Bitkisel yağ analizleri için geciktirmeli ve ön deriştirmeli SPE sistemlerinin FIA-HPLC sistemlerine entegrasyonu ve uygulamalarının geliştirilmesi
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Tarih
2015-09-30
Yazarlar
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Yayıncı
Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bitkisel yağlar esas olarak trigliserit molekülleri ve farklı kimyasal yapılı bileşiklerin oluşturduğu kompleks bir karışım olan minör bileşenlerden oluşmaktadır. Trigliserit molekülleri yağ içerisinde yüksek miktarda bulunmaları (~95-98%) nedeniyle temel bileşenler; karakteristik özellikleri kazandıran minör bileşenler (~5-2%) ise ikincil bileşenler olarak adlandırılmaktadır. Yağların kalitesi, kaynağı, tağşişi ve diğer bazı özelliklerinin belirlenebilmesi için, yağlarda bulunan bir çok bileşenin çeşitli analitik yöntemler kullanılarak tayin edilmesi gerekmektedir. Bu tayinler genellikle standart metotlar olarak bilinen metotlar kullanılarak gerçekleştirilmektedir. Yağların özelliklerinin belirlenmesinde kullanılan standart metotların uygulamaları ve gerektirdiği ön işlemler; oldukça maliyetli, zaman alan, zahmetli ve çevre açısından tehlike oluşturan çözücülerin fazla miktarda kullanımını gerektirmektedir. Bu nedenle; uygulanmakta olan standart metotlara alternatif olabilecek, çevre dostu yeni yağ analiz metotlarının geliştirilmesi gerekmektedir. Sunulan çalışma ile; birçok yağ analizinin ön işlem basamağında yer alan SPE tekniğinin, FIA ve HPLC sistemlerine entegrasyonu ile, bitkisel yağlarda mevcut türlerin tek bir enjeksiyon ile 3 boyutlu kromatografik tayinleri için; numune ön işlemlerinin on-line gerçekleştirilebildiği ve analizci müdahalesinin en aza indirildiği "On-line SPE-FIA-HPLC yağ analiz sistemi" oluşturulmuş ve sistem üzerinde yeni yağ analiz metotlarının geliştirilip/ uygulanabilirliği gerçekleştirilmiştir. Dünyada ve Türkiye'de ilk kez geliştirilen bu yeni analiz sistemi; HPLC sistemine değişik özelliklerdeki kolon, dedektör, çok yollu valf sistemleri ve bağlantı elamanlarının adapte edilmesi ile oluşturulmuştur. Yağların özelliklerinin belirlenmesinde önem arz eden ve genellikle standart metotlar kullanılarak gerçekleştirilen trigliserit, sterol, tokol, digliserit, monogliserit, FFA ve fosfolipit tayinlerinin her birisi, oluşturulan bu yeni sistem üzerinde denenmiş ve önemli deneysel parametrelerin optimizasyon çalışmaları gerçekleştirilmiştir. Deneysel parametrelerin optimizasyonu için kemometrik yaklaşım izlenerek deneysel tasarım çalışmaları uygulanmıştır. Optimum parametreler kullanılarak yürütülen analizler için; lipit standartlarının yanında ayçiçek, mısır, pamuk, soya, kanola, palm, zeytinyağı gibi farklı özellikteki bitkisel yağ numuneleri de kullanılmıştır. Sonuç olarak; bitkisel yağların özelliklerini belirlemede önem arz eden tayinlerin tamamının, numune ön işlemlerinin on-line gerçekleştirildiği tek bir analiz sistemi üzerinde, tek bir enjeksiyon ile yapılabilirliği dünya literatüründe ilk kez önerilmiş ve kapsamlı bir şekilde incelenmiştir. Elde edilen veriler neticesinde; yağlarda mevcut lipit türlerinin tayini için daha kısa sürede, yüksek oranda iyileştirilmiş ayrımların elde edilebildiği analizler gerçekleştirilebilmiştir. Çalışmanın sanayi uygulaması ile; ülkemiz yağ sektörü açısından son derece önem arz eden analizlerin, otomatikleştirilmiş sistemlerde gerçekleştirilmesine imkan sağlanacaktır. Yağlarda mevcut farklı fiziksel ve kimyasal özelliklere sahip önemli türlerin tayini için; özel bir sistem dizaynı ve enstrümantasyonu ile tamamlanan bu yeni sistem uygulamasının, "modern birleştirilmiş analiz sistemlerinin geliştirilmesi ve uygulamaları" ile ilgilenen araştırmacılar için yeni ufuklar açacağı kanaatindeyiz.
