Determination of chromatographic dissociation constants of some carbapenem group antibiotics and quantification of these compounds in human urine.

The dissociation constant values (s (s) pKa ) of some carbapenem group drugs (ertapenem, meropenem, doripenem) in different percentages of methanol-water binary mixtures (18, 20 and 22%, v/v) were determined from the mobile phase pH dependence of their retention factor. Evaluation of these data was performed using the NLREG program. From calculated pKa values, the aqueous pKa values of these subtances were calculated by different approaches. Moreover, the correlation established between retention factor and the pH of the water-methanol mobile phase was used to determine the optimum separation conditions. In order to validate the optimized conditions, these drugs were studied in human urine. The chromatographic separation was realized using a Gemini NX C18 column (250 × 4.6 mm i.d., 5 µm particles) and UV detector set at 220 and 295 nm.

Spectrophotometric determination of acidity constants of some macrolides in acetonitrile-water binary mixtures.

The acidity constants of eight macrolides (erythromycin, roxithromycin, oleandomycin, azithromycin, josamycin, tylosin tartrate, tilmicosin and spiramycin) have been determined in acetonitrile-water binary mixtures (30%, 40% and 50% (v/v)) by spectrophotometric method. The pKa's available in literature determined by various methods are compiled in comparison with the value of this work. These results are expected to essentially facilitate the research on occurrence, fate and effects, analysis method development, and control of antibiotics in various treatment occurrences.

Determination of pKa values of nonsteroidal antiinflammatory drug-oxicams by RP-HPLC and their analysis in pharmaceutical dosage forms.

In this study, pK(a) values were determined by using the dependence of the capacity factor on the pH of the mobile phase for four ionizable substances, namely, tenoxicam, piroxicam, meloxicam, and naproxen (I.S.). The effect of the mobile phase composition on the ionization constant was studied by measuring the pK(a) at different ACN concentrations, ranging from 30 to 40%. The adequate condition for the chromatographic determination of these compounds in pharmaceutical dosage forms was established based on the different retention behaviors of the species. An octadecylsilica Nucleosil C18 column (150 x 4.6 mm, 5 microm) was used for all the determinations. The chromatographic separation of oxicams was carried out using acetonitrile (ACN)/water at 35% v/v, containing 65 mM phosphoric acid and UV detection at a wavelength of 355 nm. The method developed was successfully applied to the simultaneous determination of these drug compounds in laboratory-prepared mixtures and their commercial pharmaceutical dosage forms. Each analysis requires no longer than 12 min.

Voltammetric Behaviour of Sulfamethoxazole on Electropolymerized-Molecularly Imprinted Overoxidized Polypyrrole.

In this work, preparation of a molecularly imprinted polymer (MIP) film and its recognition properties for sulfamethoxazolewere investigated. The overoxidized polypyrrole (OPPy) film was prepared by the cyclic voltammetric deposition of pyrrole (Py) in the presence of supporting electrolyte (tetrabutylammonium perchlorate-TBAP) with and without a template molecule (sulfamethoxazole) on a pencil graphite electrode (PGE). The voltammetric behaviour of sulfamethoxazole on imprinted and non-imprinted (NIP) films was investigated by differential pulse voltammetry (DPV) in Britton-Robinson (BR) buffer solutions prepared in different ratio of acetonitrile-water binary mixture, between the pH 1.5 and 7.0. The effect of the acetonitrile-water ratio and pH, monomer and template concentrations, electropolymerization cycles on the performance of the MIP electrode was investigated and optimized. The MIP electrode exhibited the best reproducibility and highest sensitivity. The results showed that changing acetonitrile-water ratio and pH of BR buffer solution changes the oxidation peak current values. The highest anodic signal of sulfamethoxazole was obtained in BR buffer solution prepared in 50% (v/v) acetonitrile-water at pH 2.5. The calibration curve for sulfamethoxazole at MIP electrode has linear region for a concentration range of 25.10-3 to 0.75 mM (R²=0.9993). The detection limit of sulfamethoxazole was found as 3.59.10-4 mM (S/N=3). The same method was also applied to determination of sulfamethoxazole in commercial pharmaceutical samples. Method precision (RSD87%) were satisfactory. The proposed method is simple and quick. The polypyrrole (PPy) electrodes have low response time, good mechanical stability and are disposable simple to construct.

Removal of phenol and chlorophenols from water with reusable dye-affinity hollow fibers.

