[关键词]
[摘要]
该文建立了同时测定自热食品接触用塑料制品所用着色剂中的14种多氯联苯的气相色谱-串联质谱法。样品中的多氯联苯经有机溶剂超声提取,用浓硫酸磺化,气相色谱-串联质谱法分析,外标法定量。结果表明,14种多氯联苯在质量浓度为0.5~5 µg/L的范围内均线性良好,相关系数(R2)均大于0.99。14种多氯联苯的检出限均为5 μg/kg,定量限均为25 μg/kg。当添加量为5、10、 25 µg/kg时,14种多氯联苯在荧光红中的回收率为81.03%~105.72%之间,相对标准偏差(RSD)在1.51~10.52之间;在荧光黄中的回收率为80.11%~108.44%之间,RSD在0.69~11.10之间;在荧光蓝中的回收率为81.07%~102.56%之间,RSD在0.72~10.80之间;在荧光绿中的回收率为80.26%~109.37%之间,RSD在1.12~11.41之间;在荧光紫中的回收率为80.15%~105.80%之间,RSD在1.21~10.89之间。该方法快速准确,能够为自热食品接触材料着色剂安全性评价作技术参考。
[Key word]
[Abstract]
A gas chromatography-mass spectrometry (GC-MS) method was developed for simultaneous determination of 14 polychlorinated biphenyls (PCBs) in colorants for plastics used in self-heating food for food contact products. The PCBs in the sample were extracted by ultrasound-assisted extraction with organic solvent, sulfonated with concentrated sulphuric acid, determined by GC-MS, and quantified with external standards. The results showed that 14 PCBs exhibited good linear relationships in the concentration range of 0.5~5 µg/L, with the correlation coefficients (R2) all higher than 0.99, the limits of detection (LODs) all being 0.1 mg/kg, and the limits of quantification (LOQs) all being 0.25 mg/kg. When the spiking concentration was 5 µg/kg, 10 µg/kg or 25 µg/kg,the recoveries of 14 PCBs in fluorescent red ranged from 81.03% to 105.72%, with the relative standard deviations (RSDs) ranging from 1.51 to 10.52; the recoveries of 14 PCBs in fluorescent yellow ranged from 80.11% to 108.44%, with the RSDs ranging from 0.69 to 11.10;the recoveries of 14 PCBs in fluorescent blue ranged from 81.07% to 102.56%, with the RSDs ranging from 0.72 to 10.80;the recoveries of 14 PCBs in fluorescent green ranged from 80.26% to 109.37%, with the RSDs ranging from 1.12 to 11.41;the recoveries of 14 PCBs in fluorescent violet ranged from 80.15% to 105.80%, with the RSDs ranging from 1.21 to 10.89. This method is rapid and accurate, and can be used as a technical reference for safety evaluation of colorants used in self-heating food contact materials.
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[基金项目]
山西省重点研发计划项目(201803D31223)