Vegetable oils are composed mainly triglyceride molecules and minor components that are a mixture of complex compounds formed different chemical structure. Triglyceride molecules are called as basic components of the oil due to the high amounts (~95-98%) according to the other components; minor compounds (~5-2%) that determine the characteristics of oils, are called as secondary components of the oil. To determine the quality of extraction and refinery process conditions used for crude and refined oil, detection source of the oil and oil adulteration, the main (triglycerides) and secondary components (minor compounds) must be identify as qualitative and quantitative by applying various analytical methods. These oil analysis are generally carried out by using several methods as known standard methods. The standard methods, other methods and front procedures applied for oil analysis, that are required for quality-control determination of the oils; are very costly, time-consuming, laborious and requires the use of large amounts of solvents that may be dangerous to the health of the environment. Therefore; the new alternative methods must be developed and optimized supporting conservation in term of time and solvent, environmentally friendly. With this study a new "On-line SPE-FIA-HPLC oil analysis system" was developed for three-dimensional chromatographic analysis of vegetable oils with a single injection, that allow the automatic sample pre-treatments and a results can be achieved by minimizing the analyst intervention, by integration of the SPE technique that being implemented to pre-treatment step of many oil analysis to the FIA and HPLC systems and gained the applicability of new oil analysis methods with this system. This system was recommended in the world and Turkey for the first time and developed by adapting the various detectors, columns, multi-valve systems and necessary system components to the HPLC system in chemistry laboratory. By means of the SPE-HPLC-FIA hyphenated system, the quality control analysis of vegetable oils, such as triglyceride, sterol, tocols, diglycerides, monoglycerides, free fatty acids and phospholipid analyses, were achieved and the pre-treatment procedures were carried out as on-line over the system. For method optimization studies, the experimental designs were utilized by using a chemometric approach and different vegetable oil samples, such as sunflower, corn, cottonseed, soybean, canola, were used. Consequently, the study suggested that all quality-control determinations/analysis of vegetable oils could be done in a single analysis system, by performing the sample pre-treatments as on-line with a single injection in the literature for the first time. The results indicate that the lipid analysis could be done in a short time and separations could be carried out with highly improved separation. In addition, if this application goes to the industrial application work, it will be a national resource for other research or implementation activities related to oil analysis and allows the analysis that are extremely significant for our country's oil sector could be carried out by minimizing the analyst intervention on automated systems. We believe that the study, completed with a special system design and instrumentation, will open new horizons for the researchers interested in "the development & implementation of modern unified analysis systems".
Vegetable oils are composed mainly triglyceride molecules and minor components that are a mixture of complex compounds formed different chemical structure. Triglyceride molecules are called as basic components of the oil due to the high amounts (~95-98%) according to the other components; minor compounds (~5-2%) that determine the characteristics of oils, are called as secondary components of the oil. To determine the quality of extraction and refinery process conditions used for crude and refined oil, detection source of the oil and oil adulteration, the main (triglycerides) and secondary components (minor compounds) must be identify as qualitative and quantitative by applying various analytical methods. These oil analysis are generally carried out by using several methods as known standard methods. The standard methods, other methods and front procedures applied for oil analysis, that are required for quality-control determination of the oils; are very costly, time-consuming, laborious and requires the use of large amounts of solvents that may be dangerous to the health of the environment. Therefore; the new alternative methods must be developed and optimized supporting conservation in term of time and solvent, environmentally friendly. With this study a new "On-line SPE-FIA-HPLC oil analysis system" was developed for three-dimensional chromatographic analysis of vegetable oils with a single injection, that allow the automatic sample pre-treatments and a results can be achieved by minimizing the analyst intervention, by integration of the SPE technique that being implemented to pre-treatment step of many oil analysis to the FIA and HPLC systems and gained the applicability of new oil analysis methods with this system. This system was recommended in the world and Turkey for the first time and developed by adapting the various detectors, columns, multi-valve systems and necessary system components to the HPLC system in chemistry laboratory. By means of the SPE-HPLC-FIA hyphenated system, the quality control analysis of vegetable oils, such as triglyceride, sterol, tocols, diglycerides, monoglycerides, free fatty acids and phospholipid analyses, were achieved and the pre-treatment procedures were carried out as on-line over the system. For method optimization studies, the experimental designs were utilized by using a chemometric approach and different vegetable oil samples, such as sunflower, corn, cottonseed, soybean, canola, were used. Consequently, the study suggested that all quality-control determinations/analysis of vegetable oils could be done in a single analysis system, by performing the sample pre-treatments as on-line with a single injection in the literature for the first time. The results indicate that the lipid analysis could be done in a short time and separations could be carried out with highly improved separation. In addition, if this application goes to the industrial application work, it will be a national resource for other research or implementation activities related to oil analysis and allows the analysis that are extremely significant for our country's oil sector could be carried out by minimizing the analyst intervention on automated systems. We believe that the study, completed with a special system design and instrumentation, will open new horizons for the researchers interested in "the development & implementation of modern unified analysis systems".
Açıklama
Anahtar Kelimeler
Bitkisel yağ, Lipit, 3-boyutlu kromatografi, Birleştirilmiş analiz sistemi, Kemometri, Vegetable oil, Lipids, Three-dimensional chromatography, Multi-dimensional separation system, Chemometrics
Kaynak
WoS Q Değeri
Scopus Q Değeri
Cilt
Sayı
Künye
Arslan, F. N. (2015). Bitkisel yağ analizleri için geciktirmeli ve ön deriştirmeli SPE sistemlerinin FIA-HPLC sistemlerine entegrasyonu ve uygulamalarının geliştirilmesi. Selçuk Üniversitesi, Yayımlanmış doktora tezi, Konya.
