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Bioakumulacija Metala U Odabranim Vrstama Voća I Lekovitih Biljaka

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Bioakumulacija Metala U Odabranim Vrstama Voća I Lekovitih Biljaka UNIVERZITET U NIŠU PRIRODNO MATEMATIČKI FAKULTET DEPARTMAN ZA HEMIJU Saša S. Ranđelović BIOAKUMULACIJA METALA U ODABRANIM VRSTAMA VOĆA I LEKOVITIH BILJAKA Doktorska disertacija Niš, 2015. UNIVERSITY OF NIŠ FACULTY OF SCIENCE AND MATHEMATICS DEPARTMEN OF CHEMISTRY Saša S. Ranđelović BIOACCUMULATION OF METALS IN SELECTED TYPES OF FRUITS AND MEDICINAL HERBS PhD thesis Niš, 2015. Mentor: dr Danijela Kostić, redovni profesor prirodno-matematičkog fakulteta Univerziteta u Nišu dr Snežana Mitić, redovni profesor prirodno-matematičkog fakulteta Univerziteta u Nišu Članovi komisije: dr Goran Nikolić, redovni profesor tehnološkog fakulteta u Leskovcu Univerziteta u Nišu dr Aleksandra Zarubica, vanredni profesor prirodno-matematičkog fakulteta Univerziteta u Nišu dr Aleksandra Pavlović, vanredni profesor prirodno-matematičkog fakulteta Univerziteta u Nišu Verovatno je ovo pravo mesto i odgovarajuće vreme da izrazim svoju zahvalnost svima koji su doprineli izradi ovog rada. Prvenstveno veliku zahvalnost dugujem svom mentoru prof. dr. Danijeli Kostić na pomoći i vođenju tokom postdiplomskih studija, na stručnim sugestijama, smernicama i komentarima prilikom izrade ove teze. Zahvalnost dugujem i prof. dr. Snežani Mitić koja je u završnoj fazi pisanja rada dala korisne stručne savete i sugestije. Bivšem šefu koji je podstakao moje analitičko razmišljanje. Jakši i Urošu koji su mi svojom ljubavlju davali snagu da istrajem u svojim zamislima i imali razumevanja za moj rad i ambicije tokom prethodnih godina. Posebnu zahvalnost dugujem mojoj majci na nesebičnoj podršci i ljubavlji čak i onda kada su moje želje bile teško ostvarive, na prilici da učim i radim ono što volim. Autor Termini i skraćenice Analit - Komponenta ili grupa komponenti čije prisustvo/odsustvo ili pak njihovu masu/koncentraciju treba odrediti u ispitvanom uzorku, Analiza - Metoda koja se koristi za detekciju, indentifikaciju i/li određivanje analita u ispitvanom uzorku, Alikvot - Tačno poznata zapremina ispitivanog rastvora koja se koristi direktno za određivanje prisustva/odsustva ili mase/koncentracije analita bez karakteristične greške uzorkovanja, Slepa proba - Slepa proba je uzorak koji sadrži sve komponente kao ispitvani uzorak izuzev analita, Detekcija - Određivanje prisustva analita kao hemijskog entieta, Određivanje (kvantifikacija) - Određivanje apsolutnog sadržaja analita (mase, zapremine, količine) ili relativnog sadržaja analita (frakcije mase, masene koncentracije) u ispitvanom uzorku, Matriks - Sve komponente ispitvanog uzorka izuzev analita, Ispitivanje - tehnička operacija za utvrđivanje jedne ili više karakteristika datog proizvoda, procesa ili usluge po specificiranom postupku, Provera (validacija) ispitnih metoda - potvrđivanje ispitivanjem i prikupljanjem objektivnih dokaza da su posebni zahtevi za predviđenu upotrebu zadovoljeni, Predmet ispitivanja/ispitni uzorak - materijal ili predmet podvrgnut procesu ispitivanja, Metoda ispitivanja - utvrđeni tehnički postupak za obavljanje ispitivanja, Rezultat ispitivanja - vrednost jedne karakteristike dobijena kao rezultat jedne specificirane metode ispitivanja, Srednja vrednost rezultata ispitivanja ( ) - zbir pojedinačnih rezultata ispitivanja x podeljen sa brojem ispitivanja n, Stvarna vrednost - bliskost u slaganju aritmetičkih sredina (srednjih vrednosti) rezultata velikog broja ispitivanja sa istinitom vrednošću ili (ukoliko ona nije poznata) prihvaćenom referentnom vrednošću, Broj stepena slobode (df) - broj ispitivanja umanjen za 1 (n-1), Standardna devijacija (procenjena) (s) - mera rasipanja vrednosti slučajne promenljive oko srednje vrednosti x, izražena u jedinicama u kojima je izražena i slučajna promenljiva, Varijansa slučajne promenljive (σ2) - mera rasipanja kvadrata standardnog odstupanja/ devijacije slučajne promenljive oko matematičkog očekivanja (prave vrednosti): σ2 odnosno s2 u slučajevima procenjene varijanse, Verovatnoća (p) - verovatnoća realizacije nekog događaja izražena kroz odnos broja realizacija povoljnih tom događaju i broja ukupno mogućih realizacija, Interval poverenja - interval u kojem se po utvrđenoj verovatnoći pretpostavlja da će se naći merena veličina, Preciznost - određuje se u odnosu na bliskost u slaganju između nezavisnih rezultata merenja jedne veličine koja su više puta izvedena na istom uzorku i pod identičnim unapred utvrđenim uslovima merenja. Ona se po konvenciji izražava standardnom devijacijom, Granica ponovljivosti (r) - vrednost manja ili jednaka apsolutnoj razlici između dva pojedinačna rezultata merenja koji su dobijeni pod uslovima ponovljivosti i kod očekivane verovatnoće 95%, Reproduktivnost (R) - razlika između dva pojedinačna i nezavisna rezultata