COMPARISON OF METHODS FOR THE ANALYSIS OF GLUCOCORTICOIDS IN MILK

Öz

Betamethasone, Dexamethasone, Prednisolone and Methylprednisolone are synthetic glucocorticoids that are widely used in various acute and chronic diseases sensitive to glucocorticoids in cattles. Glucocorticoids can cause serious health problems in humans as a result of residues in milk. In this study, in order to choose the sensitive method for the determination of glucocorticoids in milk, liquid-liquid extraction, solid phase extraction and dispersive solid phase extraction methods were compared and the most sensitive method was selected and validated. Chromatographic separation was performed with Agilent XDB-C18 column (150 mm x 4.6 mm, 5µm). Target analytes were identified by Agilent 1100 series High Performance Liquid Chromatography (HPLC) combined with Diode Array Detector (DAD). The recovery of samples spiked with betamethasone 0.12, 0.3, 0.45 μg/kg ranged from 97% to 102%, the recovery of samples spiked with dexamethasone 0.12, 0.3, 0.45 μg/kg ranged from 97% to 102%, the recovery of samples spiked with methylprednisolone analyte at 0.2, 2, 3μg/kg ranged from 94% to 100%, and the recovery of samples spiked with prednisolone at 0.6, 6, 9μg/kg ranged from 97% to 99%.

Anahtar Kelimeler

• Bethamethasone
• dexamethasone
• prednisolone
• methylprednisolone
• HPLC
• milk
• DAD
• method comparison
• liquid liquid extraction
• solid phase extraction

Sütte Glukokortikoidlerin Analizi İçin Metot Karşılaştırması

Öz

Betametazon, Deksametazon, Prednizolon ve Metilprednizolon büyükbaş hayvanlarda glukokortikoidlere duyarlı çeşitli akut ve kronik hastalıklarda yaygın olarak kullanılan sentetik glukokortikoidlerdir. Glukokortikoidler sütte kalıntı yapmaları sonucu insanlarda ciddi sağlık sorunlarına yol açabilmektedir. Bu çalışmada sütte glukokortikoidlerin belirlenmesine yönelik hassas metodun seçilebilmesi için sıvı-sıvı ekstraksiyon, katı faz ekstraksiyon ve dispersif katı faz ekstraksiyon metotları karşılaştırılmış ve en hassas metot seçilerek valide edilmiştir. Kromatografik ayırım, Agilent XDB-C18 kolonu (150 mm x 4,6 mm, 5µm ) ile gerçekleştirilmiştir. Hedef analitler Diyot Dizi Dedektörü (Diode Array Detector, DAD) ile bütünleşik Agilent 1100 serisi Yüksek Persformanslı Sıvı Kromatografi ( High Performance Liquid Chromatography, HPLC) ile tanımlanmıştır. Betametazon 0.12, 0.3, 0.45 μg/kg seviyesinde analit eklenmiş örneklerin geri alımı %97 ila % 102 arasında, deksametazon 0.12, 0.3, 0.45 μg/kg seviyesinde analit eklenmiş örneklerin geri alımı %97 ila % 102 arasında, metilprednizolon 0.2, 2, 3 μg/kg seviyesinde analit eklenmiş örneklerin geri alımı %94 ila % 100 arasında, prednizolon 0.6, 6, 9 μg/kg seviyesinde analit eklenmiş örneklerin geri alımı %97 ila % 99 arasında değişmiştir.

Anahtar Kelimeler

• Betametazon
• Deksametazon
• Prednizolon
• Metilprednizolon
• HPLC
• süt
• DAD
• metot karşılaştırma
• sıvı sıvı ekstraksiyon
• katı faz ekstraksiyon
• dispersif katı faz ekstraksiyon

Kaynakça

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