compounds in the range (0.99914-0.99997, n = 6) between the peak areas and concentration of compounds. Recovery of the sample preparation was in the range 100 ± 5% for all compounds. The intraday method precision was determined as RSD, and the values were lower than 1.00%.
- MeSH
- acetonitrily chemie MeSH
- aminofenoly analýza izolace a purifikace MeSH
- ethylaminy chemie MeSH
- fenazon analogy a deriváty analýza izolace a purifikace MeSH
- hydrofobní a hydrofilní interakce MeSH
- kalibrace MeSH
- kofein analýza izolace a purifikace MeSH
- methanol chemie MeSH
- paracetamol analýza izolace a purifikace MeSH
- polyethylenglykoly chemie MeSH
- reprodukovatelnost výsledků MeSH
- tablety analýza MeSH
- ultrafialové záření MeSH
- vysokoúčinná kapalinová chromatografie přístrojové vybavení metody normy MeSH
- Publikační typ
- časopisecké články MeSH
- práce podpořená grantem MeSH
