Determination of dimetridazole, ronidazole and their common metabolite in poultry muscle and eggs by high performance liquid chromatography with UV detection and confirmatory analysis by atmospheric pressure chemical ionisation mass spectrometry

Citation
Mj. Sams et al., Determination of dimetridazole, ronidazole and their common metabolite in poultry muscle and eggs by high performance liquid chromatography with UV detection and confirmatory analysis by atmospheric pressure chemical ionisation mass spectrometry, ANALYST, 123(12), 1998, pp. 2545-2549
Citations number
6
Language
INGLESE
art.tipo
Article
Categorie Soggetti
Chemistry & Analysis","Spectroscopy /Instrumentation/Analytical Sciences
Journal title
ANALYST
ISSN journal
0003-2654 → ACNP
Volume
123
Issue
12
Year of publication
1998
Pages
2545 - 2549
Database
ISI
SICI code
0003-2654(199812)123:12<2545:DODRAT>2.0.ZU;2-M
Abstract
A method was developed for the determination of the nitroimidazole compound s dimetridazole (DMZ) and ronidazole (RNZ) and their common metabolite, 2-h ydroxymethyl-1-methyl-5-nitroimidazole (2-OH-M). Extracts obtained from a c lean-up process using strong cation exchange (SCX) solid phase extraction ( SPE) can be analysed either by high performance liquid chromatography with UV detection (HPLC-W) or by high performance liquid chromatography with atm ospheric pressure chemical ionisation mass spectrometry (HPLC-APCI-MS) as a confirmatory method. Up to 20 samples can be extracted in approximately 4 h. The HPLC-UV analysis had a limit of detection of 0.5 mu g kg(-1). Valida tion in chicken muscle fortified at a concentration of 5 mu g kg(-1) Save r ecoveries of 75% DMZ, 77% RNZ and 81% 2-OH-M with RSDs of 16.4, 11.3 and 14 .0%, respectively (n = 17). Validation in egg fortified at the same concent ration gave recoveries of 77% DMZ, 80% RNZ and 80% 2-OH-M, with RSDs of 14. 9, 22.0 and 18.2%, respectively(n = 18). The limit of detection of the HPLC -APCI-MS method was 0.1 mu g kg(-1) for DMZ and RNZ and 0.5 mu g kg(-1) for 2-OH-M. This method gave mean recoveries in fortified egg samples of 65% D MZ, 87% RNZ and 75% 2-OH-M with RSDs of 22, 11 and 14%, respectively (n = 1 0). The ratios of the peak areas of the molecular ion and a fragment ion we re monitored as added confirmation of the presence of the analyte. Both the HPLC-UV screening procedure and the HPLC-APCI-MS confirmatory method have subsequently been used for the analysis of several hundred samples as part of UK surveillance programmes.