Introduction Clomipramine is a tricyclic antidepressant acting as a serotonin reuptake inhibitor. Its maximum plasma concentration (Cmax) is 13–310 ng/mL, the therapeutic range is 220–500 ng/mL and its toxic effect appears in doses above 900 ng/mL. Objectives The fabrication of eco-friendly solid-contact ion-selective electrodes to evaluate the concentration of Clomipramine in different matrices based on disposable screen-printed carbon electrode. Methods Disposable screen-printed carbon electrode was utilized as a substrate to fabricate the proposed sensors. The sensors were optimized to determine Clomipramine using calix[4]arene as an ionophore into PVC polymeric membrane to enhance selectivity towards the target analyte. The solid-contact sensor potential stability was improved by the incorporation of graphene nanoparticles transducer layer. Results The sensors were assessed as per the IUPAC recommendations. The linearity range was 1 × 10− 2 to 1 × 10− 5.3 M. The sensors were successfully applied to determine CLM in the pharmaceutical formulation. Furthermore, the ion selective electrodes were applied for Clompiramine assay in spiked plasma for the purpose of Point-of-Care testing to be a diagnostic tool for therapeutic monitoring of the cited central nervous system agent. The findings were statistically compared to the reported method showing no statistically significant difference. Conclusion This work was concerned with developing a green analytical method for the determination of Clomipramine. The proposed SC-ISE was mixed with graphene nanocomposite transducer interlayer. The graphene layer succeeded in preventing the formation of an aqueous layer so resulted in a stable, reproducible standard potential besides the rapid response time.
Residues of veterinary drugs in poultry meat have serious health effects on humans (e.g., antimicrobial resistance, carcinogenicity, and hypersensitivity), which make the control of veterinary drug residues an important parameter in ensuring consumer protection. This work was performed to quantitatively determine two co‐formulated anti‐infective veterinary agents, tylosin tartrate (TYT) and doxycycline hydrochloride (DOX) in different tissues of broiler chickens (liver, muscles, and fat) using high performance liquid chromatography. The chicken was treated with the recommended dose of a binary mixture of the drugs (Tydovet). Moreover, the study aimed to estimate the withdrawal time of both drugs in chicken tissues. The analysis was done by solvent extraction and solid‐phase extraction for clean‐up of samples from the tissue matrix, followed by liquid chromatographic determination of the cited drugs with UV‐detection. Residue decline with time was tracked, and both antibiotics were found to be more persistent in liver tissues than other tissues (muscle and fat). The effect of freezing and cooking was investigated on tissue residue levels. While freezing had little effect on the concentration of both antibiotics; cooking, as anticipated, led to a marked decline. Therefore, it is recommended to pay attention to the proper withdrawal periods before marketing to ensure the hygienic suitability of broilers edibles for safe human consumption. Practical Application This novel study measures tylosin and doxycycline residues simultaneously in different tissues (muscle, fat, and liver) after administration of Tydovet powder to the broiler chicken. Residues in fat persisted for a longer time than in muscle in case of TYT, whereas the reverse was noticed in DOX.
Background Over the few previous years, mathematical manipulation proved to be a very powerful practice for successfully resolving severely overlapped spectra for various multicomponent mixtures. Objective Smart and environmentally friendly spectrophotometric determination approaches were conducted for two binary mixtures; of fixed dose veterinary injections containing Flunixin meglumine (FLU); combined with either Florfenicol (FLR), or Oxytetracycline HCl (OXY). Methods Regarding the first mixture, both FLU and FLR were determined by three successive resolution techniques which were; constant multiplication coupled with spectrum subtraction (CM-SS), derivative ratio (DD1),and ratio difference (RD),and two progressive resolution techniques which were absorbance subtraction (AS) and amplitude modulation (AM). In addition to graphical representation of concentration of the two drugs through concentration value (CNV) method. Concerning the second mixture, both FLU and OXY showed severely overlapped spectra and a comparative study was conducted for the determination of each drug by constant center (CC), ratio subtraction via amplitude difference coupled with spectrum subtraction (RS/AD-SS), constant value via amplitude difference (CV-AD), and advanced concentration value (ACV) method Results Calibration graphs of the first mixture were linear over the range of 5–40 µg/mL for FLU, and 3–40 µg/mL for FLR. The proposed methods overcame the problem of the overlapped spectra and presence of a minor component in mixture. Regarding the second mixture, calibration graphs were linear over the range of 2.5–24 µg/mL for FLU and 4–28 µg/mL for OXY. Conclusion The proposed methods were succesfully validated as per ICH guidelines. The obtained results were statistically compared with the official or reported methods showing no significant difference concerning accuracy and precision. The methods were evaluated for greenness by three different assessment tools; NEMI, analytical ecoscale, and GAPI. Highlights The methods were successfully applied for the simultaneous determination of the two combinations in synthetic mixtures and their marketed antibiotic veterinary injections; Megluflor® and Floxon®.
This work describes a simple and sensitive method for simultaneous determination of zolmitriptan, naproxen and propranolol in their dosage forms using HPLC. The drugs were separated isocratically on a Zorbax C8 (4.6 × 250 mm with 5 µm particle size) column using a mobile phase composed of 20 mM phosphate citrate buffer [0.1% TEA (pH 3.1)]:methanol:THF (5:3:2, by volumes). The detection was accomplished fluorometrically setting the excitation wavelength at 280 nm and emission wavelength at 360 nm. The method was validated over a linearity range of 100-900 ng/mL for zolmitriptan, 50-300 ng/mL for naproxen and 100-800 ng/mL for propranolol. The assay was successfully applied to the determination of the studied drugs in pharmaceutical dosage forms without interference from tablet excipients with high specificity. The method can be applied successfully in the future for the pharmacokinetic study of these drugs in the human plasma with high accuracy especially that LOQs of zolmitriptan and propranolol in the proposed method cover their Cmax.
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