纸基薄层快速净化策略及辣椒油中痕量残留检测方法研究

Rapid Purification Strategy of Paper-Based Thin Layer and Detection of Trace Residues in Chili Oil

基于利用PVC包覆的纸基薄层条带(硅胶G60为固定相)构筑了快速分离纸基条带,以四种苏丹红染料(SudanⅠ~Ⅳ)为非法添加污染物模拟底物添加在辣椒油油脂样品或原料中,以正己烷:丙酮:冰乙酸(65∶35∶1)为展开体系对不同油脂基质的加标样品进行展开处理。在优化后的展开条件下该分离条带能够有效地分离油脂样品,样品中大部分基质与目标底物实现有效分开,四种苏丹红可以相对集中在<0.5 cm宽度的条带区域,裁切后的条带以氨化乙腈提取可以回收获得净化后样品。同时以苏丹红专用固相萃取小柱对比了净化效果。与固相萃取小柱相比,该净化条带能够较好的实现低溶剂消耗,快速净化且质谱检测基质影响较小。样品测定的准确性和回收率验证了本策略的有效性。本研究构建的净化条带具有安全、简便快捷、成本低等优点,在农产品品质鉴定与复杂基质样品的快速前处理净化检测痕量污染物等领域有着广泛的应用前景。

A rapid separate paper-based strip as clean-up was developed in this study for the determination of Sudan Ⅰ-Ⅳ in chili oils. This developed strip was coated with PVC with silica gel G60 as stationary phase, and the mixture of n-hexane: acetone: glacial acetic acid(65∶35∶1) was chosen as the optimized developing solvents. According to our results, we found that the matrix and the target compounds in samples could be completely separated, and Sudan Ⅰ~Ⅳ could be concentrated in a relative narrow area of the developed strip, less than 0.5 cm width. And then Sudan Ⅰ~Ⅳ from the clipped areas was extracted with acetonitrile containing ammonia, followed by clean-up. In order to investigate the clean-up effect of this developed strip, the special solid phase extraction column of Sudan was chosen. We found that the strips as clean-up combined with MS detection was with lower matrix effects, better recovery and accuracy. Above all, this developed strip as clean-up was with the advantages of safety, simplicity and low cost for the rapid determination of trace contaminations in agricultural products.