Arzu YAVUZ, İsmail AZAR, Ali ÖZCAN, Niyazi ÜLKÜ

SÜT TOZU VE PEYNİRALTI SUYU TOZUNDA ANTİBİYOTİK KALINTILARININ UPLC-MS/MS İLE ANALİZİNDE ÇOKLU GRUP YÖNTEMİ

Gıda endüstrisinde birçok ürünün hammaddesi olarak yaygın bir şekilde kullanılan süt tozu ve peyniraltı suyu tozunda beş gruptan (makrolidler, sülfanamidler, kinolonlar, linkozamidler, diaminopirimidinler) 27 antibiyotik kalıntısının belirlenmesi için bir ultra-performans sıvı kromatografisi-tandem kütle spektrometrisi (UPLC-MS/MS) çok sınıflı bir yöntem geliştirilmiş ve valide edilmiştir. Valide edilmiş bu yöntemin ana avantajı, metanol ile numunelerin ekstraksiyonuna dayanan basit, ucuz ve hızlı numune hazırlamadır. Yöntemin validasyonu, Avrupa ve Türkiye'deki resmi denetim numunelerinin analizinde kullanılan yöntemler için gerekli prosedür olan 2002/657/EC sayılı Avrupa Komisyonu Kararında belirtilen gereklilikler izlenerek gerçekleştirilmiştir. Matriks uyumlu kalibrasyon kullanılarak, numune hazırlama ve enstrümantal analiz ile ilgili matriks etkisi ve belirsizlikler minimize edilmiştir. Yöntem, kalıntıları çok düşük konsantrasyonlarda tespit etme yeteneğine sahiptir.

Anahtar Kelimeler:

antibiyotikler, kalıntılar, veteriner ilaçları, UPLC-MS/MS, validasyon, süt tozu, peynir altı suyu tozu, 2002/657/EC

A MULTICLASS METHOD FOR THE ANALYSIS OF ANTIBIOTIC RESIDUES IN MILK POWDER AND WHEY POWDER BY UPLC-MS/MS

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) multi-class method was developed and validated for the determination of 27 antibiotic residues from five classes (macrolides, sulfonamids, quinolones, lincosamids, diaminopyrimidines) in milk powder and whey powder which are commonly used as raw material of many products in the food industry. A simple, inexpensive and fast sample preparation based on the extraction of samples with methanol is the main advantage of the validated method. The validation of the method was performed following the requirements outlined in the European Commission Decision 2002/657/EC, which is required procedure for the methods used in analysis of official audits samples in Europe and Turkey. Matrix effect and uncertainties related with sample preparation and instrumental analysis were minimised by using matrix-matched calibration. The method is capable of detecting residues at very low concentrations.

Keywords:

antibiotics, residues, veterinary drugs, UPLC-MS/MS, validation, milk powder, whey powder, 2002/657/EC,

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