In the present study, a sensitive, efficient and repeatable method for the simultaneous extraction and determination of 13 types of phthalic acid esters (PAEs) in flavoring essence samples using magnetic graphene solid-phase extraction coupled with gas chromatography tandem mass spectrometry was developed. Due to the unique structure of magnetic graphene, it has several advantages, such as large surface area and fast separation ability. This unique structure not only provided strong magnetic responsiveness for the separation but also prevented the self-aggregation of graphene. The large delocalized p-electron system of graphene can form strong π-stacking interactions with the benzene ring. Thus, graphene may be also a good candidate adsorbent for the adsorption of benzenoid-form compounds. Several magnetic soild-phase extraction parameters, such as elution solvents, amounts of sorbents, enrichment time and desorption time were optimized. The optimized procedures for this method were performed by ultrasonication using ethyl acetate as elution solvent for 5 min. Under the optimal conditions, the developed method provided spiked recoveries of 75.0–105.3% with relative standard deviations of ~5.6% and limits of detection were 0.011–0.091 mg/kg. Good linear relationships were observed with the coefficient of determination (R2) > 0.993 for all the analytes. Finally, the validated method was successfully applied to the analysis of PAEs in real samples.

中文翻译：

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磁性石墨烯分散固相萃取，通过气相色谱串联质谱法测定风味香精中的邻苯二甲酸酯。

在本研究中，开发了一种灵敏，高效且可重复的方法，该方法同时使用磁性石墨烯固相萃取与气相色谱串联质谱法同时萃取和测定调味香精样品中的13种邻苯二甲酸酯（PAE）。由于磁性石墨烯的独特结构，它具有许多优点，例如大表面积和快速分离能力。这种独特的结构不仅为分离提供了强大的磁响应性，而且还阻止了石墨烯的自聚集。石墨烯的较大的离域p电子体系可以与苯环形成强烈的π堆积相互作用。因此，石墨烯也可能是吸附类苯环化合物的良好候选吸附剂。几个磁污相提取参数，例如洗脱溶剂，吸附剂的量，富集时间和解吸时间都得到了优化。通过使用乙酸乙酯作为洗脱溶剂的超声处理5分钟，对本方法进行了优化。在最佳条件下，开发的方法的加标回收率为75.0–105.3％，相对标准偏差为〜5.6％，检出限为0.011-0.091 mg / kg。对于所有分析物，观察到良好的线性关系，测定系数（R2）> 0.993。最后，将验证方法成功地应用于实际样品中PAE的分析。在最佳条件下，开发的方法的加标回收率为75.0–105.3％，相对标准偏差为〜5.6％，检出限为0.011-0.091 mg / kg。对于所有分析物，观察到良好的线性关系，测定系数（R2）> 0.993。最后，将验证方法成功地应用于实际样品中PAE的分析。在最佳条件下，开发的方法的加标回收率为75.0–105.3％，相对标准偏差为〜5.6％，检出限为0.011-0.091 mg / kg。对于所有分析物，观察到良好的线性关系，测定系数（R2）> 0.993。最后，将验证方法成功地应用于实际样品中PAE的分析。