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U sklopu ovog diplomskog rada razvijena je i validirana metoda određivanja esencijalnih i toksičnih elemenata As, Ca, Cd, Cu, Mg, Mn, Mo, Fe, Hg, Pb, Se i Zn u uzorcima ljudske kose metodom spektrometrije masa uz induktivno spregnutu plazmu (ICP–MS). Ispitana je učinkovitost različitih načina pranja uzoraka kose (uporaba etil-acetata, metanola, etanola, acetona, dušične i klorovodične kiseline te detergenta - uz ili bez korištenja ultrazvučne kupelji) radi uklanjanja vanjske kontaminacije kose metalima za što nema prihvaćene standardne procedure. Dobiveni rezultati pokazali su da su svi postupci pranja kose za analizu elemenata zadovoljavajući, osim upotrebe dušične i klorovodične kiseline. Ispitani validacijski parametri metode (granica detekcije, granica kvantifikacije, točnost, ponovljivost unutar dana i između dana) zadovoljili su unaprijed postavljene kriterije prihvatljivosti. Primjenom razvijene metode određeni su maseni udjeli elemenata u uzorcima kose rodilja iz kontinentalne i priobalne Hrvatske (N = 167). Rezultati su pokazali značajno više masene udjele Hg, Fe, Mn, Se i Zn te niže masene udjele Ca i Mg u kosi ispitanica iz priobalne u odnosu na kontinentalnu Hrvatsku što se može povezati s većim unosom hrane morskoga podrijetla, razlikama u konzumaciji mliječnih proizvoda i unosa mineralno-vitaminskih dodataka između ispitanica te mineralnim sadržajem tla u tim područjima. As part of this thesis, an inductively coupled plasma mass spectrometry (ICP–MS) method for determination of essential and toxic elements As, Ca, Cd, Cu, Mg, Mn, Mo, Fe, Hg, Pb, Se and Zn in human hair were developed and validated. Since there is no accepted standard procedure, the efficiency of different solutions for washing hair to remove the external contamination was tested (use of ethyl acetate, methanol, ethanol, acetone, nitric and hydrochloric acid and detergent - with or without the use of an ultrasonic bath). The results shows that all used hair washing procedures are satisfactory, except with nitric and hydrochloric acid as washing solution. The validation parameters tested in this study (limit of detection, limit of quantification, accuracy, repeatability within days and between days) were fit into the previously eligibility criteria. Mass fraction of elements in hair of postpartum women in continental and coastal Croatia (N = 167) were determinate by development method. Results showed that subjects from coastal Croatia had significant higher mass fractions of Hg, Fe, Mn, Se and Zn and lower mass fractions of Ca and Mg in hair, which may be related with higher fish intake, differences in dairy consumption and mineral-vitamin supplements intake between the subjects and the different soil mineral content in the coastal area vs. continental area. |
