Multiresidue determination of β-lactam antibiotics in milk and tissues with the aid of high-performance liquid chromatographic fractionation for clean up

Moats, W. A.; Romanowski, Robert D.

doi:10.1016/s0021-9673(98)00387-2

Cited by 50 publications

(31 citation statements)

References 39 publications

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“…Several methods have been established for the analysis of b-lactams in foods of animal origin, using mainly UV detection [15,16] or MS [15,[17][18][19][20][21][22][23]. These residues or a combination with other pharmaceutical compounds have also been detected in water samples by LC with UV detection [24,25] and with MS detection in tap and surface water [26] and in surface water and urban wastewater [5].…”

Section: Introductionmentioning

confidence: 99%

Multiresidue determination of penicillins in environmental waters and chicken muscle samples by means of capillary electrophoresis‐tandem mass spectrometry

et al. 2009

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A new analytical method based on CZE coupled with tandem MS detection (CE-MS/MS) has been developed for the simultaneous determination of nine penicillins of human and veterinary use (nafcillin, dicloxacillin, cloxacillin, oxacillin, ampicillin, penicillin G, amoxicillin, penicillin V and piperacillin), whose levels are regulated by the EU Council regulation No. 2377/90 in animal edible tissues. CE separation conditions, sheath liquid composition and electrospray parameters have been carefully optimized to reach high sensitivity and precision. Separation was carried out in a 96 cm total length fused-silica capillary (50 microm id, 360 microm od) using 60 mM ammonium acetate at pH 6.0 as running buffer. Lomefloxacin was used as internal standard. MS/MS experiments were carried out using an IT as analyzer operating in multiple reaction monitoring mode to achieve the minimum number of identification points established by the 2002/657/EC European Decision. The use of an SPE procedure in two steps, combining Oasis hydrophilic-liphophilic balance and Alumina N cartridges provide a satisfactory preconcentration and clean up treatment for meat samples after extraction of the compounds with ACN. Only Oasis hydrophilic-liphophilic balance cartridges were necessary in water samples to obtain adequate recoveries. The method has been characterized for its use in meat and water samples, using matrix-matched calibrations. For chicken muscle samples, LODs between 8 and 12 microg/kg have been obtained, in all cases lower than the maximum residue limits permitted. For water samples LODs from 0.18 to 0.26 microg/L could ensure its satisfactory application in aquatic samples.

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Section: Introductionmentioning

confidence: 99%

Multiresidue determination of penicillins in environmental waters and chicken muscle samples by means of capillary electrophoresis‐tandem mass spectrometry

et al. 2009

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“…HPLC has been mainly used to analyze antibiotics in different matrices, usually coupled with MS, as is shown in some review articles [5][6][7][8]. Specifically, some methods have been established for the analysis of b-lactams in milk, using mainly UV detection [9,10] or MS [9,[11][12][13][14][15][16][17]. CE is becoming a useful alternative technique in this field due to simplicity, short separation times, and lower consumption of reagents and solvents.…”

Section: Introductionmentioning

confidence: 99%

Large‐volume sample stacking for the analysis of seven β‐lactam antibiotics in milk samples of different origins by CZE

Bailón-Pérez¹,

Garcı́a-Campaña²,

Cruces‐Blanco³

et al. 2007

Electrophoresis

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A method for the simultaneous determination of eight beta-lactam antibiotics (nafcillin, cloxacillin, oxacillin, dicloxacillin, ampicillin, amoxicillin, and penicillin G) in fortified milk samples of different origins has been proposed by using CZE with diode-array detection (CZE-DAD). Optimum separation was obtained on a 64.5 cm x 75 microm bubble cell capillary using 175 mM Tris buffer with 20% ethanol at pH 8.0. Methylparaben has been used as an internal standard (IS). Taking into account the lack of sensitivity of the UV-Vis detection, a solvent extraction/SPE method was applied for off-line preconcentration and sample cleanup, and also an on-line preconcentration methodology, such as large-volume sample stacking (LVSS) with polarity switching, was developed, providing LODs ranging from 2 to 10 microg/L. The method permits the quantification of these residues below the levels established in milk by the EU Regulation. Satisfactory recoveries ranging from 86 to 93% were also obtained in milk samples of different origins.

