Determination of levetiracetam by GC-MS and effects of storage conditions and gastric digestive systems on drug samples.

Background: Epilepsy is a neurologic condition that is occurs globally and is associated with various degrees of seizures. Levetiracetam is an approved drug that is commonly used to treat seizures in juvenile epileptic patients. Accurate quantification of the drug's active compound and determining its stability in the stomach after oral administration are important tasks that must be performed. Results & methodology: Levetiracetam was extracted from drug samples and quantified by gas chromatography mass spectrometry using calibration standards. Stability of levetiracetam was studied under various storage conditions and in simulated gastric conditions. The calibration plot determined for levetiracetam showed good linearity with a coefficient of determination value of 0.9991. The limits of detection and quantification were found to be 0.004 and 0.014 µg·ml-1, respectively. The structural integrity of levetiracetam did not change within a 4-h period under the simulated gastric conditions, and no significant degradation was observed for the different storage temperatures tested. Discussion & conclusion: An accurate and sensitive quantitative method was developed for the determination of levetiracetam in drug samples. The stability of the drug active compound was monitored under various storage and gastric conditions. The levetiracetam content determined in the drug samples were within ±10% of the value stated on the drug labels.

Accurate and simple determination of oxcarbazepine in human plasma and urine samples using switchable-hydrophilicity solvent in GC-MS.

This work presents a sensitive and rapid analytical method for the determination of oxcarbazepine in human plasma and urine samples. A vortex-assisted switchable hydrophilicity solvent-based liquid phase microextraction (VA-SHS-LPME) was used to preconcentrate oxcarbazepine from the samples before the determination by gas chromatography mass spectrometry. The switchable hydrophilicity solvent was synthesized by protonating N,N-dimethylbenzylamine with carbon dioxide to make it totally miscible with an equivalent volume of water. Parameters of the VA-SHS-LPME method including volume of switchable hydrophilicity solvent, concentration/volume of sodium hydroxide and vortex period were systematically optimized. Under the optimum conditions, good linearity ranging from 27.03 to 353.47 µg/kg was obtained for the analyte. Limit of detection and quantitation values were found to be 6.2 and 21 µg/kg (mass base), respectively. The relative standard deviation was calculated as 6.9% for six replicate measurements of the lowest concentration of the calibration plot. Satisfactory recovery results were calculated in the range of 97-100% for human plasma and urine samples spiked at five different concentrations.

Sensitive determination of nickel at trace levels in surface water samples by slotted quartz tube flame atomic absorption spectrometry after switchable solvent liquid-phase microextraction.

In this study, switchable solvent (SS) for liquid-phase microextraction (LPME) was used as a tool to preconcentrate nickel from aqueous samples for determination by flame atomic absorption spectrometry. The SS-LPME method was optimized thoroughly to boost the absorbance signal of nickel for trace level determination. Parameters optimized included switchable solvent volume, sodium hydroxide concentration, sodium hydroxide volume, and eluent volume. The SS-LPME method enhanced the detection power by about 32-folds, and a slotted quartz tube (SQT) was used to obtain 2.6-folds increase in detection power. The combination of LPME and SQT-FAAS produced 104-folds enhancement, correlating to a limit of detection value of 1.8 µg/L. Low relative standard deviations calculated for the lowest calibration concentration indicated good repeatability for replicate measurements. Accuracy of the optimized method and its applicability to real samples was tested on two river samples. The results (85-103%) obtained from the spike recovery experiments were satisfactory.

A green, accurate and sensitive analytical method based on vortex assisted deep eutectic solvent-liquid phase microextraction for the determination of cobalt by slotted quartz tube flame atomic absorption spectrometry.

Preconcentration of cobalt was carried out with deep eutectic solvent based liquid phase microextraction (DES-LPME) for trace determination by a slotted quartz tube (SQT) attached flame atomic absorption spectrometry (FAAS) system. Choline chloride and phenol in a 1:2 M ratio was used as a green solvent to extract cobalt from the aqueous sample solution. Key parameters influencing the extraction efficiency of cobalt were examined and optimized. Under the conditions optimized, the linear dynamic range was found between 5.0 and 50 µg L-1, and the limits of detection and quantification (LOD and LOQ) were calculated as 2.0 and 6.6 µg L-1, respectively. The detection power of the conventional FAAS was improved upon by 67 folds using the optimized DES-LPME-SQT-FAAS method. The developed analytical method was successfully applied for the determination of cobalt in linden tea samples and the recovery results obtained for different spiked concentrations (20, 30 and 40 µg L-1) were remarkable (≈100%).

