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Determination of chloramphenicol in bovine urine, meat and shrimp by GC-MS. Method validation according to Commission Decision 2002/657/EC
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Open Access
Type
Report
Language
en
Date
2004-04-20
Research Projects
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Journal Issue
Title
Determination of chloramphenicol in bovine urine,
meat and shrimp by GC-MS. Method validation according to Commission Decision
2002/657/EC
Translated Title
Bepaling van chloramphenicol in runder-urine,
vlees en garnalen m.b.v. GC-MS. Methode validatie volgens Commissie
Beschikking 2002/657/EC
Published in
Abstract
Dit rapport beschrijft de validatie, de kwantificering
en de wijze van identificatie van een analysemethode voor de bepaling van
lage concentraties (0,1-1,0 micro g/kg) chlooramphenicol in monsters urine,
garnalen en spierweefsel (vlees) Deze validatie is gebaseerd op de criteria
beschreven in de Beschikking van de Commissie 2002657EC. Na een eerste
extractie, voorafgegaan door enzymatische hydrolyse (urine) of enzymatische
digestie (spierweefsel), wordt chlooramphenicol geextraheerd vanuit de
matrix met ethylacetaat. Het verkregen extract wordt vervolgens verder
gezuiverd met vaste fase extractie (Solid Phase Extraction, SPE) en
LC-fractionering. Bij het opwerken van monsters garnaal kan de
zuiveringsstap over SPE worden overgeslagen. Na derivatisering wordt het
verkregen extract geanalyseerd met GC-MS. Detectie kan plaatsvinden met
negatieve chemische ionisatie (NCI), de meest gevoelige methode. Indien NCI
niet beschikbaar is kunnen electron impact (EI) of positieve chemische
ionisatie (PCI) als alternatief gebruikt worden. De beschreven methode is
zowel geschikt voor screening als bevestiging. De beslissingsgrens voor
alle monsters bedraagt ongeveer 0,05 micro g/l of 0,05 micro g/kg. Het
detectievermogen voor urinemonsters is 0,3 micro g/l, voor garnalen is deze
0,1 micro g/kg. Wanneer PCI of EI gebruikt worden is het detectievermogen
0,5 microg/l of 0,5 micro g/kg.
This report describes the validation of the quantification and the identification of an analytical method for the determination of low concentrations (0.1-1.0 micro g/kg) of chloramphenicol in samples of urine, shrimps and meat. The validation study was based on the criteria described in Decision 2002/657/EC of the European Commission. The analytical method consists of an enzymatic hydrolysis (urine) or enzymatic digestion (meat), followed by liquid-liquid extraction of chloramphenicol from the matrix with ethyl acetate. The extract is cleaned with Solid Phase Extraction (SPE), followed by LC fractionation. The SPE step can be omitted for shrimps. After derivatisation of the chloramphenicol, final separation and detection is performed with GC-MS with Negative Chemical Ionisation (NCI). Detection can also be carried out using Electron Impact (EI), which is a less sensitive technique. This method can be used for both screening and quantification. The limit of determination for all samples is approximately 0.05 micro g/l or micro g/kg. The detection capability for samples of urine is 0.3 micro g/l. For shrimp samples, the detection capability is 0.1 micro g/kg. If EI is used, the detection capability is 0.5micro g/l or micro g/kg.
This report describes the validation of the quantification and the identification of an analytical method for the determination of low concentrations (0.1-1.0 micro g/kg) of chloramphenicol in samples of urine, shrimps and meat. The validation study was based on the criteria described in Decision 2002/657/EC of the European Commission. The analytical method consists of an enzymatic hydrolysis (urine) or enzymatic digestion (meat), followed by liquid-liquid extraction of chloramphenicol from the matrix with ethyl acetate. The extract is cleaned with Solid Phase Extraction (SPE), followed by LC fractionation. The SPE step can be omitted for shrimps. After derivatisation of the chloramphenicol, final separation and detection is performed with GC-MS with Negative Chemical Ionisation (NCI). Detection can also be carried out using Electron Impact (EI), which is a less sensitive technique. This method can be used for both screening and quantification. The limit of determination for all samples is approximately 0.05 micro g/l or micro g/kg. The detection capability for samples of urine is 0.3 micro g/l. For shrimp samples, the detection capability is 0.1 micro g/kg. If EI is used, the detection capability is 0.5micro g/l or micro g/kg.
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