dobijena od različitih izvršilaca koji rade u različitim laboratorijama na istom uzorku, Uslovi reproduktivnosti - uslovi kod kojih su rezultati ispitivanja na identičnom materijalu dobijeni u izmenjenim uslovima koji mogu biti: različite metode, različite laboranti, različita oprema, referentni standardi, lokacija i vreme, Granica reproduktivnosti - vrednost manja ili jednaka apsolutnoj razlici između dva pojedinačna rezultata merenja dobijena pod uslovima reproduktivnosti i kod očekivane verovatnoće 95%, Relativna standardna devijacija ili koeficijent varijacije cv (rsd)- bezdimenziona veličina koja predstavlja odnos standardne devijacije i srednje vrednosti, Kritična interval (critical range) cr - maksimalna razlika rezultata n-ispitivanja za verovatnoću raspodele kod koje je srednja vrednost rezultata prihvatljiva, Greška - razlika između stvarne vrednosti i vrednosti dobijene pojedinačnim ispitivanjem. Greške se mogu podeliti na: slučajne, sistematske i grube, Gruba greška - neprihvatljivi rezultat merenja nastao najčešće kao ljudska greška ili greška u funkciji instrumenta. Uzroci pojave grubih grešaka su obično banalni: upotreba pogrešnog reagensa, vazdušni mehuri u protočnoj kiveti spektrofotometra, kontaminacija uzorka itd. Merenja sa ovakvim greškama se moraju identifikovati i kroz jedan test proceniti i eventualno odbaciti kako ne bi uticali na podatke statističke analize, Sistematska greška merenja (bias)- razlika između srednje vrednosti n pojedinačnih merenja i stvarne vrednosti. One se mogu poznati po konstantno povećanim ili smanjenim vrednostima rezultata merenja i mogu se korigovati ukoliko se prepoznaju. Rezultat merenja treba korigovati za sve prepoznate značajne sistematske greške, Slučajna greška merenja - razlika između pojedinačnog rezultata merenja i srednje vrednosti od n pojedinačnih merenja. Ove greške prouzrokuju da rezultati merenja padaju sa obe strane srednje vrednosti i na taj način smanjuju preciznost mernih rezultata. Ova greška se ne može eliminisati ali se može smanjiti porastom broja merenja. Slučajne greške su predmet proučavanja matematičke statistike koja se odnosi na procenu najverovatnije vrednosti merne veličine, Mod - najčešće ponavljana vrednost u skupu podataka, Medijana - broj koji razdvaja gornju polovinu uzoraka, populacije ili raspodela verovatnoće od donje polovine, Referentni materijal (rm) - materijal ili supstanca kod koje su jedna ili više vrednosti svojstava dovoljno homogeni i dobro uspostavljeni da se mogu koristiti za kalibraciju aparata, ocenjivanje metode merenja ili za određivanje vrednosti materijala, Sertifikovani referentni materijal (crm) - referentni materijali koji su propraćeni certifikatom, čije su jedna ili više vrednosti svojstava certificirane procedurom koja uspostavlja sledljivost prema tačnoj realizaciji jedinice u kojoj su vrednosti svojstva izraženi i za koji je svaka certificirana vrednost praćena nesigurnošću kod određenog nivoa poverenja, Limit detekcije (LOD) - predstavlja najmanju koncentraciju ispitivane supstance u uzorkukoja, pod datim eksperimentalnim uslovima, može bit registrovana (detektovana), ali nije potrebno da bude tačno i određena pod datim eksperimentalnim uslovima, Limit kvantifikacije (LOQ) - predstavlja najmanju koncentraciju ispitivane supstance u uzorku koja, pod datim eksperimentalnim uslovima, može bit određena sa prihvatljivom preciznošću i tačnošću, Linearnost - definiše sposobnost metode u dobijanju rezultata odnosno signala koji su proporcionalni koncentracij analita, Tačnost - sposobnost mernog instrumenta i metode da rezultat koji je blizak pravoj odnosno tačnoj vrednosti, Preciznost - blizina niza nezavisnih rezultata merenja koji su dobijeni pod tačno definisanim uslovima, Osetljivost - promena mernog signala pri promeni jedinice sadržaja analita. Ova promena je praktično jednaka nagibu kalibracione krive analita, Selektivnost - sposobnost metode da pod tačno definisanim uslovima ispitivanja odredi tačno i specifično traženi analit u prisustvu drugih komponenata koji čine matriks uzorka, Ponovljivost - sposobnost mernog instrumenta da pri istim uslovima merenja prilikom ponovljene analize da približno iste ispitvane vrednosti, Reproduktivnost - dobijanje rezultata istom metodom pod identičnim eksperimentalnim uslovima u drugim laboratorijama od strane drugih analitčara korišćenjem drugih instrumenata, Robusnost - robusnost jedne analitičke metode je mera njene sposobnosti da se ne menja pod dejstvom male, ali prisutne varijacije parametara metode, čime se potvrđuje i pouzdanost primenjene metode, Preporučen dnevni unos (Recomended daily allowances - RDA) - nivo za koji se smatra da je dovoljan da zadovolji potrebe skoro svih ljudi u grupi sa sličnim karakteristikama, Dnevni unos (Daily intake - DI) - predstavlja onu količinu nutrijenta koja je potrebna da bi se izbegao njihov deficit i obezbedili
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