Electrochemical determination of rosiglitazone by square-wave adsorptive stripping voltammetry method

AbstractSquare-wave adsorptive stripping voltammetry technique was used to determine rosiglitazone (ROS) on the hanging mercury dropping electrode (HMDE) surface, in Britton Robinson buffer, pH=5. The voltammetric cathodic peak was observed at −1520mV vs. Ag/AgCl reference electrode. The voltammetric peak response was characterized with respect to pH, supporting electrolyte, accumulation potential, preconcentration time, scan rate, frequency, pulse amplitude, surface area of the working electrode and the convection rate. Under optimal conditions, the voltammetric current is proportional to the concentration of ROS over the concentration range of 5×10−8–8×10−7moll−1 (r=0.9899) with a detection limit of 3.2×10−11moll−1 using 120s accumulation time. The developed SW-AdSV procedure showed a good reproducibility, the relative standard deviation RSD% (n=10) at a concentration level of 5×10−7moll−1 was 0.33%, whereas the accuracy was 101%±1.0. The proposed method was successfully applied to assay the drug in the human urine and plasma samples with mean recoveries of 90±0.71% and 86±1.0%, respectively

Direct Enantiomeric Resolution of Betaxolol with Application to Analysis of Pharmaceutical Products

A high-performance liquid chromatographic (HPLC) method has been developed for the separation and determination of S- and R-enantiomers of betaxolol in tablets and ophthalmic preparations. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with fluorescence detection at excitation/emission wavelengths 275/305 nm. The polar ionic mobile phase (PIM) consists of methanol-glacial acetic acid-triethylamine, (100:0.020:0.025, v/v/v) has been used at a flow rate of 1.5 ml/min. All analytes with S-(–)-atenolol as internal standard were conducted at ambient temperature. The method is highly specific where another coformulated compounds did not interfere. The stability of betaxolol enantiomers under different degree of temperature also studied. The results showed that it is stable for at least 7 days at 70°C. The method validated for its linearity, accuracy, precision and robustness. Experimental design was used during validation to evaluate method robustness. Using the chromatographic conditions described, S- and R-betaxolol were well resolved with mean retention times of 11.3 and 12.6 min, respectively. Linear response (r > 0.997) was observed over the range of 10–500 ng/ml of betaxolol enantiomers, with detection limit of 5 ng/ml. The recoveries of S- and R-betaxolol from tablets and ophthalmic preparation ranged from 97.4 to 101.4% and 98.0 to 102.0%, respectively. The mean relative standard deviation (R.S.D.%) for both enantiomers were 1.1–1.4% and 1.3–1.7% in tablets and ophthalmic solution, respectively

Evaluation of some phenolic extracts against aphids (Aphis craccivora) Koch under laboratory conditions

Local farmers worldwide have complained in recent years that insect pests have become resistant to the majority of insecticides, owing to pesticide abuse. In addition, highly poisonous and harmful substances may cause health and environmental dangers. Friendly alternatives such as plant extracts are the main targets as substituents to synthetic pesticides. The present study aimed to extract total phenols from some plants and evaluate their efficacy on aphids, Aphis craccivora, under laboratory conditions. Four methanolic plant extracts from Punica granatum, Lantana camara, Portulaca oleracea and Ziziphus jujuba, containing phenolic components were evaluated against A. craccivora through: slide dipping, spraying, and leaf dipping techniques. Generally, positive relationships between the concentrations of the tested phenolic extracts and their mortality percentages were noticed in the case of slide dipping and spraying techniques. Conversely, no biological efficacy was found using the leaf dipping technique. The descending order of effectiveness of the tested extracts depending on their EC50 values was 0.017, 0.321, 1.142 and 16.114 ppm for Z. jujuba, P. oleraceae P. granatum and L. comara, respectively, in the case of the slide dipping technique. In contrast, P. granatum, L. camara, P. oleraceae and Z. jujuba had EC50 values of 0.0023, 0.017, 0.321 and 2.3409 ppm, respectively, in the case of the spraying technique. Additionally, a direct proportion was found between mortality percentages and treatment period for plant extracts under study with both techniques. After formulation and completion of additional essential field research, phenols isolated from the plants under study could be employed to combat A. craccivora

High-performance liquid chromatography and derivative spectrophotometry for simultaneous determination of pravastatin and fenofibrate in the dosage form

