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建立了超声提取、气相色谱-质谱(GC-MS)分析方法同时测定了果汁饮料包装材料中22种邻苯二甲酸酯类(PAEs)增塑剂的含量。样品经超声提取后,经程序升温、Rtx-5MS毛细柱分离,由选择离子监测(SIM)模式采集并定性、外标曲线法定量。结果表明:标准曲线在0.05~10 mg/L内(DINP和DIDP在0.5~10 mg/L浓度范围)呈现良好的线性关系,相关系数均大于0.996,检测限(LOD)在0.02~1.55 mg/kg之间,定量限(LOQ)在0.08~5.18 mg/kg之间。通过比较正己烷和正己烷/甲基叔丁基醚(1:1)混合液两种提取溶剂的加标回收率,发现正己烷更适合本体系中22种PAEs的同时检测。该方法操作简单、重现性好、灵敏度高,能满足基层检验室对果汁饮料包装材料中PAEs含量检测的实际需求。
The content of 22 kinds of phthalates (PAEs) plasticizers in fruit juice beverage packaging materials was determined by ultrasonic extraction and gas chromatography-mass spectrometry (GC-MS). Samples were extracted by ultrasound, temperature programmed, Rtx-5MS capillary column separation by the selective ion monitoring (SIM) mode acquisition and qualitative, external standard curve method. The results showed that the calibration curve showed a good linearity in the range of 0.05-10 mg / L (DINP and DIDP concentration range of 0.5-10 mg / L), the correlation coefficients were all greater than 0.996, and the limit of detection (LOD) was 0.02-1.55 mg / kg, and the limit of quantification (LOQ) was between 0.08 and 5.18 mg / kg. By comparing the recoveries of two extraction solvents of n-hexane and n-hexane / methyl tert-butyl ether (1: 1), n-hexane was found to be more suitable for the simultaneous detection of 22 PAEs in this system. The method has simple operation, good reproducibility and high sensitivity, and can meet the actual requirements of grassroots inspection laboratories for detecting PAEs content in fruit drink beverage packaging materials.