PMID- 27053017
OWN - NLM
STAT- MEDLINE
DCOM- 20170223
LR  - 20191210
IS  - 1944-0057 (Electronic)
IS  - 1944-0057 (Linking)
VI  - 33
IP  - 6
DP  - 2016 Jun
TI  - Evidence of non-extractable florfenicol residues: development and validation of a 
      confirmatory method for total florfenicol content in kidney by UPLC-MS/MS.
PG  - 983-94
LID - 10.1080/19440049.2016.1175187 [doi]
AB  - The parent compound florfenicol (FF) is a broad-spectrum antibacterial compound 
      licensed in the UK for use in cattle, pigs and the aquaculture industry. The 
      analysis of porcine tissues in this study demonstrates that significant amounts 
      of solvent non-extractable FF-related residues are present in incurred tissues 
      (kidney and muscle) from treated animals. The results indicate that methods based 
      on solvent extraction alone may carry a significant risk of reporting 
      false-negative results. The use of a strong acid hydrolysis step prior to solvent 
      extraction of tissue samples is necessary for an accurate estimate of the total 
      tissue FF content. A robust and sensitive method for the determination of total 
      FF residue content in kidney samples by ultra-performance liquid 
      chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed and 
      validated. This method covers the synthetic amphenicol drug FF and its 
      metabolites, measured as the marker residue florfenicol amine (FFA) as per 
      Commission Regulation (EU) No. 37/2010. Non-extractable and intermediate 
      metabolites are converted to the hydrolysis product FFA, and then partitioned 
      into ethyl acetate. Extracts are solvent exchanged prior to a dispersive 
      solid-phase extraction step, then analysed using an alkaline reverse-phase 
      gradient separation by UPLC-MS/MS. The method was validated around the maximum 
      residue levels (MRLs) set out in Regulation (EU) No. 37/2010 for bovine kidney in 
      accordance with Commission Decision No. 2002/657/EC. The following method 
      performance characteristics were assessed during a single laboratory validation 
      study: selectivity, specificity, sensitivity, linearity, matrix effects, accuracy 
      and precision (decision limit (CCalpha) and detection capability (CCbeta) were 
      determined).
FAU - Faulkner, Dermot
AU  - Faulkner D
AD  - a Agri-Food and Biosciences Institute , Veterinary Sciences Division , Belfast , 
      UK.
FAU - Cantley, Margaret
AU  - Cantley M
AD  - a Agri-Food and Biosciences Institute , Veterinary Sciences Division , Belfast , 
      UK.
FAU - Walker, Matthew
AU  - Walker M
AD  - a Agri-Food and Biosciences Institute , Veterinary Sciences Division , Belfast , 
      UK.
FAU - Crooks, Steven
AU  - Crooks S
AD  - a Agri-Food and Biosciences Institute , Veterinary Sciences Division , Belfast , 
      UK.
FAU - Kennedy, David
AU  - Kennedy D
AD  - a Agri-Food and Biosciences Institute , Veterinary Sciences Division , Belfast , 
      UK.
FAU - Elliott, Christopher
AU  - Elliott C
AD  - b Institute for Global Food Security, Queen's University Belfast , Belfast , UK.
LA  - eng
PT  - Journal Article
PT  - Validation Study
DEP - 20160520
PL  - England
TA  - Food Addit Contam Part A Chem Anal Control Expo Risk Assess
JT  - Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & 
      risk assessment
JID - 101485040
RN  - 0 (Anti-Bacterial Agents)
RN  - 0 (Veterinary Drugs)
RN  - 9J97307Y1H (florfenicol)
RN  - FLQ7571NPM (Thiamphenicol)
SB  - IM
MH  - Animal Feed
MH  - Animals
MH  - Anti-Bacterial Agents/*analysis
MH  - Cattle
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Drug Residues/analysis
MH  - European Union
MH  - False Negative Reactions
MH  - Food Contamination/analysis
MH  - Kidney/*chemistry
MH  - Muscles/chemistry
MH  - Sensitivity and Specificity
MH  - Swine
MH  - Tandem Mass Spectrometry/*methods
MH  - Thiamphenicol/*analogs & derivatives/analysis
MH  - Veterinary Drugs
OTO - NOTNLM
OT  - *Florfenicol amine
OT  - *UPLC-MS/MS
OT  - *hydrolysis
OT  - *incurred tissue
OT  - *kidney
OT  - *liquid chromatography
OT  - *mass spectrometry
OT  - *muscle
OT  - *non-extractable
EDAT- 2016/04/08 06:00
MHDA- 2017/02/24 06:00
CRDT- 2016/04/08 06:00
PHST- 2016/04/08 06:00 [entrez]
PHST- 2016/04/08 06:00 [pubmed]
PHST- 2017/02/24 06:00 [medline]
AID - 10.1080/19440049.2016.1175187 [doi]
PST - ppublish
SO  - Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2016 
      Jun;33(6):983-94. doi: 10.1080/19440049.2016.1175187. Epub 2016 May 20.