Fluoroquinolone analysis

Michaleas, S. and Antoniadou-Vyza, E. (2006) A new approach to quantitative NMR Fluoroquinolones analysis by evaluating the chemical shift displacements. J Pharm Biomed Anal, 42 (4), 405-410. 

Blanca-Lopez N, Ariza A, Dona I, Mayorga C, Montanez MI, Garcia-Campos J, et al. Flypersensitivity reactions to fluoroquinolones analysis of the factors involved. Clin Exp Allergy 2013 43(5) 560-7. 

GC-MS is applied in some methods for the analysis of pharmaceuticals in sludge [45, 109]. However, this technique can only be successfully applied for a limited number of nonpolar and volatile pharmaceutical compounds, while analysis of polar pharmaceuticals requires a time-consuming and often irreproducible deriva-tization. Consequently, LC-MS is the preferred technique in many laboratories. Some other detection techniques are also employed, such as diode array (DAD) and electrochemical (ED) and fluorescence detection (ELD). In the case of fluoroquinolones, ELD is still the favored technique. 

Animal and human studies support the use of antibiotics for the prevention of infectious morbidity and mortality in severe ANP. The most effective antimicrobial agents are the fluoroquinolones, imipenem-cilastatin, and metronidazole, which achieve adequate penetration into pancreatic juice and necrotic tissue and inhibit the growth of enteric bacteria. Although a recent meta-analysis [185] suggested that prophylactic antibiotic administration reduces sepsis and mortality and this approach has been recommended by recent guidelines and consensus state-... 

We have only found one example of the application of an immunoassay kit to the analysis of fluoroquinolones in environmental samples [84]. The assay is able to detect enrofloxcin as standard analyte with sensitivity levels of 5 pg L1. 

Schmitt-Kopplin, P., Burhenne, J., Freitag, D., Spiteller, M., and Kettrup, A. (1999). Development of capillary electrophoresis methods for the analysis of fluoroquinolones and application to the study of the influence of humic substances on their photodegradation in aqueous phase.. Chromatogr. A 837, 253-265. 

Recently, water-compatible imprinted monoliths were applied as specific sorbents for the analysis of fluoroquinolones in milk samples [198]. A pefloxacin-MIP monolith was prepared in capillaries by using MAA as functional monomer, di(ethylene glycol) dimethacrylate as a cross-linker and methanol-water as the porogenic solvent. The MIP monolith showed recognition properties in an aqueous environment for several fluoroquinolones with recoveries above 90%, with a relatively high non-specific adsorption on the NIP. Nevertheless, HPLC analysis of spiked milk after MIP-microextraction presents no interfering peak compared to a traditional C18-SPE. 

In recent years antibiotics residues have accumulated in different environmental compartments. Fluoroquinolone antibiotics are strongly adsorbed by soil, and therefore their extraction requires exhaustive procedures, leading to complex extracts due to coextraction. Despite this the authors succeeded in selectively detecting the fluoroquinolones from crude soil extracts directly injected onto an MIP HPLC column and using UV detection [Fig. 2 (Fig. 6 of the original)]. Recoveries close to 100% were obtained for five fluoroquinolones. The analysis time was only a few minutes, so this method was found suitable for screening soil samples for the presence of fluoroquinolones. The individual fluoroquinolones were not resolved on the column. 

Fig. 2 Chromatograms obtained in the analysis of (a) a soil crude extract spiked with 0.5 pg g-1 of the fluoroquinolone antibiotic ciprofloxacin (CIP), (b) non-spiked soil extract, and (c) a standard solution of 0.5 pg g 1 of CIP prepared in methanol [43]...

Fig. 3 Chromatograms obtained in the analysis of a soil sample extract spiked with 0.1 pg g 1 of the selected fluoroquinolones (a) with and (b) without performing MISPE. Peak assignment 1 = enoxacin (ENO), 2 = norfloxacin (NOR), 3 = ciprofloxacin (CIP), 4 = danofloxacin (DAN), 5 = enrofloxacin (ENR) [43]...