Oleic and stearic acid-coated magnetite nanoparticles for sonication-assisted binary micro-solid phase extraction of endocrine disrupting compounds, and their quantification by GC-MS.

Nanosized magnetic nanoparticles (MNPs) were utilized for the preconcentration of 12 analytes including pesticides, alkylphenols, hormones and bisphenol A prior to their determination by GC-MS. The extraction efficiency of the MNPs was enhanced by coating them with oleic acid and stearic acid. A binary system consisting of the two kinds of coated MNPs was optimized using a multivariate experimental design which evaluated main experimental variables and their interactions. Under optimized conditions, the following figures of merit are found: (a) Enrichment factors ranging from 64 to 345; (b) detection limits between 0.13 and 2.7 µg L-1; and (c) recoveries from spiked underground well water and municipal wastewater between 90 and 109%. The closeness of the results to 100% validated the method and underpinned its trueness for quantitative determinations. Graphical abstract Schematic representation of sonication-assisted binary micro-solid phase extraction based on oleic acid coated (OAc-) and stearic acid coated (SAc-) magnetite nanoparticles (MNPs) for the determination of endocrine disrupting compounds by GC-MS (TIC: total ion chromatogram).

Accurate and sensitive determination of lead in black tea samples using cobalt magnetic particles based dispersive solid-phase microextraction prior to slotted quartz tube-flame atomic absorption spectrometry.

Newly developed combination of magnetic cobalt particles based dispersive solid-phase microextraction (Co-MP-DSPME) and slotted quartz tube attached flame atomic absorption spectrometry (SQT-FAAS) was utilized to determine lead at trace levels in tea samples. Co-MPs' adsorbent properties were tested and validated for their selectiveness to lead. Only with a few and short extraction steps (i.e. adding MPs, mixing, decanting and eluting) analyte was extracted from sample solution rapidly and efficiently. Limit of detection (LOD) and limit of quantification (LOQ) for the developed method (Co-MP-DSPME-SQT-FAAS) were found to be 7.77 µg/L and 25.9 µg/L, respectively. Matrix matching strategy was performed and outcomes indicated that the developed method is applicable with the high percent recovery values of 110.1 ±â€¯4.5 and %102.9 ±â€¯4.2 for 100 and 300 µg/kg lead standard spiked black tea samples, respectively. The method was also applied to standard reference material to check the accuracy of the method.

A novel liquid-liquid extraction for the determination of naphthalene by GC-MS with deuterated anthracene as internal standard.

Polycyclic aromatic hydrocarbons are known for their carcinogenic and mutagenic effects on human health. This therefore calls for the regulation of their concentrations in air, water, and soil. Naphthalene as the simplest in structure of the polycyclic aromatic hydrocarbons is mainly used as a starter material for other chemicals but also has impacts on human health. A method is therefore proposed for the determination of naphthalene in water samples by gas chromatography mass spectrometry after liquid-liquid extraction. The extraction method was optimized to improve the extraction output, thereby lowering the limit of detection. The limits of detection and quantification obtained for naphthalene were 4.4 and 14.6 ng mL-1, respectively. Deuterated anthracene was used as internal standard to enhance the precision of the method, for which a relative standard deviation of 4.3% was obtained. The percent recovery of naphthalene obtained from tap water was ranged between 93.8 and 102.2.

Comparison of the concentration of trace metals (Ni, Zn, Co, Cu and Se), Fe, vitamins A, C and E, and lipid peroxidation in patients with prostate cancer.

The anticarcinogenic and antioxidant properties of vitamins A, C, E and pro- or antioxidant properties of trace metals have recently attracted increased attention. We examined the levels of antioxidant vitamins (A, C and E), selenium and malondialdehyde (MDA), and trace metals (Fe, Ni, Zn, Co and Cu) in patients with prostate cancer. In total, 41 subjects (21 controls and 20 prostate cancer patients) were included in the study. The levels of trace elements and Fe in whole blood were determined by atomic absorption spectrophotometry. Serum levels of Se were determined using a fluorimetric method, while a HPLC method was used for serum levels of vitamins and MDA. The levels of vitamins A and E were significantly lower and MDA levels were significantly higher (p<0.001) in patients with prostate cancer compared to controls. Serum vitamin C was significantly lower in patients with prostate cancer when compared to controls (p<0.01). Moreover, Se and Zn levels were also significantly lower, and levels of Ni, Co, and Cu were higher (p<0.001) in patients with prostate cancer than in controls. Fe levels were not significantly different in patients compared to controls (p>0.05). Our findings, together with the results of previous animal studies, suggest that the administration of vitamins A, C, and E, and Se and Zn may be beneficial in the prevention and treatment of human prostate cancer.