Screening and confirmatory method for multiclass determination of 62 antibiotics in meat

Moretti, Simone; Dusi, Guglielmo; Giusepponi, Danilo; Pellicciotti, Simona; Rossi, Rosanna; Saluti, Giorgio; Cruciani, Gabriele; Galarini, Roberta

doi:10.1016/j.chroma.2015.12.021

Cited by 46 publications

(43 citation statements)

References 25 publications

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“…The mean recoveries were in the interval from 70 to 120%, except for sulfaguanidine, sulfapyridine and sulfamethazine with recoveries from 60 to 70% Although all intra‐lab reproducibilities were lower than or equal to 22%, these three sulfonamides, together with cloxacillin and tylvalosin, demonstrated also the poorest intra‐lab reproducibility (CV wR,pooled >15%). Good recoveries were observed also for beta‐lactams and tetracyclines that demonstrated the most critical performances in muscle tissue . It must be underlined that these performance characteristics were obtained applying the screening run parameters (Table ).…”

Section: Resultsmentioning

confidence: 83%

“…The chromatographic conditions were the same described in our previous paper developed for a multiclass method for antibiotics in muscle . In contrast, important changes have been carried out in MS conditions for milk considering the stringent MRLs especially for some penicillins (4 µg kg −1 ) and specific matrix interfering substances as detailed in the following discussion.…”

Section: Resultsmentioning

confidence: 99%

“…the pooled CV Rw (CV Rw,pooled ). For substances with MRL, the decision limit (CCα) and detection capability (CCβ) were then calculated as reported elsewhere . The obtained values are listed in Table .…”

Section: Resultsmentioning

confidence: 99%

“…The chromatographic conditions were the same described in our previous paper developed for a multiclass method for antibiotics in muscle. [18] In contrast, important changes have been carried out in MS conditions for milk considering the stringent MRLs especially for some penicillins (4 μg kg À1 ) and specific matrix interfering substances as detailed in the following discussion. A two-step strategy was here followed: (1) screening run devoted to minimize false compliant results in unknown samples (Table 1) and (2) confirmatory run devoted to minimize false non-compliant results in suspect samples and definitively confirm the identity and concentration of analyte(s) ( Table 2).…”

Section: Optimization Of Mass Spectrometric Conditionsmentioning

confidence: 99%

“…Good recoveries were observed also for beta-lactams and tetracyclines that demonstrated the most critical performances in muscle tissue. [18]…”

Section: Linearitymentioning

confidence: 99%

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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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Section: Resultsmentioning

confidence: 83%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Optimization Of Mass Spectrometric Conditionsmentioning

confidence: 99%

“…Good recoveries were observed also for beta-lactams and tetracyclines that demonstrated the most critical performances in muscle tissue. [18]…”

Section: Linearitymentioning

confidence: 99%

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Multiclass method for the determination of 62 antibiotics in milk

et al. 2016

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Practical approach to develop a multi‐group screening method for detection of mycotoxins, pesticides and veterinary drugs in food

et al. 2020

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A multi-group screening method to detect residues of veterinary drugs in meat and environmental contaminants in wheat flour has been developed using liquid chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (LC-HRMS). The procedure was tested for over 300 representative compounds (173 veterinary drugs, 122 pesticides and 9 mycotoxins) analysing in parallel negative and positive (spiked) samples according to European validation rules. The Screening Target Concentrations (STCs) were chosen conservatively with respect to the method purposes. Interpretation of results was based on retention time, mass accuracy of precursor and MS 2 spectral library. Evaluating the percentage of false negative results, 280 out of the 304 analytes were detectable at the STCs (false compliant rate ≤ 5%). In wheat flours, incurred levels of mycotoxins, deoxynivalenol and 3-acetyldeoxynivalenol, higher than STCs, were frequently found, whereas in meat, the most detected veterinary drugs were antibiotics generally at negligible concentrations (<10 μg kg −1). Finally, seven test materials from proficiency test schemes were successfully tested.

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Freeze–thaw approach: A practical sample preparation strategy for residue analysis of multi‐class veterinary drugs in chicken muscle

Zhang

et al. 2018

J of Separation Science

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Seven drugs from different classes, namely, fluoroquinolones (enrofloxacin, ciprofloxacin, sarafloxacin), sulfonamides (sulfadimidine, sulfamonomethoxine), and macrolides (tilmicosin, tylosin), were used as test compounds in chickens by oral administration, a simple extraction step after cryogenic freezing might allow the effective extraction of multi-class veterinary drug residues from minced chicken muscles by mix vortexing. On basis of the optimized freeze-thaw approach, a convenient, selective, and reproducible liquid chromatography with tandem mass spectrometry method was developed. At three spiking levels in blank chicken and medicated chicken muscles, average recoveries of the analytes were in the range of 71-106 and 63-119%, respectively. All the relative standard deviations were <20%. The limits of quantification of analytes were 0.2-5.0 ng/g. Regardless of the chicken levels, there were no significant differences (P > 0.05) in the average contents of almost any of the analytes in medicated chickens between this method and specific methods in the literature for the determination of specific analytes. Finally, the developed method was successfully extended to the monitoring of residues of 55 common veterinary drugs in food animal muscles.

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Screening and confirmatory method for multiclass determination of 62 antibiotics in meat

Cited by 46 publications

References 25 publications

Multiclass method for the determination of 62 antibiotics in milk

Multiclass method for the determination of 62 antibiotics in milk

Practical approach to develop a multi‐group screening method for detection of mycotoxins, pesticides and veterinary drugs in food

Freeze–thaw approach: A practical sample preparation strategy for residue analysis of multi‐class veterinary drugs in chicken muscle

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