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Abstract

A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank.

Open access
Acta Chromatographica
Authors:
Nabil N. Al-Hashimi
,
Rand O. Shahin
,
Amjad H. El-Sheikh
,
Malak J. Jibreel
,
Nada A. Alsakhen
,
Abdelrahim M. Alqudah
,
Muna K. Oqal
, and
Jafar I. Abdelghani

Abstract

The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R 2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument.

Open access

Abstract

Residues of the fungicides difenoconazole, propiconazole, cyflufenamid, and mandipropamid were determined in tomato fruit using acetonitrile for extraction and LC-MS/MS for quantification. Validation criteria include linearity range, the limit of detection (LOD) and limit of quantitation (LOQ), accuracy in terms of precision and trueness, and matrix effect were studied. The recovery rates of the method ranged from 91.8 to 106.3%. The precision of the method in terms of repeatability at one day (RSDr) and between three days (RSDR) ranged from 2.8 to 6.4% and from 4.3 to 7.6%, respectively, with good trueness from 92.2 to 96.4%. Matrix effects (suppression effects) ranged from 3.8% to 11.1%. The validated method was used to evaluate the dissipation kinetics of three different premix formulations: 30% EC (15% difenoconazole + 15% propiconazole), 14% DC (12.5% difenoconazole + 1.5% cyflufenamid), and 50% SC (25% difenoconazole + 25% mandipropamid) used on field tomatoes in Egypt. A first-order kinetic equation best describes residue dissipation. The calculated half-lives of difenoconazole, propiconazole, cyflufenamid, and mandipropamid were 2.01–2.27, 1.89, 1.97, and 1.71 days, respectively. The dissipation rate of difenoconazole did not differ significantly in the three premix formulations. Mandipropamid also dissipated faster compared to the other fungicides tested. The chronic dietary risk assessment results showed a minimal risk to adult Egyptian consumers. Waiting periods were advised for the safe consumption of tomatoes treated with the tested premix formulations.

Open access

Az azbesztszálak kimutatására szolgáló vizsgálatok középpontjában a levegőszennyezettségi értékek álltak, de a 21. században felmerült az igény a problémakör kiterjesztésére. Az elmúlt években megjelent nemzetközi tudományos szakirodalmak megcáfolták az évtizedeken át fennálló feltételezést, miszerint az azbeszt csupán a levegőterheltség révén vált ki kockázatot. Vízminőségi és talajminőségi kutatások által teret nyert az azbesztszálak, különösen a krizotilszálak alternatív transzportútjainak vizsgálatát célzó kutatásterület. Annak ellenére, hogy mind a települési, mind pedig a mezőgazdasági vízgazdálkodás potenciálisan érintett a krizotil-azbeszt jelenléte kapcsán, nincs nemzetközi szinten egységes és elfogadott módszer vagy küszöbérték az egyes vízforrások biztonságára vonatkozóan. A kutatások nyilvánvaló korlátja, hogy csekély mennyiségű és minőségű tudás érhető el. Az azbesztszálak megjelenése az egyes vízbázisokban jelentősen megváltoztatja mind a mezőgazdasági, mind a települési vízgazdálkodás környezeti hatásoknak való kitettségéről alkotott eddigi ismereteinket. Az öntözővizzel és a gyűjtött csapadékkal kijuttatott azbesztszálak hatásainak palettája mára túlhaladta a humán- és állategészségügyi hatásokat, immár figyelmet kell fordítani a vegetációs hatásokra is. Annak érdekében, hogy nagyobb betekintést nyerjünk az azbeszttoxicitás növényekre gyakorolt hatásaiba, sokkal több tudományos eredményre van szükség.

Jelen összefoglaló tanulmányban bemutatjuk az azbeszt, különös tekintettel a krizotil azbeszt legfontosabb tulajdonságait, humán-, állat- és növényegészségügyi kockázatait. Rávilágítunk arra, hogy ismereteink rendkívül hiányosak, valamint felhívjuk a figyelmet a települési és mezőgazdasági vízgazdálkodás érintettségének egyes faktoraira, közvetlen és közvetett kockázati tényezőire, valamint arra, hogy ezek miként hatnak az élőlényekre, kiemelt tekintettel a növényekre.

Open access
Agrokémia és Talajtan
Authors:
Andrea Balláné Kovács
and
János Kátai
Restricted access

Abstract

A novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect.

Open access