Detection of migration of phthalates from agglomerated cork stoppers using HPLC‐MS/MS

Journal of Separation Science - Tập 35 Số 10-11 - Trang 1319-1326 - 2012
Raquel Sendón1, A. Sanches‐Silva2, Juana Bustos3, Patricia Martín4, Nuria García-Martínez4, Ma Eugenia Cirugeda3
1Department of Analytical Chemistry, Nutrition and Food Science, University of Santiago de Compostela, Spain
2Department of Food and Nutrition, National Institute of Health Dr. Ricardo Jorge, Lisboa, Portugal
3National Food Center, Spanish Food Safety and Nutrition Agency, Spain
4Sanidad Animal Y Servicios Ganaderos, Tragsega, Spain

Tóm tắt

Agglomerated stoppers are manufactured from natural cork granules and adhesives. Esters, such as phthalates and adipates, are commonly used in adhesives at concentrations of typically 2–5%. Because of this, and regarding consumer safety, it is necessary to ensure that these compounds do not migrate into the beverage where the cork stopper is used. A reversed‐phase high performance liquid chromatography method with tandem mass spectrometry detection is developed for the separation of nine phthalates into 12% ethanol, used as simulant of alcoholic beverages. The chromatographic separation was carried out with a Luna C18 (2) HSTcolumn (50 × 3.0 mm, 2.5 μm) with a gradient elution of water/methanol with 0.1% acetic acid at 300 μL min−1. The method was validated for four selected phthalates: di‐butylphthalate, di‐isononylphthalate, di‐isodecylphthalate, and butyl‐benzyl phthalate, with recoveries ranging between 95% and 112% and intralaboratory precision (RSD) between 5 and 14%, depending on the phthalate. The lowest quantification limit, 0.15 mg kg−1, was achieved for di‐butylphthalate. Nevertheless, in all cases, the limits obtained guarantee the method utility if restriction limits set in Commission Regulation No 10/2011 for plastic materials are taken into account.

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Thông tin xuất bản

Journal of Separation Science

Tập 35 Số 10-11

1319-1326

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