Prosülfokarbın Gaz Kromatografisi-Kütle Spektrometrisi ile Patates Unu Örneklerinde Tayini

Yıl 2024, Cilt: 14 Sayı: 3, 129 - 135, 25.11.2024

Sezin Erarpat Bodur

Öz

Bu çalışmada, patates unu örneklerinde prosülfokarbın tayini için bir gaz kromatografisi-kütle spektrometresi (GC-MS) yöntemi geliştirilmiştir. Yüksek sinyal/gürültü oranına sahip iyi ayrılmış analit sinyali elde etmek için GC-MS parametreleri ayrıntılı bir şekilde değerlendirilmiştir. Optimum enstrümantal koşullar altında, gözlenebilme ve tayin limitleri (GL ve TL) sırasıyla 0,54 mg/kg ve 1,80 mg/kg olarak bulunmuştur, bu da prosülfokarbın ppm seviyelerinde belirlenmesine imkân tanımaktadır. Belirlenen yöntem, altı farklı konsantrasyon seviyesinde (2,6-101,7 mg/kg) standart eklenen patates unu örneklerine uygulanmıştır. Üç farklı marka örnek için kör analizler yapılmış ancak prosülfokarb, tespit limitinin altında bulunmuştur. Seçilen örnek matriksi için %RSD (≤%3,6) ile %90,9 ile %105,7 arasında kabul edilebilir yüzde geri kazanımlar elde edilmiştir. Matriks eşleştirme kalibrasyon stratejisi kullanılarak elde edilen yüksek geri kazanımlar, geliştirilen yöntemin doğruluğunu ve uygulanabilirliğini kanıtlarken, düşük %RSD değerleri analitik yöntemin kesinliğini göstermiştir. Örnek çözeltilerine ön deriştirme yöntemi uygulandıktan sonra analitin ppb/ppt seviyelerini tespit etmek için oluşturulan yöntemin kullanılabileceği önerilmektedir.

Anahtar Kelimeler

GC-MS, matriks eşleştirme kalibrasyon yöntemi, patates unu, prosülfokarb

Determination of Prosulfocarb in Potato Flour Samples by Gas Chromatography-Mass Spectrometry

Öz

In this study, a gas chromatography-mass spectrometry (GC-MS) method was developed for the detection of prosulfocarb in potato flour matrix. GC-MS parameters were elaborately evaluated to achieve well-separated analyte signal with high signal to noise ratio. Under the optimum instrumental conditions, the limits of detection and quantification (LOD and LOQ) were found as 0.54 mg/kg and 1.80 mg/kg, respectively, which facilitates the determination of prosulfocarb at ppm levels. The established method was applied to potato flour samples spiked to six different concentration levels (2.6–101.7 mg/kg). Blank analyses were also performed for three different brand samples but prosulfocarb were found in the samples below the detection limit. Satisfactory percent recoveries between 90.9 and 105.7% with %RSD (≤3,6%) were acquired for the selected sample matrix. High recoveries obtained with the matrix matching calibration strategy proved the accuracy and applicability of the developed method while low %RSD value showed the precision of the analytical method. It is suggested that the established method can be used to detect ppb/ppt levels of the analyte after a preconcentration method was applied to the sample solutions.

Anahtar Kelimeler

GC-MS, matrix matching calibration method, potato flour, prosulfocarb

Kaynakça

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