加速溶剂萃取-GC-MS法检测食品接触材料——纸、纸板、木材和木制品中的6种氯酚类物质残留

建立了检测食品接触材料——纸、纸板、木材和木制品中含氯酚(CPs)残留量的气相色谱-质谱(GC-MS)分析方法。采用加速溶剂萃取(ASE)法为样品前处理手段,优化了萃取溶剂、萃取温度、静态萃取时间、冲洗体积和萃取循环次数等实验参数。优化结果为:以二氯甲烷为萃取溶剂,萃取温度为150℃,静态萃取时间为10 min,冲洗体积为(占萃取罐体积的)60%,萃取循环次数为1次。结果表明:6种CPs在0.05～2.0μg/mL质量浓度范围内具有良好的线性关系(R>0.99);平均回收率在86.8%～108.8%之间(n=6);相对标准偏差(RSD)为1.8%～14.2%(n=6);方法的检测限为0.01 mg/kg。研究表明该方法高效、简便、快捷、灵敏、准确可靠,可用于实际样品的CPs残留量的监测。

Determination of 6 Chlorophenols in Paper, Paperboard, Wood and Wood Products Used as Food Contact Materials by Accelerated Solvent Extraction and GC-MS

A new analytical method was developed for the determination of CPs in paper,paperboard,wood and wood products used as food contact materials by accelerated solvent extraction(ASE) and gas chromatography-mass spectrometry(GC-MS).The operational parameters of ASE,such as extraction solvent,extraction temperature,static extraction time,flush volume and extraction cycles,were optimized.The optimized procedure was using dichloromethane as extraction solvent,150 ℃ of extraction temperature,10 min of static extraction time,and 60% flush volume;the extraction recoveries of 6 CPs were nearly to 100% for only one cycle.The results indicated that the developed method has good linearity(R>0.99) in 0.05~2.0 μg/mL mass concentration,good recoveries(86.8%~108.8%) and precision(relative standard deviation(RSD) 1.8%~14.2%);the limited of detection(LOD) of the 6 CPs are 0.01 mg/kg.It was concluded that the developed method is efficient,simple,rapid,sensitive,accurate and reliable,which can be utilized for CPs residual inspection of sample.