Kırmızı Pul Biberde Bazı Azo Boyaların LC-MS/MS ile Belirlenmesi

Yıl 2019, Sayı: 21, 26 - 39, 25.02.2019

Ayşe Binnur Karataş İbrahim Emre Tokat Ayşegül Arıkan Asan

Öz

Amaç: Çalışmada, 11 adet azo boyanın (Sudan I, Sudan
II, Sudan III, Sudan IV, Sudan Orange G, Sudan Black B, Sudan Red B, Sudan Red
7B, Sudan Red G, Para Red, Rhodamine B) kantitatif olarak tespiti için LC-MS/MS
cihazı kullanarak metot validasyonu yapılmıştır.

Materyal
ve Yöntem: Çalışmada kırmızı
pul biber kullanılmıştır. Örnekler asetonitril ile ekstrakte edilmiştir. Kantitatif
hesaplamalar matriks uyumlu kalibrasyona göre yapılmıştır. Doğrulama için;
doğrusallık, tekrarlanabilirlik, tekrarüretilebilirlik, tespit limiti (LoD),
ölçüm limiti (LoQ) ve geri kazanım parametreleri incelenmiştir. Tüm azo
boyaları için ölçüm belirsizliği hesaplanmıştır.

Bulgular: Tüm boyalar için doğrusallık r²≥0,99 olarak saptanmıştır. LoD değerleri
0,62-13,12 µg/kg
aralığında iken, LoQ değerleri ise 2,06-43,72 µg/kg aralığında bulunmuştur. Geri kazanım oranları %83,38-100,27 arasında değişmiştir. 

Sonuç: LC-MS/MS metodunun, pul biberde azo boyaların tespiti
için yüksek hassasiyette ve uygulanabilir olduğu belirlenmiştir.

            Objective: In this study, a method validation is performed for quantitative detection
of 11 azo dyes (Sudan I, Sudan II, Sudan III, Sudan IV, Sudan Orange G, Sudan
Black B, Sudan Red B, Sudan Red 7B, Sudan Red G, Para Red, Rhodamine B) by
using LC-MS/MS system.

Material
and Methods: In this study red
pepper flakes were used and the samples were extracted with acetonitrile. Matrix-match
calibration was used for quantification. Linearity, repeatability, reproducibility,
limit of detection (LoD), limit of quantification (LoQ) and recovery were
studied as validation parameters. Uncertainity was calculated for all azo dyes.

Results: Linearity obtained for all dyes were r²≥0,99. LoD and LoQ were in the range of
0,62-13,12 µg/kg and
2,06-43,72 µg/kg
respectively. Recovery range was between 83,38-100,27%.

Conclusion: LC-MS/MS method was found to be high
sensitivity and applicable for detection of azo dyes in red pepper flakes. 

Anahtar Kelimeler

Azo Boyalar, Sudan Boyaları, LC-MS/MS, Kırmızı Pul Biber, Validasyon, Azo Dyes, Sudan Dyes, Red Pepper Flakes, Verification

Kaynakça

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