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Development and validation of HPLC assay method for marbofloxacin determination in veterinary chewable tablets

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Oliveira K. R. W. , Sversut R. A. , Singh A. K. , Amaral M. S. , Kassab N. M.

2019

tom Vol. 31, no. 4

291--293

The present study aimed to develop and validate an analytical method for determination of marbofloxacin (MAR) in veterinary chewable tablets. The isocratic reversed-phase chromatographic method was developed and validated using a Vertisep®, RP C18 column (150 mm × 4.6 mm, 5.0 μm). The mobile phase was composed of water–acetonitrile (55:45, v/v) with pH adjusted to 3.0 with ortho-phosphoric acid and a flow rate set at 0.4 mL/min. The proposed method was validated for linearity in a concentration range of 2.5 to 17.5 μg/mL with a correlation coefficient of 0.99991. The mean content of MAR found in chewable tablets was 104.40% with RSD below 2%. The accuracy expressed as average recovery of the proposed method was 98.74%, and the precision expressed as relative standard deviation among repeated analysis was 0.55%. The method has adequate sensitivity with detection and quantitation limits of 0.25 and 0.81 μg/mL, respectively. Based on the presented results and according to the ICH and AOAC guidelines on validation of analytical methods, the proposed method was considered precise, accurate with adequate sensitivity, and robust in the MAR quantitative analysis. Therefore, the method can be used in the quality control of chewable veterinary tablets containing MAR.

Characteristics of Klebsiella pneumoniae harboring QnrB32, Aac(6’)-Ib-cr, GyrA and CTX-M-22 genes

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Wang D. , Wang H. , Qi Y. , Liang Y. , Zhang J. , Yu L.

nr 1

Simultaneous determination of six quinolone antibiotics in poultry and porcine samples by capillary electrophoresis

63%

Kowalski P. , Plenis A.

nr 1

A capillary electrophoresis (CE) method for the simultaneous determination of residues of six quinolones (enrofloxacin, ciprofloxacin, ofloxacin, lomefloxacin, norfloxacin, cinoxacin) in chicken, hen, and swine tissue samples were developed and validated. The sample preparation consisted of a solid phase extraction on C-18 cartridges prior to the analysis by CE with UV detection. The method was validated in terms of selectivity, linearity, precision, accuracy, recovery, and stability. The calibration curves were linear to at least 10-1 000 ng/g for all quinolones with r² > 0.999. The values of decision limits (CCα) and detection capabilities (CCβ) for the analysed substances were between 3.2-16.9 and 3.5-20.3 ng/g, respectively. The CE method was robust and specific, allowing reliable quantification of quinolone residues in animal tissues and should also be useful for clinical and biomedical investigations.