Simultaneous determination of bisphenol A, octylphenol, and nonylphenol by pressurised liquid extraction and liquid chromatography–tandem mass spectrometry in powdered milk and infant formulas

Abstract

A new analytical method, using pressurised liquid extraction (PLE) and liquid chromatography–tandem mass spectrometry (LC–MS/MS), was developed for the simultaneous determination of bisphenol A (BPA), octylphenol (OP) and nonylphenol (NP) in powdered infant formulas (IF) and powdered skimmed milk (PM). The analytes were extracted by PLE, using this optimised conditions: ethyl acetate as solvent, 70°C of temperature, reversed-phase silica C18 as dispersing agent and three cycles of extraction. The extracts were then injected in LC–MS/MS using a Gemini C18 column and a mixture of 5% water and 95% methanol/acetonitrile, both with 0.1% ammonia, as a mobile phase. Recoveries at different fortification levels (0.5 and 0.05mgkg−1), were between 89% and 92% for BPA, 84 and 98% for OP, and 93% and 101% for NP. The method was applied to the analysis of samples of PM and IF, bought in Italian and Spanish markets. In positive samples, phenols concentration ranged from 0.07 to 1.29mgkg−1 for BPA, from 0.028 to 1.55mgkg−1 for OP and from 0.026 to 1.47mgkg−1 for NP.