磺胺类药物不仅在临床上应用广泛,而且在畜牧业中也受到高度重视。最近,磺胺类药物残留超过食品中的标准限值已变得司空见惯,会影响人类健康。目前的法规限制了这些残留物。因此,我们构建了一种新的极限测试方法来快速测定磺胺类药物残留的水平。使用称为TLC-SERS的最新方法检测了六种磺胺类药物,即,磺胺地塞米松(A),磺胺二甲嘧啶(B),磺胺多辛(C),磺胺甲氧嘧啶(D),磺胺甲恶唑(E),和磺胺噻唑(F)。研究了这六种药物的SERS检测的最佳条件,并比较了不同薄层色谱法对它们的分离效果。然后,我们成功地建立了一个分离系统,使用二氯甲烷-甲醇-氨的比例为5:1:0.25(v/v/v),这对六种药物有很好的分离效果。通过TLC初步分离残余物。将银溶胶溶液以相应的特定位移值添加到硅胶G板上的斑点上,并进行SERS检测。将样品溶液置于532nm激光下的现场,收集并分析了六种磺胺类药物的SERS光谱。结果表明,六种磺胺类药物的SERS谱有明显差异,从A到F的LOD为12.5、6.4、6.3、7.1、18.8和6.2ng/mL,分别,RSD<3.0%。在48小时内,每种磺胺类药物的SERS信号保持稳定,RSD<3.0%。TLC-SERS法检测20个样品的结果与UPLC-MS/MS法检测结果一致。所建立的TLC-SERS方法简单、快速,为食品中残留限量的快速检测提供了有益的参考。
Sulfonamides are not only widely applied in clinics but also highly valued in animal husbandry. Recently, it has become common for sulfonamide
residues to exceed the standard limits in food, which can affect human health. Current regulations limit these
residues. