Five sensitive, selective and precise spectrophotometric stability-indicating methods for the determination of fluconazole in the presence of its oxidative degradation product and in pharmaceutical formulations are developed and validated. Method A is a newly developed spectrophotometric one that is called ratio difference method by measuring the difference in amplitudes between 261.5 and 266.5 nm of ratio spectrum. Method B is a third derivative spectrophotometric one, which determines peak amplitudes from 265.5-268nm (peak-peak). Method C is ratio subtraction method. Method D is the first derivative of the ratio spectra by measuring the peak amplitude at 269 nm. Finally, method E is the mean centering of ratio spectra method by measuring the peak amplitude at 266.5 nm. The proposed methods allow the determination of fluconazole in the presence of its oxidative degradation product over a concentration range of 50-400 µg.mL -1 with mean percentage recoveries of 100.24±0.91, 99.91±0.52, 100.20±1.26, 99.79±0.69, and 100.77±0.72 respectively.The selectivity of the proposed methods is checked using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of fluconazole in pharmaceutical dosage forms without interference from other dosage form additives and the results have been statistically compared with a reported method.
A sensitive gas chromatographic method using an electron-capture detector (ECD) has been developed for the determination of tetraconazole and diniconazole fungicide residues in tomatoes and green beans. The developed method consists of extraction with methanol, partition with methylene chloride, and column chromatographic clean-up, followed by capillary gas chromatographic determination. The recoveries of both fungicides were greater than 90% for both plant samples. The limits of determination of the method were 0.001 ppm for both fungicides. The method was applied to determine residues and the rate of disappearance of tetraconazole and diniconazole from tomatoes and green beans [openˆeld treatment, 50 cc of Domark 10% EC (emulsiˆable concentrate), and 35 cc of Sumi-eight 5% EC; both for 100 l of water]. The fungicides incorporated into the plants decreased rapidly with a half-life around 3 days for diniconazole and from 4.5 to 6.5 days for tetraconazole. No residues could be detected in the plants during the period of study of 21 days afterˆeld application. Hence, the plants could be used safely after that period of time.
Two accurate and sensitive chromatographic methods have been developed and validated for simultaneous determination of cinnarizine (CIN) and dimenhydrinate (DIM). The first method uses simultaneous quantitative thin layer chromatography (TLC) spectrodensitometric evaluation of them, using ethyl acetate:methylene chloride (8 : 2 by volume) as a mobile phase. Chromatograms are scanned at 254 nm. This method analyzes CIN in a concentration range of 0.5-6 µg per band with mean percentage recovery of 99.78 ± 1.001 and DIM in a concentration range of 1-6 µg per band with mean percentage recovery of 99.87 ± 1.319. The second method is high-performance liquid chromatography using methanol:acetonitrile:water [85 : 10 : 5, by volume +0.5% tri ethyl amine (TEA)] as a mobile phase. The linearity was found to be in the range of 10-60 and 5-60 µg mL(-1) for CIN and DIM, respectively. The methods were successfully applied to the simultaneous determination of CIN and DIM in bulk powder, laboratory-prepared mixtures and pharmaceutical dosage forms. The validity of results was assessed by applying standard addition techniques. The results obtained are found to agree statistically with those obtained by a reported method, showing no significant difference with respect to accuracy and precision.
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.
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