Spectrofluorimetric Determination of Fluoroquinolones in Honey with 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone in the Presence of β-cyclodextrin

Abstract

A simple and sensitive spectrofluorimetric method was developed for the determination of four fluoroquinolone antibacterials namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in honey through charge transfer (CT) complex formation with 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), and then the inclusion complexes of FQs-DDQ with β-cyclodextrin (β-CD) were formed, which resulted in drastic fluorescence enhancement. The effect of several parameters including the concentration of reactants, reaction temperature, time and ultrasonic treatment on the efficiency of the proposed method involving CT reaction and inclusion interaction was systematically investigated. Under the optimum conditions, the limits of detection (LODs) for four FQs in honey varied from 11.6 to 15.4 μg/kg (signal-to-noise ratio (S/N) = 3). The intra- and interday relative standard deviations (RSDs) were 1.6-4.0 % (n = 5) for four FQs. The calibration graph was linear from 42.8 to 1346.8 μg/kg with correlation coefficients not less than 0.9905. The recoveries of four FQs at three different spiked concentrations in honey samples ranged from 80.9 % to 92.8 %. The results indicated that the method was successfully applied for analyzing FQs in honey.

Simultaneous determination of 16 fluoroquinolone antibiotics in cosmetics by ultra-performance liquid chromatography/triple quadrupole mass spectrometry with ultrasound-assisted extraction and solid-phase extraction

“…As are shown in Table 3, the slope ratios range between 0.86 and 1.11 for the 16 FQs in lotion and cream matrices, indicating that the interfering substances in cosmetic samples were effectively eliminated through the SPE clean-up protocol. 20 …”

“…The cone voltage and collision energy for each MS/MS transition in the SRM mode were optimized individually and the optimum values are given in Table 1. Data acquisition was performed with multiple channels set 20 based on the retention time of each reference compound. Instrumentation control and data acquisition were operated by MassLynx and TargetLynx software, supplied with the instrument (Waters, Manchester, UK).…”

“…In many published literatures, acetonitrile in an acidic medium was widely adopted as the extraction solvent for the determination of FQs in food and environmental samples. [49][50][51][52][53] Considering the ionization efficiency and the compatibility with mass spectrometry, 20 acetonitrile forcified with formic acid solution, was employed.…”

High Throughput Quantitative Bioanalytical LC/MS/MS Determination of Gemifloxacin in Human Urine

“…Blank urine was then tested to ascertain the absence of any endogenous interference at the retention time of GFX and OFX. An eight-point calibration curve (5,15,25,50,150,200, 400 and 500 ng mL −1 ) was constructed by plotting the peak area ratio of GFX to OFX (IS) ( -axis) versus GFX nominal concentrations ( -axis). Analysis of calibration samples at each concentration was performed in triplicates.…”

“…An extensive literature survey revealed that several analytical methods have been reported for the determination of gemifloxacin in pharmaceutical preparations or human plasma or even in honey. Such methods are the various spectrophotometric techniques [16][17][18][19][20][21][22][23][24][25], capillary electrophoresis [26], high performance liquid chromatography [27][28][29][30][31][32][33][34][35][36], LC-mass spectrometry [37][38][39][40][41], microchip electrophoresis [42], chemiluminescence [43] and potentiometry [44] These methods were related to some major drawbacks such as having inadequate sensitivity, being time-consuming, tedious and sophisticated sample preparation. However, to the best of our knowledge, determination of GFX with complete validation in human urine has never been published.…”