This work presents the development of a flow injection system for differential pulse amperometry (DPA) for diazepam determination in the presence of oxygen. The thin flow cell consisted of the bare glassy carbon electrode, reference silver/silver chloride, and stainless steel as the auxiliary electrode. Electrochemical reduction of diazepam (DZP) was characterised by cyclic voltammetry. Azomethine reduction peak was used for DZP quantification. The detector response was linear in the range 20–250 µmol/dm3 of diazepam, with a calculated detection limit of 3.83 µg/cm3. Intraday and interday precision were 1.53 and 10.8%, respectively. The method was applied on three beverage samples, energetic drink, and two different beer samples, and obtained recoveries were from 93.65 up to 104.96%. The throughoutput of the method was up to 90 analyses per hour.
A new glucose biosensor for selective and sensitive determination of glucose in beverage samples was developed. A copper complex with a Schiff base, N,N '-bis(acetylacetonato) propylenediimine, was used as a mediator. It was mixed with glucose oxidase (GOx) and prepared as carbon paste electrode (CPE). Cyclic voltammetry was used for electrochemical measurements. The biosensor showed improved sensitivity when enzyme mediator ratio was 1 : 5, and working pH was 6.6 in 0.1 M phosphate buffer. The linear response of the biosensor for glucose concentration was in the range from 0.5 to 10 mM, with low detection limit of 0.36 mM (calculated as 3 s/n) and sensitivity of 0.16 μA/mM. The reproducibility of the biosensor, calculated as relative standard deviation, was 1.9% for 6 intraday measurements. Biosensor was stored at + 4°C between experiments, and it was stable during 14 days after the preparation. The developed biosensor was applied on determination of glucose in commercial beverages (apple and cherry juice) and obtained results showed good agreement with the reference method.
The retention behavior and lipophilicity parameters of some antiphychotics were determined using reversed-phase thin layer chromatography. Quantitative structure-activity relationships studies have been performed to correlate the molecular characteristics of observed compounds with their retention as well as with their chromatographically determinated lipophilicity parameters. The effect of different organic modifiers (acetone, tetrahydrofuran, and methanol) has been studied. The retention of investigated compounds decreases linearly with increasing concentration of organic modifier. The chemical structures of the antipsychotics have been characterized by molecular descriptors which are calculated from the structure and related to chromatographically determinated lipophilicity parameters by multiple linear regression analysis. This approach gives us the possibility to gain insight into factors responsible for the retention as well as lipophilicity of the investigated set of the compounds. The most prominent factors affecting lipophilicity of the investigated substances are Solubility, Energy of the highest occupied molecular orbital, and Energy of the lowest unoccupied molecular orbital. The obtained models were used for interpretation of the lipophilicity of the investigated compounds. The prediction results are in good agreement with the experimental value. This study provides good information about pharmacologically important physico-chemical parameters of observed antipsychotics relevant to variations in molecular lipophilicity and chromatographic behavior. Established QSAR models could be helpful in design of novel multitarget antipsychotic compounds.
The objectives of this study were to gain insights into structure-retention relationships and to propose the model to estimating their retention. Chromatographic investigation of series of 36 Schiff bases and their copper(II) and nickel(II) complexes was performed under both normal- and reverse-phase conditions. Chemical structures of the compounds were characterized by molecular descriptors which are calculated from the structure and related to the chromatographic retention parameters by multiple linear regression analysis. Effects of chelation on retention parameters of investigated compounds, under normal- and reverse-phase chromatographic conditions, were analyzed by principal component analysis, quantitative structure-retention relationship and quantitative structure-activity relationship models were developed on the basis of theoretical molecular descriptors, calculated exclusively from molecular structure, and parameters of retention and lipophilicity.
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