College of Food Science and Biotechnology, Zhejiang Gongshang University, Hangzhou 310035, China.
Food Chem. 2013 Nov 15;141(2):1383-9. doi: 10.1016/j.foodchem.2013.04.090. Epub 2013 May 9.
An ultra-fast analytical protocol using graphene-based solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry for the rapid determination of malachite green and its metabolite, leucomalachite green in fish tissues has been developed. In the present work, graphene was synthesized and evaluated as novel solid-phase extraction sorbents for the analytes enrichment and clean-up. The target analytes were separated on an ultra-pressure BEH C8 column and quantified by a triple-quadrupole linear ion trap mass spectrometer in multiple-reaction monitoring mode. The proposed analytical procedures were carefully optimized and validated. The matrix-matched calibration curves were performed at six concentration levels and good linear relationship (R(2)>0.9990) was observed within the range of 0.25-50μgkg(-1). The proposed method has been successfully applied to the analysis of MG and LMG in several fish samples, indicating that graphene was an efficient SPE sorbent for the enrichment of trace residues in food analysis.
建立了一种基于石墨烯的固相萃取与超高效液相色谱-串联质谱联用的快速分析方法，用于快速测定鱼组织中的孔雀石绿及其代谢物隐色孔雀石绿。在本工作中，合成了石墨烯，并将其评估为新型固相萃取吸附剂，用于分析物的富集和净化。采用超压 BEH C8 柱对目标分析物进行分离，采用三重四极杆线性离子阱质谱仪在多反应监测模式下进行定量分析。对所提出的分析程序进行了仔细的优化和验证。在六个浓度水平上进行了基质匹配校准曲线，在 0.25-50μgkg(-1)范围内观察到良好的线性关系（R(2)>0.9990）。该方法已成功应用于几种鱼样中 MG 和 LMG 的分析，表明石墨烯是一种有效的 SPE 吸附剂，可用于食品分析中痕量残留的富集。
