University of Nova Gorica (PNG)
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Določanje neonikotinoidov v medu in cvetnem prahu s HPLC-DAD in TLS detekcijo : diplomsko deloMejač, IrenaRazvili smo kromatografsko metodo HPLC za določevanje nekaterih neonikotinoidov (imidakloprid, tiametoksam, acetamiprid in tiakloprid) v vzorcih medu in cvetnega prahu. Neonikotinoide smo iz vzorcev ... medu ekstrahirali z ekstrakcijo tekoče-tekoče v diklorometan, iz cvetnega prahu pa z ekstrakcijo trdno-tekoče v diklorometan:aceton. Z dodatkom standardnih raztopin neonikotinoidov vzorcem medu in cvetnega prahu pred ekstrakcijo smo pripravili umeritvene premice z visokimi regresijskimi koeficienti (> 0,994) v koncentracijskem območju 0,1-5 mg/kg. Vzorce smo analizirali na reverzno-fazni kromatografski koloni C[sub]18 ob uporabi izokratične metode elucije z acetonitrilom:10mM amonijevim acetatom (3:7, v/v) in pretoka 1 mL/min. Za detekcijo neonikotinoidov po kromatografski ločbi smo uporabili spektrofotometrično metodo z diodno matriko DAD in spektrometrijo s toplotnimi lečami TLS. Zaradi različnih absorbcijskih spektrov posameznih neonikotinoidov smo v primeru DAD določevali insekticide pri štirih valovnih dolžinah (254, 270, 245 in 242 nm), v primeru TLS pa smo lahko uporabili le valovno dolžino vzbujevalnega laserja 244 nm. Doseženi izkoristki ekstrakcij iz medu so bili med 76 in 83 % za acetamiprid, tiakloprid in tiametoksam ter 99 % za imidakloprid. Relativni standardni odmiki pri koncentraciji 1 mg/kg in petih ponovitvah so bili v območju 15-38 %. Meje zaznavnosti so bile 50 [mi]g/kg za imidakloprid, 100 [mi]g/kg za tiametoksam in acetamiprid ter 250 [mi]g/kg za tiakloprid. Izkoristki ekstrakcij iz cvetnega prahu so bili občutno nižji, v območju 45-54 %, in so omogočali doseganje meje zaznavnosti 500 [mi]g/kg za vse štiri insekticide. Z metodo HPLC-TLS smo za primer standardnih raztopin neonikotinoidov dosegli meje zaznavnosti v območju 10 [mi]g/kg za acetamiprid do 25 [mi]g/kg za tiametoksam in imidakloprid in s tem znižanje vrednosti LOD v primerjavi s HPLC-DAD metodo.Type of material - undergraduate thesisPublication and manufacture - Nova Gorica : [I. Mejač], 2006Language - slovenianCOBISS.SI-ID - 536315
Author
Mejač, Irena
Other authors
Franko, Mladen
Topics
diplomske naloge |
ekstrakcija |
med |
cvetni prah |
kromatografija |
kromatografija

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