Turiel E, Martin-Esteban A, Tadeo JL (2007) Molecular imprinting-based separation methods for selective analysis of fluoroquinolones in soils. J Chromatogr A 1172(2) 97-104... 

Leone R, Venegoni M, Motola D, Moretti U, Piazzetta V, Cocci A, Resi D, Mozzo F, Velo G, Burzilleri L, Montanaro N, Conforti A. Adverse drug reactions related to the use of fluoroquinolone antimicrobials an analysis of spontaneous reports and fluoroquinolone consumption data from three Italian regions. Drug Saf 2003 26 109-20. 

If analysis of the frequency of adverse events is based on prescription event monitoring (PEM), the rates of adverse events are usually substantially lower. In one study, over 11 000 patients taking each antibiotic were monitored (19). Among the fluoroquinolones, ciprofloxacin, norfloxacin, and ofloxacin were used. Adverse events resulted in withdrawal of norfloxacin or ofloxacin in under 1% of patients (19). 

A polyurethane was synthesised from 1,6-hexane diisocyanate, polycaprolactone diol and a fluoroquinolone antibiotic, ciprofloxacin and characterised by size exclusion chromatography and elemental analysis. The PU was incubated in a solution of an inflanunatoiy cell-derived enzyme, cholesterol esterase or phosphate buffer for 30 days at 37C and its biodegradability determined by HPLC, mass spectroscopy and Carbon 14 radiolabel release. Analysis of the solution revealed that ciprofloxacin was released and able to inhibit the growth of Pseudomonas aeruginosa. 53 refs. 

Cyclization of benzoyl acrylates 174 to condensed fluoroquinolones 180 takes place via intermediates 179, which are not always isolated because of the fast closure of the thiadiazine ring. The structure of tricyclic fluoroquinoline 180 (R = thiomorpholin-l-yl) was established by X-ray analysis. 

While mainly used as a qualitative technique for identification, NMR has been used for quantitative analysis. Examples include the determination of glyphosate in biological fluids, ions in serum and fluoroquinolones in aqueous samples . 

Tables 2.20 and 2.21 present estimated data for sales of AMDs for treatment and prevention of BRD in three countries and the EU, together with an analysis of major products used in the United States. The market is dominated by the United States and EU, which together account for 63% of the global BRD market. The US market is dominated by two products containing macrolides (53% of total), three products containing ceftiofur (22.5% of total), and two products containing fluoroquinolones (21.5% of total). While florfenicol has a much smaller percentage share, it is nevertheless signiflcant in view of the market...

Turnipseed et al. described a method for the multi-class residue determination of P-Iactams, sulfonamides, tetracyclines, fluoroquinolones, and macroiides in milk and other dairy products. The sample preparation combines extraction with acetonitrile, clean-up with Oasis HLB cartridges, and ultrafiltration using molecular weight cut-off filters to improve the overall performance of the analysis. Acceptable recoveries were obtained for sulfanomides, macroiides, and quinolones (>70%) however, recoveries were rather low for tetracyclines (50-60%) and P-lactams (<50%). Despite the extensive clean-up procedure, significant matrix ion suppression was observed for many compounds, making it necessary to include matrix-matched calibration standards for quantification purposes. 

Other applications of MIPs have been described by Hung and Hwang for the analysis of sulfonamides and by Turiel et al. for the analysis of fluoroquinolones in soil. 

Zheng MM, Gong R, Zhao X, Feng, YQ, Selective sample pretreatment by molecularly imprinted polymer monolith for the analysis of fluoroquinolones from milk samples, J. Chromatogr A 2010 1217 2075-2081. 

Heller D, Nochetto CB, Rumel NG, Thomas MH, Development of multi-class methods for drug residues in eggs hydrophilic solid-phase extraction clean-up and liquid chro-matography/tandem mass spectrometry analysis of tetracycline, fluoroquinolone, sulfonamide, and -lactam residues, J. Agric. Food Chem. 2006 54 5267-5278. 

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