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The oils were partitioned into heptane and aqueous methanol (MeOH 1 phase, Fig. 1). The heptane phases of selected oils were further partitioned into methanol (MeOH2 phase) andheptane, to increase the extraction recovery for arsenic into methanol. The heptane phases were partitioned into acetonitrile (ACN) and heptane, to further increase the extraction recovery of arsenic into apolar solvent. Acetonitrile was selected as third solvent as it is more non-polar compared to methanol and has a different selectivity than methanol [34]. MeOH1, MeOH2 and ACN phases were analyzed for total arsenic. The MeOH1 phase of all fish oils were analyzed by reversed-phaseHPLC¨CICP-MS, and the arseno- lipids were quantified using DMA and Ph3AsO. The arsenolipids in the MeOH1 phase of selected fish oils were also quantified using a synthesized AsHC compound (dimethylarsinoylnonadecane; AsHC¨CC19). The MeOH1 phases of selected fish oils were analyzed by HPLC coupled to quadrupole Time-of-Flight Mass Spectrometry (qTOF-MS) for identification of the molecular structures and determination of accurate masses of the arsenolipids present. All MeOH 2 and ACN phases of selected fish oils were analyzed by reversed-phase HPLC¨CICP-MS.

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