A packaging contaminant: isopropylthioxanthone (ITX) in dairy products

A fast, simple and very selective liquid chromatography-mass spectrometry (LC-MS) method for the detection of isopropylthioxanthone (ITX) in dairy products has been developed and validated. After addition of an ITX-d(3) as internal standard and a simple extraction from the sample with acetonitrile, the extract was centrifuged and directly injected into the LC-MS system. Chromatographic separation was achieved by means of a Gemini C18 column (100 mm x 2.0 mm i.d. 5 microm) using a gradient of aqueous 20 mM ammonium formiate at pH 4.5 and methanol as the mobile phase, at a flow rate of 0.25 mL min(-1). The method was validated according to the guidelines laid down by the Commission Decision 2002/657/EC using the parent ion [M+H](+) (m/z 255) as quantification ion, and the fragment ion (m/z 213) obtained by in-source collision-induced dissociation (IS-CID) as confirmation ion. Absolute and relative recoveries rates were verified at 5, 10, 15 microg kg(-1) in yoghurt samples and at 5 microg kg(-1) in milk and pudding: mean absolute recoveries were 77% in yoghurt, 50% in pudding and 67% in milk; relative recoveries (after internal standard correction) were always >97% in each matrix. The detection limit (CCalpha) and the detection capability (CCbeta) of method were 6.2 and 7.2 microg kg(-1), respectively.