目的 建立食品接触用复合膜袋中10种全氟和多氟烷基化合物的测定方法,研究食品接触用复合膜袋中相关成分的安全风险和法规符合性。方法 以乙酸乙酯为提取溶剂,采用超声辅助提取待测物,在酸催化条件下用乙酸酐将其中的醇类物质转化为对应的乙酸酯,采用气相色谱-串联质谱（GC-MS/MS）法检测目标物。通过考察催化剂种类、衍生反应温度和反应时间对回收率的影响,最终确定以硫酸为催化剂,在60 ℃条件下用乙酸酐衍生化处理60 min。目标物经DB-5MS（30 m×0.25 mm×0.25μm）毛细管柱分离,采用程序升温法和GC-MS/MS多反应监测（MRM）模式检测,并以内标法定量。结果 实验结果表明,10种PFASs在10~200 μg/L浓度范围内线性关系良好,相关系数r≥0.997;方法检出限（LOD）为0.001~0.003 mg/kg,定量限（LOQ）为0.003~0.01 mg/kg;在食品接触用复合膜袋基质中,3个添加水平（高、中、低）下的平均回收率为85.8%~108.4%,相对标准偏差（RSD,n=6）为1.6%~7.6%。结论 本方法具有定性定量准确、灵敏度高、选择性好和重现性优等特点,适用于食品接触用复合膜袋中10种PFASs的同步检测。
Abstract
The work aims to establish a method for the determination of 10 PFASs in food contact composite films and bags and investigate the safety risks and regulatory compliance of these substances in such materials. With ethyl acetate as the extraction solvent, ultrasound-assisted extraction was employed to extract the substances of interest. Under acid catalysis, the alcohols were converted to their corresponding acetates with acetic anhydride. The target substances were detected with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). By examining the effects of catalyst type, derivatization reaction temperature, and reaction time on recovery rates, it was determined that sulfuric acid was the best catalyst, with derivatization by acetic anhydride at 60 °C for 60 minutes. The target substances were separated by a DB-5MS (30 m×0.25 mm×0.25 μm) capillary column with a temperature gradient method and GC-MS/MS multiple reaction monitoring (MRM) mode. Quantification was performed with the internal standard method. Experimental results showed that the 10 PFASs had good linearity in the concentration range of 10-200 μg/L, with correlation coefficients r≥0.997. The LODs ranged from 0.001 to 0.003 mg/kg, and the LOQs ranged from 0.003 to 0.01 mg/kg. In the matrix of composite food contact films and bags, the average recoveries at three spiked levels (high, medium, and low) ranged from 85.8% to 108.4%, with relative standard deviations (RSD, n=6) of 1.6% to 7.6%. This method is characterized by accurate qualitative and quantitative results, high sensitivity, good selectivity, and excellent reproducibility, making it suitable for the simultaneous detection of 10 PFASs in composite food contact films and bags.
关键词
气相色谱-串联质谱法（GC-MS/MS） /
全氟和多氟化合物 /
食品接触用复合膜袋
Key words
gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) /
PFASs /
food contact composite films and bags
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基金
广州市科技计划项目（2023B04J0407）; 广州市院士专家工作站（2024-D012）; 广州市市场监督管理局科技计划项目（2025KJ04）
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