微波辅助萃取-气相色谱/串联质谱法同时测定纸质食品接触材料中18种多环芳烃

Simultaneous Determination of 18 Kinds of Polycyclic Aromatic Hydrocarbons in Paper Packaging Materials Intended to Come into Contact with Foodstuffs using Gas Chromatography-Tandem Mass Spectrometry Combined with Microwave Assisted Extraction

以正己烷／二氯甲烷（1：1）为溶剂，在90℃下微波辅助萃取纸质食品接触材料中的多环芳烃（PAHs），萃取液经处理后先用二甲亚砜进行萃取，再用环己烷进行反萃取，用硅胶固相萃取柱进行净化后，进行气相色谱／串联质谱分析，外标法定量，从而建立了一种同时测定纸质食品接触材料中18种禁用PAHs的气相色谱／串联质谱方法。在S／N=10的条件下，各目标化合物的定量下限为0．1～1．Oμg／kg，线性相关系数均不小于0．998，加标平均回收率为57．73％～96．87％，相对标准偏差均小于10％。该方法简便快捷、定性定量准确，灵敏度高，可完全满足多环芳烃检测的技术要求，可用于纸质食品接触材料中PAHs的检测。采用建立的方法对市售纸质食品接触材料进行测试，结果在一个黄色包装纸袋中检出多种PAHs。

An effective method was established to determine simultaneously the contents of 18 kinds of banned polycyclic aromatic hydrocarbons （PAHs） in paper packaging materials intended to come into contact with foodstuffs.PAHs in paper packaging materials intended to come into contact with foodstuffs were microwave assisted extracted at 90~C using hexaue/dichloromethane （ 1 ： 1 ） as the extraction solvent. The extract was first extracted by dimethyl sulfoxide, then reverse - extracted by cyclohexanc, followed by purification of silica solid phase extraction column. The extract was at last analyzed by gas chromatography - tandem mass spectrometry and the concentration of each analytes was calibrated by external standard method. The limits of quantitation varied from 0. i μg/kg to 1.0txg/kg at the condition of signal/noise （S/N） of 10 while the correlation coefficients were all lager than 0. 998. The spiked average recoveries changed from 57.73% to 96.87% while the relative standard deviation （RSD） all less than 10%. The proposed method was simple, rapid, sensitive and accurate, which could satisfy completely the demand of the analysis of PAHs in paper packaging materials intended to come into contact with foodstuffs. The developed method was applied to the determination of the content of PAHs in commercially available paper packaging materials intended to come into contact with foodstuffs and PAHs of high contents were detected in a yellow paper packaging material