Mine ANTEP, Melis KAYNAKER, Melek MERDİVAN

GIDALARDAKİ TETRASİKLİN KALINTILARININ İYONİK SIVI DESTEKLİ DİSPERSİF SIVI SIVI MİKROEKSTRAKSİYONU SONRASI HPLC İLE TAYİNİ

Bu çalışmada, süt, yumurta ve bal numunelerinde yüksek performanslı sıvı kromatografisi tayininden önce altı tetrasiklin kalıntısının (minosiklin, oksitetrasiklin, tetrasiklin, klortetrasiklin, metasiklin, doksisiklin) zenginleştirilmesi için iyonik sıvı bazlı dispersif sıvı-sıvı mikro ekstraksiyon yöntemi geliştirilmiştir. Çalışmada ekstraktant olarak 1-hegzil-3- metilimidazolyum bis[(triflorometan)sülfonil]imid iyonik sıvısı kullanılmıştır. Ekstraksiyon verimliliğini arttırmak için, pH, iyonik sıvı hacmi, dispersif çözücü türü ve hacmi, ekstraksiyon ve santrifüj süresi optimize edilmiştir. İncelenen tetrasiklin antibiyotiklerinin zenginleştirme faktörleri, optimize koşullar altında 15 ile 105 aralığında hesaplanmıştır. Çalışılan gerçek numunelerde herhangi bir tetrasiklin kalıntısına rastlanmamıştır. Yöntemin doğruluğu için, süt, bal ve yumurta örneklerine 100 ve 250 μg L-1 derişimde standart tetrasiklin karışımı eklenmiş ve geri kazanım değerleri 50 ile 95 arasında elde edilmiştir.

Anahtar Kelimeler:

Tetrasiklinler, iyonik sıvı, imidazolyum, süt, bal, yumurta, sıvı-sıvı mikroekstraksiyondispersif

DETERMINATION OF TETRACYCLINE RESIDUES AFTER IONIC LIQUID ASSISTED DISPERSIVE LIQUID LIQUID MICROEXTRACTION IN DAIRY FOODS

In this study, ionic liquid based dispersive liquidliquid preconcentration of the six tetracycline residues (minocycline, oxytetracycline, tetracycline, chlortetracycline, methacycline , doxycycline) before high performance liquid chromatographic determination in milk, egg and honey samples. For extraction, 1-hexyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl] imide ionic liquid was used as an extractant. To enhance the extraction efficiency, pH, volume of ionic liquid, type and volume of dispersive solvent, extraction time and centrifugation time were optimized. The enrichment factors of the studied tetracycline antibiotics were calculated in the range of 15 to 105 at optimized conditions. No residue of tetracyclines were found in the studied real samples. For the accuracy of this method, the 100 and 250 µg L-1 of standard tetracycline mixture solutions were spiked to the milk, honey and egg samples and the percentage recoveries were obtained between 50 and 95

Keywords:

Tetracyclines, ionic liquid, imidazolium, milk, honey, egg, dispersive liquid-liquid microextraction,

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