Simultaneous Determination of the Migration of 9 Bisphenols in Food Contact Material by RRLC-MS/MS

A method of rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS) was developed for the simultaneous determination of the migration of 9 bisphenols (bisphenol A, bisphenol F, bisphenol S, bisphenol B, bisphenol E, tetrabromobisphenol A, hexafluorobisphenol A, bisphenol AP, bisphenol BP) in food contact materials. Different types of food simulants (4% acetic acid，50% ethanol，isooctane) were used for migration test to simulate different types of food, such as acidic foods, alcoholic foods and oils. After the migration test, 10 mL of 4% acetic acid soaking solution were directly put in to solid phase extraction cartridge which had been pretreated, while 10 mL of 50% ethanol or isooctane soaking solution were dried by nitrogen in the water bath of 45 ℃, re-dissolved in 2 mL methanol, and fixed to 10 mL by water before purification. An Oasis HLB solid phase extraction cartridge (200 mg/6 mL) was applied for purification. The separation was performed on an Agilent poroshell 120 SB-C18 column （2.1 mm×100 mm×2.7 μm） by using methanol and 0.1 mmol/L ammonium acetate as mobile phases with gradient elution. The electrospray ionization source in negative ion (ESI^-) mode was used for the determination of the 9 bisphenols under the multiple reaction monitoring (MRM) mode. The results verified that, under the optimized experimental conditions, satisfactory linearities of the 9 bisphenols were obtained with correlation coefficients (R²) higher than 0.99. The limits of detection (LOD) and quantitation(LOQ) of the 9 bisphenols were in the range of 0.01-0.2 μg/kg and 0.05-1.0 μg/kg, respectively. The average recoveries of 9 bisphenols ranged from 76.9% to 113.1% at three spiking levels, and the relative standard deviations (RSDs) were between 1.9% and 6.7%. The method is sensitive, accurate, reliable and rapid, and can fully meet the requirements for the simultaneous determination of migration of the 9 bisphenols in food contact materials and products. 60 samples of different types of food contact materials and products, including polycarbonate buckets, baby bottles, cups, food cans and food metal covers, were analyzed by the method. The results showed that bisphenol A and bisphenol F were found in food simulant soaking solution of 4 and 1 food metal covers, respectively. The test results indicate that bisphenols may be present in certain food contact materials and products, and also can be transferred to food in the process of product use.