High performance liquid chromatography (HPLC) and second-order derivative spectrophotometry have been used for simultaneous determination of pravastatin (PS) and fenofibrate (FF) in pharmaceutical formulations. HPLC separation was performed on a phenyl HYPERSIL C18 column (125 mm 4.6 mm i.d., 5 m particle diameter) in the isocratic mode using a mobile phase acetonitrile/0.1 % diethyl amine (50:50, V/V, pH 4.5) pumped at a flow rate of 1.0 mL min–1. Measurement was made at 240 nm. Both drugs were well resolved on the stationary phase, with retention times of 2.15 and 5.79 min for PS and FF, respectively. Calibration curves were linear (R = 0.999 for PS and 0.996 for FF) in the concentration range of 5–50 and 20–200 µg mL–1 for PS and FF, respectively. Pravastatin and fenofibrate were quantitated in combined preparations also using the second-order derivative response at 237.6 and 295.1 nm for PS and FF, respectively. Calibration curves were linear, with the correlation coefficient R = 0.999 for pravastatin and fenofibrate, in the concentration range of 5–20 and 3–20 µg mL–1 for PS and FF, respectively. Both methods were fully validated and compared; the results confirmed that they were highly suitable for their intended purpose

CHEMICAL PROFILE OF TWO JASMINUM SAMBAC L. (AIT) CULTIVARS CULTIVATED IN EGYPT–THEIR MEDIATED SILVER NANOPARTICLES SYNTHESIS AND SELECTIVE CYTOTOXICITY

Objective: Evaluation of two Jasminum sambac L. (Ait) cultivars; Arabian Nights (JSA) and Grand Duke of Tuscany (JSG) ethanolic leaves extracts as reducing agents for the green synthesis of silver nanoparticles (AgNPs) and evaluation of their cytotoxicity against MCF-7 breast cancer and 5637 bladder cancer cell lines and chemical profiling of the two cultivars. Methods: The synthesis of silver nanoparticles (AgNPs) by the two cultivars and characterization of AgNPs by ultraviolet (UV)–visible spectroscopy, Transmission electron microscopy (TEM) and Fourier Transform Infrared Spectroscopy (FTIR). Additionally, the use of The high-performance liquid chromatography coupled with photodiode array-mass-mass-spectroscopy (HPLC-PDA-MS/MS) for chemical profiling of both cultivars and evaluation of total leaves extracts and corresponding nanoparticles towards MCF-7 and 5637 cell lines compared to aneuploidy immortal keratinocyte (Ha Cat) normal cells by neutral cell assay. Results: The green synthesized AgNPs (of an average size range of 8.83 and 11.24 nm for JSA and JSG, respectively) exhibited cytotoxicity against MCF-7 and 5637 cell lines. The IC50 was determined for each total extract JSA (15.29±2.16 μg/ml) and JSG (20.28±1.20 μg/ml) and corresponding AgNPs 17.32±2.22 μg/ml and 6.32±1.01μg/ml for JSA and JSG, respectively. The IC50 of JSA and JSG against 5637 bladder cancer cell line were 13.76±1.11 μg/ml and 50.69±3.75 μg/ml, while the corresponding AgNPs showed IC50 of 5.54±0.88 μg/ml and 27.89±2.84 μg/ml, respectively. The HPLC-PDA-MS/MS allowed the identification of 59 compounds; 10 simple phenols, 17 flavonoids; quercetin and kaempferol glycosides, 2 lignans, and 30 secoiridoids; oleuropein, molihauside, and sambacoside. Conclusion: This study proved that JSA is an excellent source for the synthesis of AgNPs with optimum characters and enhanced activities toward MCF-7 and 5637 cell lines in correlation to identified compounds

Određivanje donepezil hidroklorida u humanoj plazmi i ljekovitim oblicima pomoću HPLC s detekcijom fluorescencije

