Simultaneous determination of 38 veterinary antibiotic residues in raw milk by UPLC–MS/MS

Han, Rongwei; Zheng, Nan; Yu, Zhongna; Wang, J.; Xu, Xiaorong; Qu, Xueyin; Li, S.L.; Zhang, Y.D.; Wang, J.Q.

doi:10.1016/j.foodchem.2015.02.041

Cited by 112 publications

(44 citation statements)

References 25 publications

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“…(Bohm et al 2009;Chico et al 2008;Dasenaki and Thomaidis 2015;Freitas et al 2014;Frenich et al 2010;Geis-Asteggiante et al 2012;Granelli and Branzell 2007;Han et al 2015;Hermo et al 2008;Kaufmann et al 2014;Martins-Júnior et al 2007;Mastovska and Lightfield 2008;Ortelli et al 2009;Stolker et al 2008;Turnipseed et al 2014;Wang et al 2015) but there is a lack in the method development for processed dairy products, since antibiotics are not fully degraded during pasteurization process (Pérez et al 2013).…”

Section: Additionally This Technique Fulfills the Requirements Demmentioning

confidence: 99%

Development and Validation of a Multi-class UHPLC-MS/MS Method for Determination of Antibiotic Residues in Dairy Products

2017

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In regard to the knowledge of provoking a worldwide resistance against antibiotics due to incorrect application and the resulting uptake of residues via the food chain, the European Union set maximum residue levels (MRLs) for these substances in animal derived products to protect the customers. In respect of these MRLs a multi-class UHPLC-MS/MS multiclass method has been developed for the simultaneous determination of 30 substances from different compound groups (quinolones, macrolides, lincosamides, β-lactams, sulphonamides, diamino-pyrimidine derivates and tetracyclines) in various kinds of dairy products. Since this method should be suitable for routine laboratory use, sample preparation requires an easy and fast approach to ensure high sample throughput. Therefore a sample preparation with C18EC dSPE bulk sorbent as a combination of the easy and quick sample preparation provided by QuEChERS and the clean-up principle of reversed phase SPE was applied. This method was validated for all compounds in all matrices in compliance with the requirements of Commission Decision 2002/657/EC.

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Section: Additionally This Technique Fulfills the Requirements Demmentioning

confidence: 99%

Development and Validation of a Multi-class UHPLC-MS/MS Method for Determination of Antibiotic Residues in Dairy Products

2017

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“…Also, other important antibiotics such as ciprofloxacin, enrofloxacin and marbofloxacin (quinolones); erythromycin, spiramycin and neospiramycin (macrolides); and cephapirin, ceftiofur, cefazolin and cefoperazone (cephalosporins) demonstrated scarce accuracies. Four published methods, after milk extraction, applied reverse‐phase SPE as purification step (generally OASIS HLB) . Unfortunately, these papers did not always report real recoveries, applying pre‐extraction matrix‐matched curves to quantify the analytes and then furnishing data already recovery‐corrected.…”

Section: Introductionmentioning

confidence: 99%

Multiclass method for the determination of 62 antibiotics in milk

et al. 2016

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A multiclass method for screening and confirmatory analysis of antimicrobial residues in milk has been developed and validated. Sixty-two antibiotics belonging to ten different drug families (amphenicols, cephalosporins, lincosamides, macrolides, penicillin, pleuromutilins, quinolones, rifamycins, sulfonamides and tetracyclines) have been included. After the addition of an aqueous solution of EDTA, the milk samples were extracted twice with acetonitrile, evaporated and dissolved in ammonium acetate. After centrifugation, 10 µl were analysed using LC-Q-Orbitrap operating in positive electrospray ionization mode. The method was validated in bovine milk in the range 2-150 µg kg(-1) for all antibiotics; for four compounds with maximum residue limits higher than 100 µg kg(-1) , the validation interval has been extended until 333 µg kg(-1) . The estimated performance characteristics were satisfactory complying with the requirements of Commission Decision 2002/657/EC. Good accuracies were obtained also taking advantage from the versatility of the hybrid mass analyser. Identification criteria were achieved verifying the mass accuracy and ion ratio of two ions, including the pseudomolecular one, where possible. Finally, the developed procedure was applied to 13 real cases of suspect milk samples (microbiological assay) confirming the presence of one or more antibiotics, although frequently, the maximum residue limits were not exceeded. The availability of rapid multiclass confirmatory methods can avoid wastes of suspect, but compliant, raw milk samples. Copyright © 2016 John Wiley& Sons, Ltd.

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“…Based on a previous study [16], the linearity and analytical limits were validated. The linearity was evaluated by matrix-matched calibration curves at different spiked levels.…”

Section: Validationmentioning

confidence: 99%

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

Kee¹,

Ryu²,

Cha³

et al. 2016

Korean Journal of Veterinary Research

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Abstract:This study was conducted to analyze penicillin G (PEG), streptomycin (STR) and neomycin (NEO) residues in milk of healthy lactating cows. Milk samples were collected from all four quarters of 12 dairy cows 2−7 days after intramammary infusions of an ointment containing PEG, STR and NEO once (n = 4; group I) or twice (n = 4, group II) daily. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry was used to determine the antibiotic residues in the samples. The correlation coefficient (r 2 ) of the calibration curves for all antibiotics was > 0.999 and the limits of detection and quantification were 0.002-0.005 µg/mL and 0.007-0.02 µg/ mL, respectively. Recovery rates were ranged from 75.5 to 92.3%. In group I, PEG, STR and NEO residues were detected in milk at 2, 3 and 2 days post-treatment, respectively, which were below the maximum residue limit (MRL). In group II, PEG, STR and NEO residues were detected in milk at 2, 3 and 3 days post-treatment, respectively, which were bellow the MRL. These results suggest that a 3-day for milk withdrawal period after the ointment treatment might be sufficient for reduction of the antibiotic residues below the MRL.

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Simultaneous determination of 38 veterinary antibiotic residues in raw milk by UPLC–MS/MS

Cited by 112 publications

References 25 publications

Development and Validation of a Multi-class UHPLC-MS/MS Method for Determination of Antibiotic Residues in Dairy Products

Development and Validation of a Multi-class UHPLC-MS/MS Method for Determination of Antibiotic Residues in Dairy Products

Multiclass method for the determination of 62 antibiotics in milk

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

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