Comparison of high pressure liquid chromatography methods in fish and fish products by usingo-phthaldialdehyde and benzoyl chloride derivatization for the determination of histamine levels

Abstract

In this study, by the parameters of validation a comparison of two high pressure liquid chromatography (HPLC) methods one of which utilizes coupled the FLD and the o-phthaldialdehyde derivatization method of Antoine et al. (1999) versus DAD coupled, benzoyl chloride derivatization method with a modification of Özdestan and Üren (2009) were made for the selection of sensitive and safe assay for the determination of histamine. Alive horse mackerels caught from the sea of Marmara in Kucukcekmece Istanbul were used for the limit of detection studies. For the other validation parameters, recovery, accuracy, precision and comparison of methods a certified reference material; FAPAS T2775QC were used. Results of the analyses indicated that the FLD coupled; o-phthaldialdehyde derivatization method the limit of quantification (LOQ) and recovery were 1.38 ppm and 100% respectively; and for DAD coupled; benzoyl chloride derivatization modified method these values were 10.66 ppm and 88% respectively. There was a significant difference between for both methods in t-test (p<0.5). According to the calculations of Horrat value; the reproducibility was normal for o-phthaldialdehyde method but found to be higher than the accepted limits in benzoyl chloride method. In conclusion, it is advised to choose FLD coupled o-phthaldialdehyde derivatization method for the safe and sensitive determination of histamine in fish and fish products

Keywords

• Fish
• fish products
• histamine
• methods
• validation

Balık ve balık ürünlerinde histamin düzeylerinin tespiti için o-fitaldialdehit ve benzoil klorür türevlendirmesi kullanılan yüksek performans sıvı kromatografisi yöntemlerinin karşılaştırılması

Abstract

Çalışmada histamin düzeylerinin hassas ve güvenilir bir şekilde tespit edilmesi için, yüksek performans sıvı kromatografisi (HPLC) cihazı kullanılarak Antoine ve ark. (1999) tarafından önerilen floresans dedektör (FLD) ve o-fitaldialdehit türevlendirmesi kullanılan yöntem ile Özdestan ve Üren (2009) tarafından geliştirilen fotodiyot array dedektörü (DAD) ve benzoil klorür türevlendirmesinin kullanıldığı yöntem validasyon parametreleri kullanılarak karşılaştırılmıştır. Teşhis limiti çalışmaları için İstanbul’da Küçükçekmece sahilinden tutulan canlı istavrit balığı, geri kazanım, doğruluk, kesinlik parametreleri ve yöntemler arası karşılaştırma için ise sertifikalı referans materyal olan FAPAS T2775QC kullanılmıştır. Yapılan analizler sonucunda FLD ve o-fitaldialdehit türevlendirmesi ile elde edilen ölçüm limiti (LOQ) 1.38 ppm, geri kazanım %100; benzoil klorür yönteminde bu parametreler 10.66 ppm ve % 88’dir. Her iki yöntemde de yapılan t-testi hesaplamalarına göre iki yöntem arasındaki fark anlamlıdır (p<0.5). Horrat Değeri hesaplamalarına göre o-fitaldialdehit yönteminde tekrar üretilebilirlik normal bulunurken, benzoil klorür yöntemi için tekrar üretilebilirlik beklenenden daha yüksektir. Sonuç olarak balık ve balık ürünlerinde histamin düzeylerinin tespiti için FLD ve o-fitaldialdehit yönteminin hassasiyetinin ve güvenilirliğinin uygun olduğu ve rutin analizlerde kullanılabileceği kanısına varılmıştır

Keywords

• Balık
• balık ürünleri
• histamin
• metot
• validasyon

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