Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples
Mikroekstrakcija u čvrstoj fazi – uzorkovanje iz gasovite faze: 2. Uzorci jabuka
Pregled/ Otvaranje
Autor
Djurovic, Rada
Milinovic, Jelena
Markovic, Mirjana
Markovic, Dragan
Ključne reči
HS/SPMEPesticide residues
Apple samples
ostaci pesticida
jabuke
Metadata
Prikaz svih podataka o dokumentuApstrakt
Headspace solid phase microextraction method (HS/SPME), optimised previously for
pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion
and bifenthrin in apple samples. One-hour extraction procedure was performed
at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS) fiber was used.
Detection and quantification were carried out by gas chromatography/mass spectrometry
(GC/MS).
A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-
1.25 mg/kg concentration range in order to determine analytical parameters of the method
applied. Linearity with regression coefficient (R) values higher than 0.99 were obtained over
the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence
was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values
for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection
(LOD) values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion
and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD) values obtained for
multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%. Metoda mikroekstrakcije u čvrstoj fazi - uzorkovanje iz gasovite faze (HS/SPME) optimizovana sa mešanim standardnim rastvorima hlorpirifosa, fentiona i bifentrina je testirana
na uzorcima jabuka. Ekstrakcija u trajanju od 60 minuta je izvršena na temperaturi od
60oC sa 2 ml pripremljenog uzorka. Korišćeno je nepolarno 100 μm polidimetilsiloksansko
(PDMS) vlakno. Detekcija i kvantifikacija su izvr.ene metodom gasno-masene spektrometrije
(GC/MS).
U cilju određivanja analitičkih parametara, pravljena je serija obogaćenja referentnog
uzorka jabuka mešanim standardnim rastvorom pesticida tako da finalne koncentracije budu
u rasponu 0.025-1.25 mg/kg. Linearnost (r2 > 0.99) je dobijena za ceo ispitivani koncentracioni
opseg. Prinosi ekstrakcije za sve pesticide i sve koncentracije uključene u ispitivanje
su u rasponu 56.68-82.91%. Granice detekcije metode (LOD) su bile 0.014 mg/kg za hlorpirifos,
0.021 mg/kg za fention i 0.053 mg/kg za bifentrin. Preciznost, odnosno ponovljivost
merenja je određena na uzorku obogaćenom sa 0.6 mg/kg svakog pesticida. Izračunate
RSD vrednosti su uvek bile ispod 20%.