KÜMES HAYVANLARI YUMURTALARINDAKİ PİPERİDİN-1-YUM {[5-(2-FURİL)-4- FENİL-4H-1,2,4-TRİAZOL-3-İL]TİYO}ASETAT ARTIKLARININ BELİRLENMESİ İÇİN BİR LC-ESI-MS YÖNTEMİNİN GELİŞTİRİLMESİ VE VALİDASYONU

ESI-MS yöntemi tasarlanmıştır. Numuneler ultrasonik banyoda dimetil sülfoksit ile ekstre edilmiş, 15.000 g'da santrifüjlenmiş, ultrafiltre ile süzülmüş ve HPLC sistemine enjekte edilmiştir. Suda %0,1 (h/h) formik asit (A) ve asetonitrilde %0,1 (h/h) formik asit (B) içeren mobil faz ile izokratik elüsyon yapılmıştır. Mobil fazın bileşimi, 0,4 mL. dak-1 akış hızında, A/B (%70: %30, h/h)dır. Toplam çalışma süresi 5 dakikadır. Kütle spektrometrik koşullar, SIM modu (m/z 302,1), pozitif polaritedir. Doğruluk %0,2887-7,204 dır. Kesinlik, %1,564-5,636 dır. Yöntem, kümes hayvanları yumurtalarındaki Trifuzol kalıntısı kantitatif tayininde kullanılabilir.

DEVELOPMENT AND VALIDATION OF A LC-ESI-MS METHOD FOR DETECTION OF PIPERIDIN-1-IUM {[5-(2-FURYL)-4-PHENYL-4H- 1,2,4-TRIAZOL-3-YL] THIO}ACETATE RESIDUES IN POULTRY EGGS

A simple, rapid and reproducible isocratic reversed-phase LC-ESI-MS method has been elaborated for determination of the piperidin-1-ium {[5-(2-furyl)-4-phenyl-4H-1,2,4-triazol-3-yl] thio}acetate, active pharmaceutical ingredient (API) of the antiviral veterinary drug “Tryfuzol” in the poultry eggs. The samples were extracted by dimethyl sulfoxide at ultrasonic bath, centrifuged at 15000 g, filtrated through ultrafilter and injected into HPLC system. A mobile phase was used 0.1% (v/v) formic acid in water (A) and acetonitrile containing 0.1% (v/v) formic acid (B) at isocratic elution. The composition of the mobile phase was A/B (70%:30%, v/v) at flow rate of 0.4 ml min-1. Total running time was 5 minutes. Mass spectrometric conditions were SIM mode (m/z 302.1), positive polarity. The mean concentration were 0.2887-7.204% of the nominal values for the QC samples. The within-run CV values were 1.564-5.636% for the QC samples. The method is applicable for determination of the residual quantities of API of the “Tryfuzol” in the poultry eggs.