Spectrofluorimetric determination of organic and inorganic selenium in vitamin supplements after cloud point extraction

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Tezin Türü: Yüksek Lisans

Tezin Yürütüldüğü Kurum: Orta Doğu Teknik Üniversitesi, Fen Edebiyat Fakültesi, Kimya Bölümü, Türkiye

Tezin Onay Tarihi: 2010

Öğrenci: MERVEGÜL MADEN

Danışman: MÜRVET VOLKAN

Özet:

Selenium is a trace and essential element for good health but required only in very narrow range. Hence, determination of selenium in trace level in any matrix related with human health is important. A preconcentration method is performed to obtain a low detection limit for analyte. In this study, the methodology of cloud point extraction (CPE) was used as the preconcentration method for speciation of selenium in vitamin tablets. Non-ionic surfactant Triton X-114 and a fluorimetric ligand, 2,3- diaminonaphtalene (DAN) were used for the extraction of trace levels of organic and inorganic selenium species as a prior step to their determination by spectrofluorimetry. The aqueous solutions of nonionic and zwitterionic surfactant materials become cloudy when temperature reaches the cloud point temperature and analyte collapses with surface active material. The volume of surfactant rich phase is smaller than the solution volume and by this way high preconcentration factor was obtained. Optimization of the CPE parameters affecting complexation and phase separation was performed. Standard addition method was used in the quantitative measurements. Spectrofluorimetric determination of selenium was done using excitation and emission wavelegths of 380 nm end 570 nm respectively. The detection limit, established as 3s /slope where s is the standard deviation of 12 measurements of 0.02 mg/L Se-DAN complex after 10 fold preconcentration was 2.3 µg/L. Accuracy of the method was checked using EnviroMat Waste Water, EU-L-2 as SRM and the result was in good agreement with certified value.Besides, selenium rich vegetables (dill, watercress herb and garlic) were grown in a pot at a controlled atmosphere.Selenium in plants (dill, watercress gerb and garlic), both control and enriched groups was determined by ICP-MS.