RRLC-MS/MS同时测定食品接触材料中9种双酚类化合物迁移量

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

  • 摘要: 建立了高分离度快速液相色谱-串联质谱(RRLC-MS/MS)法同时测定食品接触材料中9种双酚类化合物的迁移量。样品经不同类型食品模拟物浸泡后,用Oasis HLB固相萃取柱净化,Agilent poroshell 120 SB-C18柱(2.1 mm×100 mm×2.7 μm)分离,以甲醇和0.1 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,在电喷雾负离子模式(ESI-)和多反应监测(MRM)模式下进行分析。结果表明,在优化的实验条件下,9种双酚类化合物的线性关系良好,相关系数(R2)均大于0.99,检出限为0.01~0.2 μg/kg,定量限为0.05~1.0 μg/kg,在低、中、高3个加标水平下的回收率为76.9%~113.1%,相对标准偏差为1.9%~6.7%。本方法灵敏、准确、可靠、快速,能满足食品接触材料中9种双酚类化合物迁移量的检测需求。

     

    Abstract: 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.

     

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