Fast concurrent determination of guaifenesin and pholcodine in formulations and spiked plasma using first derivative synchronous spectrofluorimetric approach.

Guaifenesin and pholcodine are frequently co-formulated in certain dosage forms. A new fast first derivative synchronous spectrofluorometric method has been used for their simultaneous analysis in mixtures. Here, first derivative synchronous spectrofluorometry enabled the successful simultaneous estimation of guaifenesin at 283 nm and pholcodine at 275 nm using a wavelength difference (Δλ) of 40 nm. The method was fully validated following International Council of Harmonization guidelines. For guaifenesin and pholcodine, linearity was determined within the corresponding ranges of 0.05-0.30 and 0.10-6.0 µg/ml. The two drugs were effectively analyzed using the developed approach in their respective formulations, and the results showed good agreement with those attained using reference methods. The method demonstrated excellent sensitivity, with detection limits down to 0.007 and 0.030 µg/ml and quantitation limits of 0.020 and 0.010 µg/ml for guaifenesin and pholcodine, respectively. Therefore, the procedure was successful in determining these drugs simultaneously in vitro in spiked plasma samples and syrup dosage form. The developed methodology also offered an environmentally friendly advantage by utilizing water as the optimal diluting solvent throughout the whole work. Different greenness approaches were investigated to ensure the method's ecofriendly properties.

Green quality by design HPLC approach for the simultaneous determination of Bilastine and Montelukast.

For the simultaneous estimation of two co-formulated antihistaminic drugs (Bilastine and Montelukast), a novel and eco-friendly reversed-phase HPLC approach with both diode array and fluorescence detection modes was designed. Rather than using the routine methodology, the Quality by Design (QbD) approach was adopted to speed up the method development and to test robustness of the method. To evaluate the effect of variable factors on chromatographic response, a full factorial design was used. The chromatographic separation was performed using isocratic elution on the C18 column. The mobile phase consists of 92% methanol, 6% acetonitrile, and 2% phosphate buffer with 0.1 (v/v) triethylamine adjusted to pH 3, it was pumped at a flow rate of 0.8 mL/min with an injection volume of 20 µL. The developed stability indicating HPLC approach was used to assess the stability of montelukast (MNT). It was subjected to a variety of stress conditions, including hydrolytic (acid-base), oxidative, thermal, and photolytic stress conditions. All of these conditions were found to have relevant degradation pathways. Under the described experimental conditions, MNT degradation followed pseudo-first-order kinetics. The kinetic parameters of its degradation (rate constant and t1/2) were calculated and a proposal for the degradation pathway was postulated.

A Design-assisted Spectrofluorometric Method Utilizing a One-pot Fluorescent Probe for the Quantitation of some Calcium Channel Blockers.

Based on their reaction with highly fluorescent carbon quantum dots (CQDts), a precise and reliable spectrofluorometric approach was developed for the determination of three calcium channel blockers. The studied drugs are: lercanidipine, nimodipine and nifedipine. (CQDts) were produced using a one-step hydrothermal method with ascorbic acid as the carbon source. The produced CQDts were capped by alcohol to create yellow emitters displaying a high fluorescence emission at 524 nm when excited at 325 nm. The fluorescence intensity of CQDts was noticeably quenched by each of the three calcium channel blockers. The relation between their concentrations and fluorescence quenching is linear over the concentration range of 0.5-20 µg/mL for each of the three drugs. A full factorial design was used to optimize the effect of variable factors. Therefore, under optimum experimental design conditions, the detection limits for lercanidipine, nimodipine, and nifedipine were 0.11 ± 1.09, 0.10 ± 0.25 and 0.12 ± 0.71 µg/mL, respectively. The LOQ was 0.33, 0.30, and 0.37 µg/mL respectively. The quenching of fluorescent CQDts occurred through the inner filter effect (IFE) for nimodipine, while it was mixed with dynamic quenching for lercanidipine and nifedipine. The proposed method was effectively used to determine the cited drugs in their pharmaceutical products and had an acceptable level of precision. The selectivity of the CQDts system towards the studied drugs was examined indicating no interference from interfering species.

Direct infusion nano-electrospray ionization mass spectrometry for therapeutic drug monitoring of ciprofloxacin and its metabolites in human saliva.

A rapid and sensitive method based on direct infusion-nano-electrospray ionization mass spectrometry (DI-nESI-MS) has been developed for the detection and quantification of ciprofloxacin and its metabolites in human saliva. Saliva samples were collected after the oral administration of 500 mg ciprofloxacin tablets. Internal standard (IS), tamoxifen, was added to the collected samples, and then diluted with the ionization solvent, centrifuged and filtered. An aliquot of 4 µL of the filtrate was loaded into a nanospray (NS) capillary. The NS capillary was then fitted into an off-line ion source and the instrument was operated to acquire a two-minute run by applying a voltage of 1000 V (positive-ion detection mode). Quantification of ciprofloxacin relied on the ratio of its peak intensity to the IS peak intensity. The DI-nESI-MS method was validated and provided satisfactory precision with relative standard deviation ranging from 0.39 to 7.48 % and accuracy with relative error ranging from -2.12 to 9.72 %. The calibration curve showed good linearity (r2) > 0.999 over the concentration range of 10-4000 ng/mL. These results verify the effectiveness of the DI-nESI-MS method for monitoring of ciprofloxacin and its metabolites in human saliva samples.