Determination of five tetracyclines and their epimers by LC-MS/MS based on a liquid-liquid extraction with low temperature partitioning.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess
; 35(4): 686-694, 2018 Apr.
Article
in En
| MEDLINE
| ID: mdl-29337659
ABSTRACT
An LC-MS/MS method is presented for screening five tetracyclines and their epimers in a broad range of food products. The scope of matrices includes meat-, fish-, seafood-based products, various dairy ingredients, infant formulae and fats. The method principle is based on a liquid-liquid extraction with aqueous ethylenediaminetetraacetic acid (EDTA) and acetonitrile followed by a freezing step to promote phase separation at low temperature. After defatting with hexane, sample extracts were evaporated and reconstituted before injection onto the LC-MS/MS system. The addition of oxalic acid in the aqueous mobile phase was mandatory to maintain good peak shape and sensitivity over the run. The screening is based upon a double preparation of each sample, one 'as such' and a second one with the analytes spiked in the sample, in order to mitigate the risk of false negative response. The method was validated according to the European Community Reference Laboratories Residues Guidelines. A total of 93 samples were included in the validation by two independent laboratories giving both false-negative and false-positive rates at 0% for all compounds. Over the last two years, 2600 samples were analysed routinely and only one chicken sample was found above the regulatory limit.
Key words
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Temperature
/
Tetracyclines
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Food Contamination
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Tandem Mass Spectrometry
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Liquid-Liquid Extraction
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Food Analysis
Language:
En
Journal:
Food Addit Contam Part A Chem Anal Control Expo Risk Assess
Journal subject:
CIENCIAS DA NUTRICAO
Year:
2018
Document type:
Article
Affiliation country:
Switzerland
Publication country:
ENGLAND
/
ESCOCIA
/
GB
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GREAT BRITAIN
/
INGLATERRA
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REINO UNIDO
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SCOTLAND
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UK
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UNITED KINGDOM