@conference{
author = "Tasić, Aleksandra and Pavlović, Ivan and Baltić, Milan Ž.",
year = "2022",
abstract = "Određivanje prisustva polihlorovanih bifenila je značajno jer oni spadaju
u perzistentne organske zagađivače, koju su dobijeni sintetičkim putem.
Ova jedinjenja se koriste za kondenzatore i transformatore, i nakon
toga akomuliraju se u sedimentima, a zbog lipofilnih osobina ove
kancerogene i mutagene supstance dospevaju u tkivu riba. Zbog štetnog
uticaja po ljudsko zdravlje i životnu sredinu monitoringu prisustva
PCB-a u svim vrstama riba se daje na važnosti. Metode pripreme
uzorka su validirane za analizu indikatorskih PCB-a u ribama oslića
korišćenjem gasne hromatografije-masene spektrometrije (GC/MS)
za kvantifikaciju. Analizirani su uzorci dve vrste riba iz porodice
Merlucciidae, i to Merluccius hubbsi i Merluccius senegalenensis. Obzirom
da u matriksu prisutne koektrakcione supstance mogu oštetiti GC
koluni, kao i interferirati tokom detekcije ispitano je poređenje tri tipa
sredstva za prečišćavanje ekstrakta. Disperzni sorbenti koji su korišćeni
su: 1) PR Florisil 500 mg; 2) MgSO4, C18, PSA i dodatno prečišćavanje
eluiranjem na 100 mg C18 ketridžu i 3) dodatno eluiranje na 200 mg
C18. U prvom i drugom slučaju je dobijen zadovoljavajući recovery
od 73.5-86.2%, odnosno 71.3-86.8 %, respektivno. Dok su u trećem
slučaju korišćenjem ketridža 200 mg/3 ml C18 srednji recovery su bili
nezadovoljavajući u opsegu od 45.0-52.3%, ali su hromatogrami bili
bez interefrirajućih supstanci, što je dovelo do zadržavanja i ispitivanih
PCB. Tako da je treći postupak pripreme odbačen za određivanje realnih
uzoraka. Metode su validovane kroz linearnost, preciznost, specifičnost,
tačnost i limit kvantifikacije. Limiti kvantifikacije za indikatore PCB su 3 ng/g računato na vlažnu masu. U svim ispitanim uzorcima vrednosti
PCB-a su bile ispod LOQ. Uredbom Komisije (EU) br. 1259/2011 utvrđen
je maksimalni nivo za zbir šest markera ili indikatorskih PCB-a (PCB 28,
52, 101, 138, 153 i 180) u mišićnom mesu ribe u vrednosti od 75 ng/g
(v.m.). Obe metode pripreme su potvrđene zadovoljavajućim rezultatom
za PCB 153 korišćenjem sertifikovanog referentnog materijala - masne
ribe (Fapas, UK), pri čemu su dobijene vrednosti 24.2 ng/g i 26.4 ng/g,
respektivno, a tačna vrednost je bila 28.0 ng/g sa dozvoljenim opsegom
15.7-40.3 ng/g., Determination of the presence of polychlorinated biphenyls has become
important because they belong to the persistent organic pollutants, which
are obtained synthetically. These compounds are used for capacitors and
transformers, and after that they accumulate in sediments, and due to
lipophilic properties, these carcinogenic and mutagenic substances reach
the fish tissue. Due to the detrimental impact on human health and the
environment, monitoring the presence of PCBs in all fish species is given
importance. Sample preparation methods were validated for the analysis
of the indicator PCBs in the hake fish using gas chromatography-mass
spectrometry (GC/MS) for quantification. The analyzed samples were
from two species of fish from the family Merlucciidae, namely Merluccius
hubbsi and Merluccius senegalenensis. Since the co-extractants present
in the matrix can damage GC columns, as well as interfere during
detection, a comparison of three types of extract cleanup was examined.
Dispersive sorbents used are: 1) PR Florisil 500 mg; 2) MgSO4, C18,
PSA and additional clean-up by elution on a 100 mg C18 cartridge and
3) additional elution at 200 mg C18. In the first and second cases, a
satisfactory recovery of 73.5-86.2% and 71.3-86.8%, respectively, was
obtained. While in the third case using a 200 mg/3 ml C18 cartridge,
the mean recovery was unsatisfactory in the range of 45.0-52.3%, but
the chromatograms were free of interfering substances, which led
to retention and tested PCBs. Thus, the third preparation procedure
was rejected for the determination of real samples. The methods Determination of the presence of polychlorinated biphenyls has become
important because they belong to the persistent organic pollutants, which
are obtained synthetically. These compounds are used for capacitors and
transformers, and after that they accumulate in sediments, and due to
lipophilic properties, these carcinogenic and mutagenic substances reach
the fish tissue. Due to the detrimental impact on human health and the
environment, monitoring the presence of PCBs in all fish species is given
importance. Sample preparation methods were validated for the analysis
of the indicator PCBs in the hake fish using gas chromatography-mass
spectrometry (GC/MS) for quantification. The analyzed samples were
from two species of fish from the family Merlucciidae, namely Merluccius
hubbsi and Merluccius senegalenensis. Since the co-extractants present
in the matrix can damage GC columns, as well as interfere during
detection, a comparison of three types of extract cleanup was examined.
Dispersive sorbents used are: 1) PR Florisil 500 mg; 2) MgSO4, C18,
PSA and additional clean-up by elution on a 100 mg C18 cartridge and
3) additional elution at 200 mg C18. In the first and second cases, a
satisfactory recovery of 73.5-86.2% and 71.3-86.8%, respectively, was
obtained. While in the third case using a 200 mg/3 ml C18 cartridge,
the mean recovery was unsatisfactory in the range of 45.0-52.3%, but
the chromatograms were free of interfering substances, which led
to retention and tested PCBs. Thus, the third preparation procedure
was rejected for the determination of real samples. The methods were validated through linearity, precision, specificity, trueness and
quantification limit. The quantification limits for PCB indicators were
3 ng/g wet weight. In all tested samples, PCB values were below LOQ.
Commission Regulation (EU) No 1259/2011 established a Maximum
level for sum of the six marker or indicator PCBs (PCB 28, 52, 101,
138, 153 and 180) in muscle meat of fish at a value of 75 ng/g (w. w).
Both preparation methods were confirmed by satisfactory results for
PCB 153 using certified reference material - fatty fish (Fapas, UK), with
values of 24.2 ng/g and 26.4 ng/g, respectively, and the assigned value
was 28.0 ng/g with a permissible range of 15.7-40.3 ng/g.",
publisher = "Banja Luka : Veterinarska komora Republike Srpske",
journal = "27. godišnje savjetovanje doktora veterinarske medicine Republike Srpske (Bosna i Hercegovina), Trebinje, 15-18. jun 2022",
title = "Poređenje različitih sorbenata u prečišćavanju ekstrakata za validaciju i analizu polihlorovanih bifenila u osliću, Comparison of different sorbents in clean-up extracts for validation and analysis of polychlorinated biphenyls in hake",
pages = "251-254",
url = "https://hdl.handle.net/21.15107/rcub_veterinar_2854"
}
