title: Extraction and Liquid Chromatography-Tandem Mass Spectrometry Detection of 3-Monochloropropanediol Esters and Glycidyl Esters in Infant Formula.
abstract: A method was developed for the extraction of fatty acid esters of 3-chloro-1,2-propanediol (3-MCPD) and glycidol from infant formula, followed by quantitative analysis of the extracts using liquid chromatography-tandem mass spectrometry (LC-MS/MS). These process-induced chemical contaminants are found in refined vegetable oils, and studies have shown that they are potentially carcinogenic and/or genotoxic, making their presence in edible oils (and processed foods containing these oils) a potential health risk. The extraction procedure involves a liquid-liquid extraction, where powdered infant formula is dissolved in water and extracted with ethyl acetate. Following shaking, centrifugation, and drying of the organic phase, the resulting fat extract is cleaned-up using solid-phase extraction and analyzed by LC-MS/MS. Method performance was confirmed by verifying the percent recovery of each 3-MCPD and glycidyl ester in a homemade powdered infant formula reference material. Average ester recoveries in the reference material ranged from 84.9 to 109.0% (0.6-9.5% RSD). The method was also validated by fortifying three varieties of commercial infant formulas with a 3-MCPD and glycidyl ester solution. Average recoveries of the esters across all concentrations and varieties of infant formula ranged from 88.7 to 107.5% (1.0-9.5% RSD). Based on the validation results, this method is suitable for producing 3-MCPD and glycidyl ester occurrence data in all commercially available varieties of infant formula.
authors.affiliation: Center for Food Safety and Applied Nutrition, United States Food and Drug Administration , 5001 Campus Drive, College Park, Maryland 20740, United States.
authors.forename: Jessica K
authors.initials: JK
authors.lastname: Leigh
authors.affiliation: Center for Food Safety and Applied Nutrition, United States Food and Drug Administration , 5001 Campus Drive, College Park, Maryland 20740, United States.
authors.forename: Shaun
authors.initials: S
authors.lastname: MacMahon
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004852:Epoxy Compounds / Q000032:analysis* / Q000302:isolation & purification*; D005506:Food Contamination / Q000032:analysis*; D041943:Infant Formula / Q000032:analysis*; D059625:Liquid-Liquid Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D000517:alpha-Chlorohydrin / Q000032:analysis* / Q000302:isolation & purification*
chemical_list: D004852:Epoxy Compounds; C020344:glycidyl ethers; D000517:alpha-Chlorohydrin
keywords: 3-MCPD; 3-MCPD esters; 3-monochloropropanediol; fat extraction; glycidol; glycidyl esters; infant formula; processing contaminants