Reactive Green HE 4BD carrying polyamide hollow fibers were investigated as dye-affinity adsorbents for removal of chlorophenols (i.e., phenol, o-chlorophenol, p-chlorophenol and 2,4,6-trichlorophenol). Adsorption rates of chlorophenols were very high. Equilibrium was achieved in about 30 min. The applicability of two kinetic models including pseudo-first order and pseudo-second order model was estimated on the basis of comparative analysis of the corresponding rate parameters, equilibrium capacity and correlation coefficients. Results suggest that chemisorption process could be the rate-limiting step in the adsorption process. The maximum adsorption values of chlorophenols onto the Reactive Green HE 4BD carrying hollow fibers were 145.9 micromol/g for phenol, 179.2 micromol/g for 2,4,6-trichlorophenol, 194.5 micromol/g for p-chlorophenol and 202.8 micromol/g for o-chlorophenol. The affinity order was as follows: o-chlorophenol>p-chlorophenol>2,4,6-trichlorophenol>phenol. The adsorption capacity of chlorophenols decreased with increasing pH. Desorption of chlorophenols was achieved using methanol solution (30%, v/v). The Reactive Green HE 4BD-carrying hollow fibers are suitable for repeated use for more than 10 cycles without noticeable loss of adsorption capacity.

Protective effects of N-acetylcysteine and erdosteine on hemorrhagic shock-induced acute lung injury.

BACKGROUND: The drugs N-acetylcysteine and erdosteine were used to evaluate their protective effects in hemorrhagic shock-induced acute lung injury in an animal model. METHODS: Forty rats were used and randomly allocated into four groups (n=10). Animals in group III were fed with water containing 1 mg/dl erdosteine, and those in group IV were given 0.5 mg/dl N-acetylcysteine 3 days before the experiment. Group I was taken as the control and group II was taken as the hemorrhagic shock group. Hemorrhagic shock was initiated by blood withdrawal and reduction of the mean arterial pressure to 40 mmHg within 10 min via the right carotid artery. After a hypotensive period of 2 h, animals were resuscitated by transfusion of the shed blood and Ringer lactate in a volume equal to the shed blood. After a period of 1 h, blood samples were taken via the carotid artery. Bronchoalveolar lavage was performed to recover cells from the alveolar space with 40 ml of bronchoalveolar lavage fluid. Lung tissues were also resected to measure tissue malondialdehyde and L-gamma-glutamyl-L-cysteinyl-glycine levels with high performance liquid chromatography. The numbers of neutrophils and alveolar macrophages in bronchoalveolar lavage fluid were counted. RESULTS: Serum malondialdehyde levels were significantly higher in the shock groups (P<0.05), but there was no significant difference (P>0.05). Lung malondialdehyde levels were also significantly increased in the shock groups (P<0.05). In the erdosteine-applied group, tissue malondialdehyde levels were lower than in group II and the NAC-applied group (P<0.05). In the analyses of serum and lung tissue L-gamma-glutamyl-L-cysteinyl-glycine, the values of groups I, II and IV were found to be below the calibration graphics. The alveolar macrophage count was found to be the highest and the neutrophil count the lowest in group III when compared with the other groups in bronchoalveolar lavage fluid analyses (P<0.05). CONCLUSION: We may say that in the model of hemorrhagic shock-induced acute lung injury, it was found that erdosteine has a protective effect on lung tissue.

Removal of chlorophenols from aquatic systems using the dried and dead fungus Pleurotus sajor caju.

In this study, the potential use of the fungus Pleurotus sajor caju to remove phenols (i.e., phenol, o-chlorophenol, p-chlorophenol and 2,4,6-trichlorophenol) from aqueous solutions was evaluated. Biosorption of phenol or chlorophenols reached equilibrium in 4 h. The maximum adsorptions of phenol and chlorophenols onto the Pleurotus sajor caju were 0.95 mmol/g for phenol, 1.24 mmol/g for o-chlorophenol, 1.47 mmol/g for p-chlorophenol and 1.89 mmol/g for 2,4,6-trichlorophenol. The affinity order was as follows: 2,4,6-trichlorophenol> p-chlorophenol> o-chlorophenol>phenol. Phenol and chlorophenols bindings onto Pleurotus sajor caju were clearly pH dependent. The adsorption of phenol and chlorophenols increased with increasing pH. Desorption was achieved using methanol solution (30%, v/v). Pleurotus sajor caju biomass is suitable for reuse for more than five cycles without noticeable loss of adsorption capacity.

Combined effect of polarity and pH on the chromatographic behavior of some angiotensin II receptor antagonists and optimization of their determination in pharmaceutical dosage forms.

In the present study, the combined effect of mobile phase polarity and pH on retention behavior of some ARA-IIs (irbesartan, losartan, valsartan and telmisartan) is investigated. The linear relationships established between retention factors of the species and the polarity parameter of the mobile phase has proved to predict accurately retention in LC as a function of the acetonitrile content (50%, 55%, 60%, v/v). The suggested model uses the pH value in the acetonitrile-water mixture as mobile phase instead of pH value in water and takes into account the effect of activity coefficients. Moreover, correlation between retention and the mobile phase pH can be established allowing prediction of the retention behavior as a function of the mobile phase pH. The model can be used to estimate the pKa in an acetonitrile percentage between 50% and 60%, at 30 degrees C. The developed method was successfully applied to both the simultaneous separation of these drug-active compounds and individual determination in their commercial pharmaceutical dosage forms.