Bitkisel yağ deodorize distilatındaki E vitamininin karakterizasyonu ve yarı- preparatif HPLC ile geri kazanımı
Yükleniyor...
Tarih
2019
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu tez çalışmasında; yarı-preparatif HPLC tekniği kullanılarak, herhangi bir ön işleme tabii tutulmayan deodorize distilatında bulunan tokoferol ve tokotrienoller ayrılmaya ve GC-MS sistemi ile bu maddeler karakterize edilmeye çalışılmıştır. Tokol tayini baz alarak gerçekleştirilen deneyler; ilk aşama deodorize distilatlardaki tokoferol ve tokotrienol varlığını belirlemek ve birbirinden ayırtetmek için analitik HPLC ile optimizasyon çalışmaları, ikinci aşama belirlenen tokoferol ve tokotrienol fraksiyonlarını toplamak için yarı preparatif HPLC analizleri ve son aşama da toplanan bu fraksiyonları karakterize etmek için gaz kromatografisi kütle spektroskopi (GC-MS) analizleri olmak üzere 3 aşama da gerçekleştirilmiştir. Analizler; Agilent 1200 yüksek performanslı sıvı kromatografisi (HPLC-FLD-DAD) ve Agilent 7890N-5975C gaz kromatografisi kütle spektroskopi (GC-MS) cihazları ile gerçekleştirilmiş olup, deneylerde Reprosil-Pur 120 CN, sabit fazı Silicycle CN 120 A 10 µm olan laboratuvarda hazırlanan kolon ve HP-5MS (30 m x 0.25 mm; 0.25 µm) kolonları kullanılmıştır. Deneylerden elde edilen sonuçlardan, mısır yağı deodorize distilatında yapılan incelemede sabunlaştırma işlemi yapmadan %1,54 α-tok, %0,21 β ve Ɣ tok, %0,13 δ-tok olmak üzere %1,88 toplam tokoferol içerdiği görülmüştür. Yarı-preparatif HPLC tekniği ile toplanan 6 fraksiyon içerikleri GC-MS ile analiz edildiğinde, Frk-1 ve Frk-2 çeşitli yağ asitleri ve esterlerini, Frk-3 α-tok ve α-tokotrienol, Frk-4 β-tok ve δ- tok, Frk-5 β ve δ tokotrienol ve Frk-6 ise δ-tok ve sterol çeşitleri içerdiği tespit edilmiştir.
In this thesis study; using semi-preparative HPLC technique, tocopherol and tocotrienols in the deodorized distillate which were not subjected to any pretreatment, were separated and characterized by GC-MS system. In experiments carried out based on the determination of tocol three stages were performed; the first stage is optimization analysis by analytical HPLC to determine the presence of tocopherol and tocotrienol in deodorized distillates, the second stage is semi-preparative HPLC analysis to collect the determined tocopherol and tocotrienol fractions, and the final stage is gas chromatography mass spectroscopy (GC-MS) analysis to characterize these fractions collected. In this thesis; semi-preparative HPLC analysis was performed using Agilent 1200 high performance liquid chromatography (HPLC-FLD-DAD) and Agilent 7890N-5975C gas chromatography mass spectroscopy (GC-MS) devices.In addition, Reprosil-Pur 120 CN (250x4.6; 5µm), the stationary phase Silicycle CN 120 A 10 µm laboratory column and HP-5MS (30 m x 0.25 mm; 0.25 µm) columns were used in the experiments. According to the results obtained from the experiments, corn oil deodorized distillate showed that 1.54% α-toc, 0.21% β and Ɣ toc, and 0.13% δ-toc without to saponification, 1.88% total tocopherol. When the contents of 6 fractions collected by semi-preparative HPLC technique were analyzed by GC-MS, Frk-1 and Frk-2 are various fatty acids and esters, Frk-3 α-toc and α tocotrienol, Frk-4 β-toc and δ-toc, Frk-5 β and δ tocotrienol and Frk-6 δ-toc and sterol varieties were found to contain.
In this thesis study; using semi-preparative HPLC technique, tocopherol and tocotrienols in the deodorized distillate which were not subjected to any pretreatment, were separated and characterized by GC-MS system. In experiments carried out based on the determination of tocol three stages were performed; the first stage is optimization analysis by analytical HPLC to determine the presence of tocopherol and tocotrienol in deodorized distillates, the second stage is semi-preparative HPLC analysis to collect the determined tocopherol and tocotrienol fractions, and the final stage is gas chromatography mass spectroscopy (GC-MS) analysis to characterize these fractions collected. In this thesis; semi-preparative HPLC analysis was performed using Agilent 1200 high performance liquid chromatography (HPLC-FLD-DAD) and Agilent 7890N-5975C gas chromatography mass spectroscopy (GC-MS) devices.In addition, Reprosil-Pur 120 CN (250x4.6; 5µm), the stationary phase Silicycle CN 120 A 10 µm laboratory column and HP-5MS (30 m x 0.25 mm; 0.25 µm) columns were used in the experiments. According to the results obtained from the experiments, corn oil deodorized distillate showed that 1.54% α-toc, 0.21% β and Ɣ toc, and 0.13% δ-toc without to saponification, 1.88% total tocopherol. When the contents of 6 fractions collected by semi-preparative HPLC technique were analyzed by GC-MS, Frk-1 and Frk-2 are various fatty acids and esters, Frk-3 α-toc and α tocotrienol, Frk-4 β-toc and δ-toc, Frk-5 β and δ tocotrienol and Frk-6 δ-toc and sterol varieties were found to contain.
Açıklama
Anahtar Kelimeler
Deodorizasyon, deodorize distilat, tokoferol, tokotrienol, yarı-preparatif HPLC, Deodorization, deodorizer distillate, tocopherol, tocotrienol, semi-preparative HPLC
Kaynak
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Künye
Taş, H. Ç. (2019). Bitkisel Yağ Deodorize Distilatındaki E Vitamininin Karakterizasyonu ve Yarı- Preparatif HPLC ile Geri Kazanımı. (Yüksek Lisans Tezi). Selçuk Üniversitesi, Fen Bilimleri Enstitüsü, Konya.