单滴微萃取——气相色谱—质谱联用法检测食品中5种邻苯二甲酸酯类塑化剂

Determination of 5 kinds of phthalate acid esters in food by single drop microextraction combined with gas chromatography-mass spectrometry

建立酱油、醋和果汁样品中5种邻苯二甲酸酯类(PAEs)塑化剂的单滴微萃取结合气相色谱—质谱联用检测方法。采用气相色谱—质谱仪进行测定。结果表明:5种邻苯二甲酸酯类塑化剂在1~10mg/mL范围内线性关系良好(r≥0.995);5种PAEs在3种样品基质中3个添加水平的平均回收率在75.4%~113.0%,日内精密度和日间精密度分别为2.4%~7.3%和1.9%~8.5%。5种PAEs中DBP检出率最大为100%,且检出量均超出GB 9685—2008规定的限值0.3 mg/kg。塑料袋、塑料瓶和纸盒包装样品中PAEs的量高于玻璃瓶包装的样品。该方法操作简单,快速,灵敏度高,可以满足酱油、醋和果汁等类样品中PAEs的检测要求。

To develop a rapid and simple method for the determination of five phthalate acid esters（PAEs）in soy sauce,vinegar,and juice by gas chromatography-mass spectrometry（GCMS）after single drop microextration.The five PAEs was analyzed by GC-MS.Good linearity was obtained for five PAEs at the concentration of 1~10mg/mL,r≥0.995.At three different spiked concentration levels,the average recoveries of 5PAEs in three different samples were between 75.4% and 113.0%.The intra-day and interday precisions（relative standard deviation,RSD）were 2.4%~7.3%and 1.9%~8.5%,respectively.Among 5PAEs,the detection rate of DBP was 100% utmost.The DBP of all the samples was more than the limited standard of 0.3 mg/kg,according to the national standards of GB 9685-2008.5PAEs in samples packed in plastic bags,plastic bottles and packaging cartons were more than those in samples packed in glass bottles.The method,which is simple,rapid,and high sensitive,is suitable for the determination of 5PAEs in soy sauce,vinegar,and juice.