Development of Carbon Nanotube-Polyamide Nanocomposite-based Stir Bar Sorptive Extraction Coupled to HPLC-UV Applying Response Surface Methodology for the Analysis of Bisphenol A in Aqueous Samples.

A novel nanocomposite based on reinforcing of multiwalled carbon nanotubes in polyamide (PA) was prepared by solvent exchange method as stir bar coating. The morphology and surface characteristic of PA and CNT/PA coated stir bars were investigated using scanning electron microscopy. The stir bar coated by CNT/PA nanocomposite was used as an extraction device for stir bar sorptive extraction of bisphenol A from aqueous samples followed by high performance liquid chromatography-UV detection. The effect of CNTs doping level and oxidation of CNTs on the extraction capability of the coating was investigated. Response surface methodology applying central composite design was used for modeling and optimization of important factors influencing the extraction and desorption processes including extraction time, salt and methanol content, desorption solvent, its volume and desorption time. Limit of detection and linear dynamic range of the method were 0.3 ng mL-1 and 1-10 ng mL-1, respectively. The method precision (RSD%) with four replicate determinations was 4.9% for distilled water at the concentration level of 10 ng mL-1 The obtained RSD% for reproducibility of stir bars was 7.4%. The developed method was successfully applied to the bottled mineral water samples, while the relative recoveries (RR%) were obtained to be in the range of 92.0-101.9%.

PVC membrane sensor for diclofenac: applications in pharmaceutical analysis and drug binding studies.

A PVC membrane sensor for diclofenac based on its ion pair complex with silver is prepared. The influences of membrane composition (PVC, plasticizer, and ion pair complex), pH of test solution and presence of other anions on the performance of the electrode were investigated. The optimized membrane demonstrates Nernstian response (-58.9 +/- 0.2 mV/decade) for diclofenac anions over a wide linear range from 5.2 x 10(-5) to 1.1 x 10(-2) M at 25 +/- 1 degree C. The potentiometric response is independent from pH at the range of 6.0-9.5. The advantages of the proposed sensor are: easy preparation, good selectivity and fast response time. It was successfully used for determination of diclofenac in pharmaceuticals and also in potentiometric study of interaction of diclofenac with bovine serum albumin. The results of diclofenac assay with the proposed sensor were in good agreement with the official HPLC method.

Mathematical representation of analyte's capacity factor in binary solvent mobile phases using the Jouyban-Acree model.

Applicability of a solution model, namely the Jouyban-Acree model, for mathematical representation of capacity factors of phenobarbital, phenytoin and carbamazepine in mobile phases containing water and the organic modifiers: methanol, acetonitrile, acetone and tetrahydrofuran and also a number of data sets collected from the literature has been shown. The accuracy of the proposed model is compared with those of the linear model and the quadratic equation using average percentage deviation (APD) as an accuracy criterion. The obtained mean and standard deviation of APDs of the Jouyban-Acree, linear and quadratic models are 8.1 +/- 8.4, 25.2 +/- 18.0 and 14.5 +/- 16.2%, respectively. The results showed that the Jouyban-Acree model provided more accurate calculations than the previously published models and the mean differences were statistically significant (p < 0.002).

A simple spectrophotometric method for determination of sodium diclofenac in pharmaceutical formulations.

A new, simple, rapid and accurate spectrophotometric method is proposed for determination of sodium diclofenac (SD) in pharmaceutical preparations based on its reaction with concentrated nitric acid (63% w/v). The reaction product is a yellowish compound with maximum absorbance at 380 nm. The corresponding calibration curve is linear over the range of 1-30 mg l(-1), while the limit of detection is 0.46 mg l(-1).