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A simple and reliable novel kinetic method for the determination of piroxicam (PX) was proposed and validated. For quantitative determination of PX, the Bray-Liebhafsky (BL) oscillatory reaction was used in a stable non-equilibrium stationary state close to the bifurcation point. Under the optimized reaction conditions (T = 55.0°C, [H2SO4]0 = 7.60×10−2 mol L−1, [KIO3]0 = 5.90×10−2 mol L−1, [H2O2]0 = 1.50×10−1 mol L−1 and j 0 = 2.95×10−2 min−1), the linear relationship between maximal potential shift ΔE m , and PX concentration was obtained in the concentration range 11.2–480.5 µg mL−1 with a detection limit of 9.9 µg mL−1. The method had a rather good sample throughput of 25 samples h−1 with a precision RSD = 4.7% as well as recoveries RCV ≤ 104.4%. Applicability of the proposed method to the direct determination of piroxicam in different pharmaceutical formulations (tablets, ampoules and gel) was demonstrated. [...]
A simple and highly sensitive spectrofluorometric method was developed for the determination of some 1,4-dihydropyridine compounds namely, nicardipine, nifedipine and isradipine in pharmaceutical preparations and biological fluids. The method is based on the reduction of nicardipine, nifedipine and isradipine with Zn/HCl and measuring the fluorescence intensity obtained (λem/λex) at 460/364, 450/393 and 446/360 nm, respectively. The factors affecting the development of the fluorophore and its stability were studied and optimized. The effect of some surfactants such as β-cyclodextrin (βCD), carboxymethylcelullose (CMC), sodium dodecyl sulphate (SDS) and triton X-100, on the fluorescence intensity was studied. The fluorescence intensity-concentration plots of nicardipine, nifedipine and isradipine were rectilinear over the ranges 0.4–6.0, 0.2–4.0 and 0.1–9.0 μg ml−1 with detection limits of 0.0028, 0.017 and 0.016 μg ml−1, respectively. The proposed method was successfully applied to commercial tablets containing the compounds; the percentage recovery agreed well with those obtained using the official methods. The method was further extended to the in vitro determination of the compounds in spiked human plasma and urine samples. A proposal of the reduction reaction pathway was postulated. [...]
An efficient ion chromatographic (IC) method was developed for the simultaneous quantitative determination of Li+, Na+, NH4+, K+, Cs+, Ca2+, Mg2+, Sr2+, Ba2+ and Be2+ in energy drinks, pharmaceutical and drinking water samples by non-suppressed conductometric detection. The separation of ten cations including ammonium was achieved using a cation-exchange column and low conductivity mobile phase. The mobile phase consisted of tartaric acid, dipicolinic acid and boric acid. The separation of the cations was completed in less than 18 min, with a flow rate of 1.2 mL min−1. The separation was not affected by the existence of cations Co2+, Cr3+, Cd2+, Cu2+, Bi3+, Ag+, Fe3+ and Zn2+ in concentrations up to 20 mg L−1. Using an injection volume of 20 μL the obtained detection limits were 0.003 mg L−1, 0.02 mg L−1, 0.01 mg L−1, 0.01 mg L−1, 0.10 mg L−1, 0.01 mg L−1, 0.02 mg L−1, 0.02 mg L−1, 0.003 mg L−1 and 0.1 mg L−1, for Li+, Na+, NH4+, K+, Cs+, Ca2+, Mg2+, Sr2+, Be2+ and Ba2+ respectively. The intra-day repeatability (RSD%, n=5) ranged from 1.1% to 4.8%, and the inter-day (n=5) between 1.8% and 5.4% respectively. The method was applied to the analysis of various bottled and tap water, pharmaceutical preparations and energy drinks commercially available. [...]
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