Razvoj i primena metode tečne hromatografije - tandem masene spektrometrije za određivanje pesticida u voću i voćnim sokovima
Development and application of liquid chromatography-tandem mass spectroskopy method for pesticide analysis in fruits and fruit juices
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Predmet ovog rada je razvoj i primena nove, brze i osetljive multirezidualne analitičke
metode za određivanje tragova pesticida različitih hemijskih grupa u voćnim sokovima i
voću. Za analizu su odabrani pesticidi koji spadaju u najčešće korišćene u našoj zemlji.
Rad obuhvata razvoj metode disperzije matrice na čvrstoj fazi, za efikasnu ekstrakciju i
predkoncentrisanje veoma različitih analita. Metoda obuhvata istovremeno razaranje,
usitnjavanje i homogenizaciju čvstih i polučvstih uzoraka, kao i ekstrakciju i
prečišćavanje analita. Kao sorbent korišćena je dijatomejska zemlja a dihlormetan je
korišćen za eluiranje analita. Takođe, urađena je optimizacija hromatografskog
razdvajanja i uspostavljen je protokol za potvrdu prisustva analita pomoću masenog
detektora sa jonskim trapom. Kvantifikacija analita je urađena posmatranjem
najintenzivnijeg fragmenta. Razvijena metoda za određivanje pesticida u voćnim
sokovima obuhvata dvanaest pesticida i uspešno je validirana na uzorcima soka od
j...abuke, narandže, breskve i maline. Metoda je proširena sa još pet pesticida i uspešno
validirana na uzorcima voća, jabuke, kajsije, narandže i jagode. Kao parametri
validacije određivani su: prinos, linearnost, granica detekcija i granica kvantifikacije za
sve ispitivane pesticide u svim ispitivanim matricama. Vrednosti dobijene za prinose u
većini slučajeva su bile u opsegu od 70 do 120% uz relativnu standardnu devijaciju
uglavnom ispod 20%. Dostignute su veoma niske granice detekcije i kvantifikacije.
Razvijena metoda je primenjena na realne uzorke komercijalno dostupnih sokova i voća
dostupnih na beogradskom tržištu
This study presents the development and application of a new, rapid and sensitive
analytical method for determination of pesticide residues in fruit juices and fruits.
Pesticides, chosen for the analysis, belong to different chemical classes and are among
the most frequently used in our country. The study includes the development of the
matrix solid-phase dispersion sample preparation method for extracting and preconcentrating
different analytes. This sample preparation technique involves
simultaneous disruption, fragmentation and homogenization of solid and semi-solid
samples as well as extraction and clean-up of the analytes. Diathomeus earth was used
as a dispersant, while dichloromethane was used as an eluting solvent. Also,
optimization of the chromatographic separation was done and the protocol for reliable
confirmation of pesticide residues with ion trap mass detector was established. The
quantification of the analytes was carried out using the most sensitive transition.
Develop...ed method for pesticide analysis in fruit juices includes twelve pesticides and
was successfully validated in apple, orange, peach and raspberry fruit juices. The
method was expanded with five more pesticides and it was successfully validated for
fruit samples, apple, apricot, orange and strawberry. The method was validated for
accuracy, linearity, reproducibility, and sensitivity. Mean values for recoveries were in
the range of 70–120 % for all tested matrices. Repeatability of the method, expressed as
the relative standard deviation, was in general, lower than 20 %. Low limits of detection
and quantification were readily achieved with this method for all tested pesticides. The
applicability of the method to routine analysis was tested in real fruit and fruit juices
samples with good performance.