Ekmek ve bazı unlu mamullerde HG-AAS ile selenyum analizi ve karşılaşılan analitik problemler
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Date
2012
Authors
Ersoy, Muazzez
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Publisher
Uludağ Üniversitesi
Abstract
Bu çalışmada, hidrür oluşturmalı atomik absorpsiyon spektrometrisi (HGAAS) ile ekmek ve unlu mamüllerde selenyum tayini yapılmıştır. Homojen hale getirilen numuneler açık sistem ve mikrodalga sistem çözünürleştirme ile hazırlanmıştır. Uygun çözünürleştirme yöntemi olarak mikrodalga sistem belirlendikten sonra HCl derişimi, NaBH4 derişimi ve taşıyıcı gazın akış hızı vb. değişkenlerin en uygun değerleri deneysel olarak saptanmıştır. Ekmek ve unlu mamullerde bulunabilecek elementler ile HGAAS'de tayin edilebilen elementlerin girişim etkileri de incelenmiştir. HGAAS için gözlenebilme sınırı (LOD) ve gözlenebilme miktarı (LOQ) sırasıyla; 0,53 ?g/mL, 1,78 ?g/mL olarak tespit edildi. Yöntemin doğruluğunun kontrolü için standart referans madde olarak 1567a wheat flour kullanıldı. HGAAS ile yapılan analizlerde selenyum kepekli ekmek çeşitlerinde 0,50-2,10 µg/g, beyaz ekmek çeşitlerinde 0,10-1,25 µg/g, çavdar ekmek çeşitlerinde 0,15-1,45 µg/g, farklı un çeşitlerinde 0,30-1,35 µg/g, mayalarda 0,1-0,6 µg/g, simitte 0,20 µg/g ve açmada 1,84 µg/g olarak tespit edilmiştir.
A method has been developed for the determination of selenium in bread and flour products using hydride generation atomic absorption spectrometry (HGAAS). Homogenized samples are prepared by open and microwave wet digestion system. Microwave digestion has been chosen for appropriate wet-digestion procedure. Optimum values of the variables such as HCl and NaBH4 concentration, flow rate of the carrier gas were determined experimentally. The interfering effects of the elements which is possibibly present in bread and flour products and the elements which could be determined by HGAAS were investigated. Limit of detection (LOD) and limit of quantification (LOQ) were also determined for HGAAS as 0.53 ?g mL-1, 1.78 ?g mL-1, inrespectively. Standard reference materials such as 1567a wheat flour was used to control methods. Selenium concentrations are found 0.50-2.10 µg g-1 in whole wheat bread, 0.10-1.25 µg g-1 in white bread, 0.15-1.45 µg g-1 in rye bread, 0.30-1.35 µg g-1 in different flours, 0.1-0.6 µg g-1 in yeast, 0.20 µg g-1 in simit (ring-shaped bread with sesame ) and 1.84 µg g-1 in acma (savory pastry).
A method has been developed for the determination of selenium in bread and flour products using hydride generation atomic absorption spectrometry (HGAAS). Homogenized samples are prepared by open and microwave wet digestion system. Microwave digestion has been chosen for appropriate wet-digestion procedure. Optimum values of the variables such as HCl and NaBH4 concentration, flow rate of the carrier gas were determined experimentally. The interfering effects of the elements which is possibibly present in bread and flour products and the elements which could be determined by HGAAS were investigated. Limit of detection (LOD) and limit of quantification (LOQ) were also determined for HGAAS as 0.53 ?g mL-1, 1.78 ?g mL-1, inrespectively. Standard reference materials such as 1567a wheat flour was used to control methods. Selenium concentrations are found 0.50-2.10 µg g-1 in whole wheat bread, 0.10-1.25 µg g-1 in white bread, 0.15-1.45 µg g-1 in rye bread, 0.30-1.35 µg g-1 in different flours, 0.1-0.6 µg g-1 in yeast, 0.20 µg g-1 in simit (ring-shaped bread with sesame ) and 1.84 µg g-1 in acma (savory pastry).
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Keywords
Selenyum, Ekmek, Unlu mamuller, Hidrür oluşturmalı atomik absorpsiyon spektroskopisi, Selenium, Bread, Flour products, Hydride generation atomic absorption spectrometry
Citation
Ersoy, M. (2012). Ekmek ve bazı unlu mamullerde HG-AAS ile selenyum analizi ve karşılaşılan analitik problemler. Yayınlanmamış yüksek lisans tezi. Uludağ Üniversitesi Fen Bilimleri Enstitüsü.