Easy sample treatment for the determination of enrofloxacin and ciprofloxacin residues in raw bovine milk by capillary electrophoresis

Abstract

An easy, selective, and sensitive method has been developed for the determination of enrofloxacin (ENR) and its main active metabolite, ciprofloxacin (CIP), in raw bovine milk using CE with UV detection at 268 nm. Milk samples were prepared by a clean-up/extraction procedure based on protein precipitation with hydrochloride acid followed by being defatted by centrifugation and SPE using a hydrophilic-lipophilic balance cartridge. Optimum separation was obtained using a 50 mM phosphoric acid at pH 8.4 and the total electrophoretic run time was 6 min. Sample preparation by this method yielded clean extracts with quantitative and consistent mean recoveries from 89 to 97% for CIP and from 93 to 98% for ENR. LODs obtained were lower to the maximum residue limits for these fluoroquinolones. The precision of the ensuing method is acceptable; thus, the RSD for peak area and migration time was less than 8.5 and 0.5% for CIP and 9.9 and 0.9% for ENR, respectively. The results showed that the proposed method was efficient showing good recoveries, sensitivity, and precision for the studied compounds and could be satisfactorily applied in routine analysis for the monitoring of ENR and CIP residues in milk, due to its ruggedness and feasibility demonstrated.

Detection of Enrofloxacin and Its Metabolite Ciprofloxacin Using Gold Nanoparticles and Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

“…The sensitivity of our method is comparable to ELISA and electrophoresis, and may not have an advantage over routine analytical methods such as HPLC, LC/MS, and ELISA in terms of sensitivity. [12][13][14][15][16][17][18][19][20][21][22][23] However, our approach is advantageous over these methods since it has a short assay time, a simple experimental protocol, and low background signals. We believe that our strategy has wide potential for use as a detection method for small molecules that have corresponding antibodies or capturing agents.…”

“…[9][10][11] Along with tightening up the regulations on FQ use, various analytical methods have been developed for determining or screening FQ residues, including high-performance liquid chromatography (HPLC), [12][13][14] liquid chromatography-mass spectrometry (LC/MS), 15,16 enzyme-linked immunosorbent assays (ELISA), [17][18][19][20] and capillary electrophoresis. [21][22][23] Although these methods are routinely used with high sensitivity, general use of these methods is sometimes hampered by the need for sophisticated and time-consuming processes. In this respect, a new method with a simple experimental protocol is demanded, while sustaining high sensitivity.…”

Simultaneous Determination of Four Antibiotics in Raw Milk by UPLC-MS/MS Using Protein Precipitation as Sample Preparation: Development, Validation, and Application in Real Samples

“…18,19 However, LC-mass spectrometry (MS), 18,20,21 based on triple quadrupole, 22,23 ion trap, 24 and quadrupole-orbitrap 25,26 systems have been replacing the aforementioned detection methods for unequivocal detections. 13 Additionally, electrochemical methods, 27 room temperature phosphorescence detection 28 and capillary electrophoresis 29 are also employed for such determinations. Due to the low concentrations of antibiotics in milk, sample preparation methods are typically required for pre-concentration of the analytes and the elimination of interferents.…”

Highly sensitive detection of five typical fluoroquinolones in low‐fat milk by field‐enhanced sample injection‐based CE in bubble cell capillary

“…It is necessary to develop analytical methods that are sensitive enough to monitor and determine these antibiotics at such a low level in bovine milk. Different strategies have been carried out to monitor residual levels of FQs in bovine milk including immunoassays [8][9][10], HPLC with optical [11][12][13] or MS [3,14] detection, and CE with electrochemical [15], UV [16,17], or MS [18,19] detection. Owing to its limitation in sensitivity, CE is not so commonly used as HPLC in the field of multiresidue separation and detection.…”