Naslov
Cadmium and lead in grey wolf liver samples: optimisation of a microwave-assisted digestion method

Autori
Vihnanek Lazarus, Maja ; Sekovanić, Ankica ; Kljaković-Gašpić, Zorana ; Orct, Tatjana ; Jurasović, Jasna ; Kusak, Josip ; Reljić, Slaven ; Huber, Đuro

Izvornik
Arhiv za higijenu rada i toksikologiju (0004-1254) 64 (2013), 3; 395-403

Vrsta, podvrsta i kategorija rada
Radovi u časopisima, članak, znanstveni

Ključne riječi
inductively coupled plasma mass spectrometry; reference material bovine liver; toxic metal

Sažetak
A microwave-assisted digestion method for the determination of cadmium (Cd) and lead (Pb) by inductively coupled plasma mass spectrometry (ICP-MS) was optimised on certified reference material (CRM) (bovine liver, BCR-185R) and wolf liver samples. Different factors influencing digestion efficiency (temperature, time, composition of the digestion mixture, sample mass) were tested. Validation included linearity (up to 200 μg/L for Cd and Pb), detection (0.003 μg/L for Cd and 0.035 μg/L for Pb), and quantification (0.008 μg/L for Cd and 0.081 μg/L for Pb) limits. Good agreement between measured and certified values was achieved in all conditions, with recoveries ranging from 94 % to 111 % for Cd and from 95 % to 105 % for Pb. The precision of the method, expressed as relative standard deviation, was up to 3 % for Cd and 8 % for Pb. The best digestion parameters (260 °C, 30 min, 1 mL HNO3+4 mL H2O, 0.1 g of CRM) based on accuracy and precision were applied on two wolf liver samples to evaluate the need for the predigestion step (freeze-drying) and appropriate mass of the sample. Freeze-drying improved precision and minimising the tissue mass to 0.1 g reduced the matrix effect. Using these optimised digestion conditions, we determined Cd and Pb in 40 wolf livers collected in Croatia, and their medians (0.055 μg/g and 0.107 μg/g, respectively) were in the range of previously reported data for the grey wolf.

Izvorni jezik
Engleski

Znanstvena područja
Kemija, Javno zdravstvo i zdravstvena zaštita, Veterinarska medicina

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