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 0.05 mg kg1), 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 1.29 mg kg1 for BPA, from 0.028 to 1.55 mg kg1 for OP and from 0.026 to 1.47 mg kg1 for NP.
Simultaneous Determination of Bisphenol A, Octylphenol, and Nonylphenol by Pressurized Liquid Extraction and Liquid Chromatography-Tandem Mass Spectrometry in Powdered Milk and Infant Formulas
VITTORI, Sauro;SAGRATINI, Gianni
2011-01-01
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 0.05 mg kg1), 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 1.29 mg kg1 for BPA, from 0.028 to 1.55 mg kg1 for OP and from 0.026 to 1.47 mg kg1 for NP.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