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“…A significant number of methods use precolumn derivatization techniques for fluorescence detection performed by reaction with TCA (20% w/v) aqueous solution and HCHO (7% w/v) [16,19,20] or for UV detection at 320 -345 nm by benzoic anhydride to acrylate aminopenicillins and 1,2,4-triazole/imidazole and mercury(II) chloride at alkaline media (pH l 9) at 60 -658C in order to form mercury mercaptide derivatives and thus achieve higher sensitivity [21 -24]. Mass spectroscopy and MS/MS are used for confirmation analysis [25 -28].…”

Section: Introductionmentioning

confidence: 99%

“…Deproteinization of the samples can be achieved by 5% Na 2 WO 4 and 0.33 N H 2 SO 4 [12,21,22], by 2% NaCl, 5% Na 2 WO 4 , and 0.17 M H 2 SO 4 [18], by Et 4 NCl [15,27], by ACN [16], by phosphate buffer (pH 8.5) and H 2 SO 4 [24] or 30% TCA [20]. Extraction of penicillins can be achieved by CH 2 Cl 2 , CH 3 CN, and hexane [29], H 2 O, CH 3 CN, and NaCl solution [26], 2% NaCl [17,26], HCOOH [30], ACN/H 2 O (30:70 v/v) [17,18,25,26], or by tert-butyl alcohol and water [15,16].…”

Section: Introductionmentioning

confidence: 99%

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Development and validation of an HPLC method for the determination of penicillin antibiotics residues in bovine muscle according to the European Union Decision 2002/657/EC

Samanidou¹,

Nisyriou

Papadoyannis

2007

J of Separation Science

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A high-performance liquid chromatographic method was developed for the determination of five penicillins: penicillin G (PENG), penicillin V (PENV), oxacillin (OX), cloxacillin (CLO), and dicloxacillin (DICLO), in bovine muscle. Samples were macerated with a mixture of H(2)O/CH(3)CN (1:1) and purified using RP-8 Adsorbex SPE cartridges after centrifugation, with mean recovery from spiked samples higher than 89%. The separation of the examined penicillins was achieved on an analytical column, an Inertsil C8 5 microm, 250x4 mm(2), at ambient temperature. The mobile phase consisted of 0.1% TFA/ACN 50:50 v/v delivered isocratically at a flow rate of 1.1 mL/min. Analytes were monitored at 240 nm. The procedure was validated according to the European Union Decision 2002/657/EC by means of selectivity, stability, decision limit, detection capability, accuracy, and precision. Method's LOQ values achieved were 54 microg/kg for PENG and DICLO, 46 microg/kg for PENV, 16 microg/kg for OX, and 43 microg/kg for DICLO. The detection capabilities (CC(beta)) were 73.6 microg/kg for PENG, 29.1 microg/kg for PENV, 350.6 microg/kg for OX, 379.9 microg/kg for CLO, and 355.8 microg/kg for DICLO. The method was applied to various samples from the local market. Two penicillins were identified by photodiode array (PDA) detection and quantified.

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Multiresidue determination of β-lactam antibiotics in milk and tissues with the aid of high-performance liquid chromatographic fractionation for clean up

Cited by 50 publications

References 39 publications

Multiresidue determination of penicillins in environmental waters and chicken muscle samples by means of capillary electrophoresis‐tandem mass spectrometry

Multiresidue determination of penicillins in environmental waters and chicken muscle samples by means of capillary electrophoresis‐tandem mass spectrometry

Large‐volume sample stacking for the analysis of seven β‐lactam antibiotics in milk samples of different origins by CZE

Development and validation of an HPLC method for the determination of penicillin antibiotics residues in bovine muscle according to the European Union Decision 2002/657/EC

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