TLC-DB as an Alternative to the HPLC Method in the Determination of Cefacetril Residues in Cow's Milk

Choma, Irena; Kowalski, C.; Lodkowski, R.; Burmańczuk, Artur; Komaniecka, Iwona

doi:10.1080/10826070802194815

Cited by 18 publications

(9 citation statements)

References 11 publications

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“…The proteins can be removed by, e.g. the addition of organic solvents, such as: ethanol [14], acetonitrile [16,19], trichloroacetic acid [15,17,20] or trifluoroacetic acid [21], sometimes with addition of strong mineral alkali or heavy metals. In this studies seventeen various procedures of deproteinization of milk samples were tested.…”

Section: Resultsmentioning

confidence: 99%

“…In this studies seventeen various procedures of deproteinization of milk samples were tested. Some of them were taken from the literature [14][15][16][17] or were their modifications, the others were the original ones. A few of procedures were rejected almost immediately, because of insufficient protein denaturation.…”

Section: Resultsmentioning

confidence: 99%

“…Some of them were already known from the literature [14][15][16][17]. We tested both those procedures and their modifications as well as original, new procedures.…”

Section: Introductionmentioning

confidence: 99%

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Comparison of Deproteinization Methods Used Before TLC-DB and HPLC Analysis of Flumequine Residues in Milk

Choma

Grzelak²,

Majer³

et al. 2012

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Seventeen various extraction procedures based on precipitation of proteins in milk samples spiked with flumequine were tested. Several criteria were taken into account, when choosing the most effective. The supernatants were analyzed by thin-layer chromatography direct bioautography (TLC-DB) and high performance liquid chromatography (HPLC-UV). The results obtained from both methods indicate as the best the same deproteinization procedure. The addition of acetonitrile to milk in 1:1 volume proportions gave the highest concentration of flumequine in supernatant and prompt coagulation of proteins in milk samples.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

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Comparison of Deproteinization Methods Used Before TLC-DB and HPLC Analysis of Flumequine Residues in Milk

Choma

Grzelak²,

Majer³

et al. 2012

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“…Sample pre‐treatment techniques used for the isolation of cephalosporins from various matrices are usually SPE, liquid‐liquid extraction and dilution 5–10.…”

Section: Introductionmentioning

confidence: 99%

“…The prevailing analytical technique for the determination of cephalosporins in various matrices (food, biofluids and pharmaceutical tablets) is LC 5–8, 22–25. Other analytical techniques reported in the literature for the determination of cephalosporins are HPLC‐FIA 26, TLC‐direct bioautography 9, a chemiluminescence micro‐flow system combined with on‐line SPE 10 and finally a surface plasmon resonance‐based biosensor 27.…”

Section: Introductionmentioning

confidence: 99%

Application of ultrasound‐assisted matrix solid‐phase dispersion extraction to the HPLC confirmatory determination of cephalosporin residues in milk

Karageorgou

Samanidou

2010

J of Separation Science

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Ultrasound-assisted matrix solid-phase dispersion (MSPD) was applied to isolate eight cephalosporins (cefadroxil, cefaclor, cephalexin, cefotaxime, cefazolin, cefuroxime, cefoperazone and ceftiofur) from milk. Multi-residue analysis was subsequently performed by HPLC-diode array detection. Extraction yield by matrix solid-phase dispersion using Nexus sorbent was higher than various investigated SPE protocols. Three analytical columns, two conventional silica based and one monolithic, were compared based on resolution, peak shape and retention time. The optimum method using Chromolith RP-18e (100×4.6 mm) achieved separation in less than 16 min. Method validation was performed according to the European Union Decision 2002/657/EC, determining linearity, selectivity, stability, decision limit, detection capability, accuracy and precision. RSD values observed were lower than 15.3%. Recovery rates of examined antimicrobials from milk ranged from 93.8 to 101.9% for cefadroxil, from 94.7 to 103.6% for cefaclor, from 93.4 to 106.6% for cephalexine, from 104.1 to 115.3% for cefotaxime, from 97.1 to 105.6% for cefazolin, from 97.4 to 108.6% for cefuroxime, from 98.8 to 103.4% for cefoperazone and from 95.5 to 103.6% for ceftiofur. Correlation coefficients ranged from 0.9926 to 0.9999. CC(b) values were in the range from 103.5 to 112.3 μg/kg for analytes with a maximum residue limit of 100 μg/kg and from 54.4 to 56.3 μg/kg for those with a maximum residue limit of 50 μg/kg.

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Multiresidue LC–MS/MS analysis of cephalosporins and quinolones in milk following ultrasound‐assisted matrix solid‐phase dispersive extraction combined with the quick, easy, cheap, effective, rugged, and safe methodology

Karageorgou

Myridakis

Stephanou

et al. 2013

J of Separation Science

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A sensitive and selective confirmatory method for milk-residue analysis of ten quinolones and eight cephalosporins by LC-MS/MS has been developed herein. For the chromatographic separation of target analytes, a Perfectsil ODS-2 (250 × 4 mm, 5 μm) analytical column was used and gradient elution was applied, using a mobile phase of 0.1% w/w TFA in water and 0.1% w/w TFA in ACN. Ultrasound-assisted matrix solid-phase dispersion procedure was applied for the extraction and clean-up procedure of antimicrobials agents from milk matrix using a mixture of Bond Elut Plexa sorbent and QuEChERS. The method was validated meeting the European Legislation determining selectivity, linearity response, trueness, precision (repeatability and between-day reproducibility), decision limit, detection capability, and ruggedness following the Youden approach. Recoveries of all antibiotics ranged from 81.7 to 117.9%, while RSD values were lower than 13.7%. Limits of quantification for all examined compounds ranged from 2.4 to 15.0 μg/kg, substantially lower than the maximum residue limits established by the European Union (30-100 μg/kg).

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TLC-DB as an Alternative to the HPLC Method in the Determination of Cefacetril Residues in Cow's Milk

Cited by 18 publications

References 11 publications

Comparison of Deproteinization Methods Used Before TLC-DB and HPLC Analysis of Flumequine Residues in Milk

Comparison of Deproteinization Methods Used Before TLC-DB and HPLC Analysis of Flumequine Residues in Milk

Application of ultrasound‐assisted matrix solid‐phase dispersion extraction to the HPLC confirmatory determination of cephalosporin residues in milk

Multiresidue LC–MS/MS analysis of cephalosporins and quinolones in milk following ultrasound‐assisted matrix solid‐phase dispersive extraction combined with the quick, easy, cheap, effective, rugged, and safe methodology

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