Assessment of liquid chromatography–tandem mass spectrometry approaches for the analysis of ceftiofur metabolites in poultry muscle

Berendsen, B.J.A.; Stolker, Linda; Nielen, Michel W. F.

doi:10.1080/19440049.2011.635348

Cited by 14 publications

(11 citation statements)

References 29 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The threshold Table 1. Precursor ion Mass, Product Ion Mass and Retention Time of Sebuthylazine, NPAMOZ, Oxolinic Acid,17 ß-trenbolone, and Ceftiofur Including Calculation of P(I) Sebuthylazine [20] NPAMOZ [21] Oxolinic acid [36] 17ß-Trenbolone [53] Ceftiofur [54] Precursor ion 230 335 262 271 524 P(Mpr) 7.5*10 -4 4.0*10 -3 1.5*10 Figure 4. Cumulative distribution function of the fraction of the compounds (n0200) versus P(I) in the authors' laboratory using (dashed line) one product ion and (solid line) two product ions should be fixed in such a way that it can be concluded that the method is sufficiently selective (fit for purpose) (i.e., (1) the calculated probability of the occurrence of an incorrect identification is low enough to persuade a judge or jury in court, and (2) an expert scientist would feel comfortable in defending the probability of an incorrect identification).…”

Section: Setting a Threshold For P(i)mentioning

confidence: 99%

The (Un)Certainty of Selectivity in Liquid Chromatography Tandem Mass Spectrometry

Berendsen

Stolker

Nielen

2012

J. Am. Soc. Mass Spectrom.

View full text Add to dashboard Cite

We developed a procedure to determine the "identification power" of an LC-MS/MS method operated in the MRM acquisition mode, which is related to its selectivity. The probability of any compound showing the same precursor ion, product ions, and retention time as the compound of interest is used as a measure of selectivity. This is calculated based upon empirical models constructed from three very large compound databases. Based upon the final probability estimation, additional measures to assure unambiguous identification can be taken, like the selection of different or additional product ions. The reported procedure in combination with criteria for relative ion abundances results in a powerful technique to determine the (un)certainty of the selectivity of any LC-MS/MS analysis and thus the risk of false positive results. Furthermore, the procedure is very useful as a tool to validate method selectivity.

show abstract

Section: Setting a Threshold For P(i)mentioning

confidence: 99%

The (Un)Certainty of Selectivity in Liquid Chromatography Tandem Mass Spectrometry

Berendsen

Stolker

Nielen

2012

J. Am. Soc. Mass Spectrom.

View full text Add to dashboard Cite

show abstract

“…Finally, because of the complex profile of ceftiofur's metabolites due to their chemically labile nature in the biological environment, proper selection of surrogate compounds in place of total DFC should match the specific animal species, the target tissue, and the intended regulatory purpose. In the work presented by Berendsen et al, 12 DCCD was detectable (LOD 1 μg/kg −1 ) in broiler breast muscle until at least 8 h postdosing, but at <24 h by extrapolation, with significant underestimation of total DFC. The ammonolysis approach was deemed more suitable for screening off-label use of cephalosporin antibiotics in poultry.…”

Section: ■ Materials and Methodsmentioning

confidence: 93%

Determination of Ceftiofur Metabolite Desfuroylceftiofur Cysteine Disulfide in Bovine Tissues Using Liquid Chromatography–Tandem Mass Spectrometry as a Surrogate Marker Residue for Ceftiofur

Feng

Chiesa

Kijak

et al. 2014

J. Agric. Food Chem.

View full text Add to dashboard Cite

Ceftiofur is a widely used cephalosporin β-lactam antibiotic with frequently reported residue violations. This paper reports a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining a ceftiofur metabolite, desfuroylceftiofur cysteine disulfide (DCCD), in bovine kidney, liver, and muscle tissues. Incurred tissue samples were obtained from dosed animals and analyzed to evaluate the utility of the method. For kidney, the target tissue, the method utilized a simple extraction with phosphate buffer followed by solid phase extraction (SPE) cleanup. For liver and muscle, acetonitrile and hexane were used to remove most proteins and fat from the initial buffer extract before the SPE cleanup. Method accuracy was between 97 and 107%, and the coefficient of variation was between 3.4 and 11.0% for all three types of tissues. The relationship between the new and regulatory methods for bovine kidney was established. It was concluded that DCCD is a suitable surrogate marker residue for ceftiofur in bovine kidney.

show abstract

“…In literature, chromatographic separation of ceftiofur and cefquinome is mostly performed by using a C18 column [ 31 , 32 , 33 , 34 , 35 , 36 , 37 ]. A few methods use a PLRP-S column because of the robustness of this type of column in combination with an acidic mobile phase [ 38 , 39 ].…”

Section: Discussionmentioning

confidence: 99%

Development and Validation of Liquid Chromatography-Tandem Mass Spectrometry Methods for the Quantification of Cefquinome, Ceftiofur, and Desfuroylceftiofuracetamide in Porcine Feces with Emphasis on Analyte Stability

Rutjens¹,

Croubels²,

Baere³

et al. 2021

Molecules

View full text Add to dashboard Cite

Cefquinome and ceftiofur are β-lactam antibiotics used for the treatment of bacterial infections in swine. Although these antimicrobials are administered intramuscularly, the exposure of the gut microbiota to these cephalosporins is not well described. This exposure can contribute to the emergence and spread of antimicrobials in the environment and to the possible spread of antimicrobial resistance genes. To assess the impact of drug administration on the intestinal excretion of these antimicrobials it is essential to measure the amounts of native compound and metabolites in feces. Two (ultra)-high-performance liquid chromatography-tandem mass spectrometry ((U)HPLC–MS/MS) methods were developed and validated, one for the determination of cefquinome and ceftiofur and the other for the determination of ceftiofur residues, measured as desfuroylceftiofuracetamide, in porcine feces. The matrix-based calibration curve was linear from 5 ng g−1 to 1000 ng g−1 for cefquinome (correlation coefficient (r) = 0.9990 ± 0.0007; goodness of fit (gof) = 3.70 ± 1.43) and ceftiofur (r = 0.9979 ± 0.0009; gof = 5.51 ± 1.14) and quadratic from 30 ng g−1 to 2000 ng g−1 for desfuroylceftiofuracetamide (r = 0.9960 ± 0.0020; gof = 7.31 ± 1.76). The within-day and between-day precision and accuracy fell within the specified ranges. Since β-lactam antibiotics are known to be unstable in feces, additional experiments were conducted to adjust the sampling protocol in order to minimize the impact of the matrix constituents on the stability of the analytes. Immediately after sampling, 500 µL of an 8 µg mL−1 tazobactam solution in water was added to 0.5 g feces, to reduce the degradation in matrix.

show abstract

Assessment of liquid chromatography–tandem mass spectrometry approaches for the analysis of ceftiofur metabolites in poultry muscle

Cited by 14 publications

References 29 publications

The (Un)Certainty of Selectivity in Liquid Chromatography Tandem Mass Spectrometry

The (Un)Certainty of Selectivity in Liquid Chromatography Tandem Mass Spectrometry

Determination of Ceftiofur Metabolite Desfuroylceftiofur Cysteine Disulfide in Bovine Tissues Using Liquid Chromatography–Tandem Mass Spectrometry as a Surrogate Marker Residue for Ceftiofur

Development and Validation of Liquid Chromatography-Tandem Mass Spectrometry Methods for the Quantification of Cefquinome, Ceftiofur, and Desfuroylceftiofuracetamide in Porcine Feces with Emphasis on Analyte Stability

Contact Info

Product

Resources

About