Velimir STOJKOVSKI, Pavle SEKULOVSKI, Risto UZUNOV, Dean JANKULOSKI, Elizabeta DIMITRIESKA-STOJKOVIC, Biljana STOJANOVSKA-DIMZOSKA, Zehra HAJRULAI-MUSLIU

Sığır İdrarında 10 Beta Agonist Varlığının Belirlenmesi İçin LC-MS/MS Metodu Geliştirilmesi ve Validasyonu

Bir çok ülkede β-agonistlerin hayvancılıkta kullanılması yasaklanmıştır, çünkü gıda ürünlerinde bulunan β-agonist kalıntıları insan sağlığı için risk oluşturmaktadır. Bu çalışma, komisyon kararı 2002/657/EC ye uygun olarak, sığır idrarındaki 10 adet β-agonistin tespitini sağlayan metod gelişimini ve validasyonunu içermektedir. Doğrusallık korelasyon katsayısı >0.990 ile sonuçlanmıştır. Karar limitleri (CCα) 0.127 ng/ml ile 0.646 ng/ml arasında ve tespit kapasitesi (CCβ) 0.140 ng/mL ile 0.739 ng/ml arasında bir değer almıştır. Geri kazanım %73.67 ile %118.80 arasında bulunmuştur. Korelasyon varyasyonu (CV, %) her üç konsantrasyon seviyesi için Komisyon Kararı 2002/657/EC ‘ye tamamen uygun olarak yapılmıştır. Gün içi kesinlik CV değeri %1.619 ile %15.472 arasında ve günler arası CV kesinlik değeri %2.695 ile %10.441 arasında değişmektedir. Bu çalışmada elde edilen validasyon değerlerine göre geliştirilen metod sığır idrarında β-agonist tespiti için uygundur.

Development and Validation of LC-MS/MS Method for Determination of Ten Beta Agonists in Bovine Urine

The use of β-agonists in livestock production is prohibited in many countries because the residues of β-agonists in food pose a potential riskto human health. The present work describes the development and validation of the LC-MS/MS method for detection of ten β-agonists inbovine urine according to Commission Decision 2002/657/EC requirements. Linearity of the method resulted with coefficient of correlation>0.990. The decision limits (CCα) ranged from 0.127 ng/mL to 0.646 ng/mL, and the detection capability (CCβ) resulted in the range 0.140ng/mL to 0.739 ng/mL. The observed recoveries in the fortified bovine urine samples were satisfactory at every fortification level with valuesfrom 73.67% to 118.80%. The coefficient of variation (CV, %) at three fortification levels for each β-agonist was in complete agreement withthe requirements from Commission Decision 2002/657/EC. The CV for intraday precision varied from 1.619% to 15.472% and the CV forinterday precision varied from 2.695% to 10.441%. From the obtained validation results the proposed method is an appropriate method fordetermination of β-agonists in bovine urine.

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