TY - JOUR
T1 - Multiresidue determination of organochlorines in fish oil by GC-MS
T2 - A new strategy in the sample preparation
AU - Nevado, Juan José Berzas
AU - Martín-Doimeadiós, Rosa Carmen Rodríguez
AU - Bernardo, Francisco Javier Guzmán
AU - Fariñas, Nuria Rodríguez
AU - Cogolludo, José María González
AU - Osma, José Antonio Castro
AU - Castro-Osma, Jose
PY - 2010/5/15
Y1 - 2010/5/15
N2 - A rapid, economic and environmentally friendly analytical methodology has been implemented for the determination of α-, β-, γ- and δ-HCH, p,p′-DDT, p,p′-DDD and p,p′-DDE, PCBs congeners #28, #52, #101, #153, #138 and #180 and Hexachlorobenzene in fish oil. 1,2,3,4-Tetrachloronaphtalene was used as internal standard. The sample preparation, consisting of a single step of clean-up and fractionation, took place in a column filled with different layers of neutral and sulphuric acid modified silica. The analytes were eluted by vacuum with of hexane. Significant reduction in terms of solvents, sorbents, and analysis time was achieved in comparison with literature. Gas chromatography coupled to mass spectrometry was used for the separation and determination of the analytes. The instrumental limits of detection were from 0.1 to 1.3 ng mL-1 and the response of the detector was linear up to 200 ng mL-1. The separation proved to be precise (RSD < 3.7% in peak area) and robust in terms of peak area, peak efficacy and resolution. The methodology was validated with two certified reference materials of cod liver oil, BCR 598 and BCR 349, obtaining no statistically significant differences between the concentrations found and certified. For the analytes that were not certified, aliquots of the reference materials were spiked and the recoveries obtained were satisfactory. These results were consistent with those found previously for DDTs by gas chromatography with an electron-capture detector. The methodology was applied to the analysis of three fish oil pills sold in Spain as a dietary supplement of vitamins and omega-3 fatty acids. The sum of the analytes studied was from 64 to 80 ng g-1. The most abundant compounds are PCBs, followed by DDTs in all samples.
AB - A rapid, economic and environmentally friendly analytical methodology has been implemented for the determination of α-, β-, γ- and δ-HCH, p,p′-DDT, p,p′-DDD and p,p′-DDE, PCBs congeners #28, #52, #101, #153, #138 and #180 and Hexachlorobenzene in fish oil. 1,2,3,4-Tetrachloronaphtalene was used as internal standard. The sample preparation, consisting of a single step of clean-up and fractionation, took place in a column filled with different layers of neutral and sulphuric acid modified silica. The analytes were eluted by vacuum with of hexane. Significant reduction in terms of solvents, sorbents, and analysis time was achieved in comparison with literature. Gas chromatography coupled to mass spectrometry was used for the separation and determination of the analytes. The instrumental limits of detection were from 0.1 to 1.3 ng mL-1 and the response of the detector was linear up to 200 ng mL-1. The separation proved to be precise (RSD < 3.7% in peak area) and robust in terms of peak area, peak efficacy and resolution. The methodology was validated with two certified reference materials of cod liver oil, BCR 598 and BCR 349, obtaining no statistically significant differences between the concentrations found and certified. For the analytes that were not certified, aliquots of the reference materials were spiked and the recoveries obtained were satisfactory. These results were consistent with those found previously for DDTs by gas chromatography with an electron-capture detector. The methodology was applied to the analysis of three fish oil pills sold in Spain as a dietary supplement of vitamins and omega-3 fatty acids. The sum of the analytes studied was from 64 to 80 ng g-1. The most abundant compounds are PCBs, followed by DDTs in all samples.
KW - Environmentally friendly
KW - Fish oil
KW - GC-MS
KW - Organochlorine
KW - Rapid
UR - http://www.scopus.com/inward/record.url?scp=77949309737&partnerID=8YFLogxK
U2 - 10.1016/j.talanta.2010.01.033
DO - 10.1016/j.talanta.2010.01.033
M3 - Article
C2 - 20298869
AN - SCOPUS:77949309737
SN - 0039-9140
VL - 81
SP - 887
EP - 893
JO - Talanta
JF - Talanta
IS - 3
ER -