Baby food safety is an essential issue in health policy. For this reason, a simple, cheap, and fast analytical procedure to developed arsenic(III) and total arsenic determination in baby food samples using functionalized magnetic graphane oxide nanocomposite. A new nanocomposite anchored of tiopronin (TSH) magnetic graphane oxide (GO-PG4@Fe 3 O 4 -TSH) was first synthesized/characterized and used as an adsorbent to determine arsenic(III) and total arsenic for baby food samples. Arsenic(III) was directly determined on GO-PG4@Fe 3 O 4 -TSH nanocomposite at pH 4.5. The determination of total arsenic used KI and L( +) ascorbic acid solution as reducing reagents. The parameters influential on arsenic(III) determination in the baby food samples including the sample's pH, adsorption time, amount of GO-PG4@Fe 3 O 4 -TSH, eluent type, sample volume, reducing reagent type and amount, and also foreign ion effect were investigated. The GO-PG4@Fe 3 O 4 -TSH carrying As(III) could easily be separated from baby food samples via applying an external magnetic field. The detection limit for arsenic(III) was found as 0.11 μg L −1 , while the limit of quantification values was computed as 0.37 μg L −1 . The precision of results, expressed as relative standard deviation, was always lower than 1.6% at 1 mg L −1 As(III) levels. The accuracy of this method was confirmed by analysis of certified reference material. The method was successively applied to determine arsenic(III) and total arsenic in baby food samples.