A sensitive, isocratic reversed-phase high performance liquid chromatographic method involving fluorescence detection was developed for the determination of donepezil hydrochloride in tablets and in human plasma. Pindolol was successfully used as an internal standard. Good chromatographic separation was achieved by using analytical column C18. The system operated at room temperature using a mobile phase consisting of methanol, phosphate buffer (0.02 mol L1) and triethyl amine (pH 3.5) (55: 45: 0.5 V/V/V) at a flow rate 0.9 mL min1. The analyte and internal standard were extracted from human plasma via liquid-liquid extraction. The proposed method was validated for selectivity, linearity, accuracy and precision. The calibration curve was linear over the range of 5-2000 ng mL1 of donepezil with detection limit of 1.5 ng mL1. Intra- and inter-day relative standard deviations were less than 2.5 %. The method was found to be suitable for the quality control of donepezil hydrochloride in bulk drug as well as in human plasma.Ovaj rad opisuje HPLC metodu određivanja donepezil hidroklorida (DP) u tabletama i u ljudskoj plazmi u nano području. Postavljena je osjetljiva metoda izokratične HPLC s fluorescencijskom detekcijom. Kao unutarnji standard upotrebljen je pindolol. Dobro kromatografsko odjeljivanje postignuto je primjenom analitičke kolone C18. Radna temperatura bila je sobna, a kao mobilna faza upotrebljena je smjesa metanola, fosfatnog pufera (0,02 mol L1) i trietilamina (pH 3,5) (55:45:0.5 V/V/V). Analit i unutarnji standard su ekstrahirani iz ljudske plazme ekstrakcijom tekuće-tekuće. Predložena metoda je validirana s obzirom na selektivnost, područje linearnosti, ispravnost i preciznost. Kalibracijska funkcija bila je linearna u području od 5-2000 ng mL1 donepezila, a granica detekcije iznosila je 2 ng mL1. Relativna standardna devijacija za repetabilnost i intermedijarnu preciznost bila je manja od 2,5 %. Metoda je primjenljliva u kontroli kvalitete ljekovitih formulacija s DP-om i u praćenju DP-a u ljudskoj plazmi

Honey, a Gift from Nature to Health and Beauty: A Review

Benefits of honey are contributed by the composition of its elements such as glucose, fructose, glucose oxidase, vitamins and phenolic compounds. For health, honey can be used to treat wounds due to the antibacterial activity conferred by the hydrogen peroxide produced by glucose oxidase in honey. Anti-inflammatory, anti-oxidant, deodorizing and tissue regeneration activities in honey also help in the wound healing process. It can also be an alternative sweetener for diabetic patients to ensure compliance to a healthy diet. Moreover, honey exerts several effects such as lowering low density lipids and increasing high density lipids, thus reducing risk of atherosclerosis. In terms of beauty, honey can be used on skin and hair. It moisturizes skin through its natural humectant properties contributed by high contents of fructose and glucose. Honey treats acne on the skin due to its antibacterial activity, anti-inflammatory action and tissue repair. The hair can benefit from honey in such a way that the hair has abundance, and becomes easier to comb. However, there have not been as many studies regarding the use of honey in skin in comparison to its use for health. Therefore, future studies on honey could research its use, action and benefits in both cosmetics and dermatology

Development of an HPLC method for the quantitation of bisoprolol enantiomers in pharmaceutical products using a teicoplanin chiral stationary phase and fluorescence detection

High performance liquid chromatography(HPLC) has become one of the most applied techniques in the chiral separation of different racemates.Several chiral stationary phases (CSPs) have been developed and used for the chiral separation of a variety of racemates. Among these CSPs, macrocyclic glycopeptide antibiotic based CSPs are very important as they have achieved an excellent reputation in the field of chiral separation. The importance of this type of CSPs includes its ease of use, reproducible results, and a wide range of applications.A selective high performance liquid chromatographic (HPLC) method was developed for the separation and quantification of bisoprolol enantiomers in pharmaceutical products. The method is highly specific where another coformulated drug, hydrochlorothiazide, did not interfere. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP), known as Chirobiotic T, with fluorescence detection at excitation/emission wavelengths 275/ 305 nm. The polar ionic mobile phase (PIM) consisting of methanol-glacial acetic acid-triethylamine, (100:0.020:0.025), (v/v/v) has been used at a flow rate of 1.5 mL/min. All analytes with S-(-)-atenolol as the internal standard were conducted at room temperature. The stability of bisoprolol enantiomers under different degrees of temperature was also studied. The results showed that the drug is stable for at least 7 days at 708C. The method was validated for its linearity, accuracy, precision, and robustness. An experimental design was used during validation to evaluate method robustness. The calibration curves were linear over the range of 5-250 ng/mL for each enantiomer, with a correlation coefficient of 0.999 for both enantiomers. The overall recoveries of S-(-)- and R-(+)-bisoprolol from pharmaceutical products ranged from 97.6 to 100.5% with %RSD ranging from 0.7 to 2.6%. The limit of quantification (LOQ) and limit of detection (LOD) for each enantiomer were 5 and 2 ng/mL, respectively. The method proved to be of chiral quality control for bisoprolol formulations by HPLC