Naslov
Validation of a liquid chromatography–tandem mass spectrometry (LC-MS/MS) for the determination of sulphonamides in muscle tissue

Autori
Varenina, Ivana ; Bilandžić, Nina ; Solomun, Božica ; Nekić, Tamara

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, znanstveni

Izvornik
Abstracts of the 7th International Congres of Food Technologists, Biotechnologists and Nutritionists / Božanić, Rajka, Bursać Kovačević, Danijela, i ostali - Zagreb, 2011, 250-250

ISBN
978-953-99725-3-8

Skup
International Congres of Food Technologists, Biotechnologists and Nutritionists (7 ; 2011)

Mjesto i datum
Opatija, Hrvatska, 20.09.2011. - 23.09.2011

Vrsta sudjelovanja
Poster

Vrsta recenzije
Međunarodna recenzija

Ključne riječi
sulphonamides; validation; LC-MS/MS

Sažetak
Sulphonamides, as derivatives of sulphanilic acid, are an important group of synthetic antibiotics commonly used in veterinary medicine for the prevention and treatment of various microbial infections, and as an addition to animal feed as a growth promoter. Frequent use of antibiotics increases the threat of development of resistance and the appearance of residues in food. If they enter the food chain, they can cause allergic and toxic reactions, while some also possess carcinogenic properties. Control of veterinary medicine residues is regulated by a national ordinance, with a prescribed total maximum permitted sulphonamides quantity of 100 μg kg-1 for muscle and milk samples. This paper describes the validation method liquid chromatography–tandem mass spectrometry (LC-MS/MS) for the simultaneous detection of 5 sulphonamides according to the validation method criteria pursuant to Commission Decision 2002/657/EC. For that purpose, the following parameters were set: specificity, linearity, limit of decision (CCα), detection of capability (CCβ), limit of detection, precision, within-laboratory reproducibility and accuracy. The group of sulphonamides covered by the method included sulphadiazine, sulphamerazine, sulphametazine, sulphachloropyridazine and sulphisoxazole. Analyses were conducted using a sulphonamide standard and internal sulphametazine-phenyl-13C6 standard according to the procedure of four identification points (two precursors and two ion products). The calibration curves for all analytes were linear in the area from 25 to 750 μg kg-1 with a correlation coefficient greater than 0.997. Accuracy was expressed as recovery and ranged from 98.9 to 107.8%. Within-laboratory reproducibility did not exceed 20%. The calibration curve method was used to determine the limit of decision CCα, which ranged from 117.9 to 137.6 μg kg-1, and detection of capability CCβ, which ranged from 134.6 to 173.7 μg kg-1. Precision was expressed using the coefficient of variation and ranged from 1.6 to 20.3%. The detection limits for each analyte were less than 35 μg kg-1. The validation method proved to meet the set criteria for the confirmation and quantification of sulphonamides in the muscle matrix.

Izvorni jezik
Engleski

Znanstvena područja
Javno zdravstvo i zdravstvena zaštita

POVEZANOST RADA