啤酒中邻苯二甲酸酯检测方法优化及迁移量研究

该试验建立了顶空固相微萃取-气质联用法（HS-SPME-GC/MS）分析啤酒中塑化剂邻苯二甲酸酯（PAEs）的测定方法，采用单点标准加入法测定了6种市售啤酒以及在3种迁移试验条件下瓶盖内垫片在啤酒和模拟物（体积分数为10%乙醇溶液）中PAEs的迁移量。啤酒样品采用50 μm聚二乙烯基苯/碳分子筛/聚二甲基硅氧（DVB/CAR/PDMS）萃取头萃取，在55 ℃水浴保温60 min，该方法共定量了16种PAEs的组分。结果表明，通过对啤酒PAEs的检测，发现使用PVC内垫片和PE内垫片的啤酒中DBP的迁移量均为最高，分别为9.48 μg/L与8.26 μg/L，而DIBP、DEHP则迁移量较低，但DEHP在体积分数为10%的乙醇溶液中含量较高。通过试验可知温度及时间是啤酒中PAEs增加的一个重要因素，应严格禁止将啤酒横放、倒放或高温储存，避免酒液接触内垫片。

Optimization of detection method and migration amount for phthalate acid esters in beer

A determination method for analyzing the plasticizer phthalate acid esters (PAEs) in beer by headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC/MS) was established in this tests. The migration amount of PAEs in 6 kinds of beer commercially available and inner gasket of bottle cap in beer and simulants (ethanol solution volume fraction 10%) under 3 migration test conditions were determined by single point standard addition method. The beer samples were extracted by 50 μm polydivinylbenzene/carbon molecular sieve/polydimethylsiloxane (DVB/CAR/PDMS) extraction head and incubated in 55 ℃ water bath for 60 min. 16 PAEs components were quantified by this method. The results showed that the migration amount of DBP in beers with PVC and PE inner gaskets was highest by determining PAEs of beer, which was 9.48 μg/L and 8.26 μg/L, respectively, while the migration amount of DIBP and DEHP was lower. However, the contents of DEHP in ethanol solutions of 10% volume fraction was higher. It could be known by experiment that temperature and time were important factors in the increase of PAEs in beer. It should be strictly forbidden to store beer horizontally, upside down or at high temperature to prevent beer from contacting the inner gasket.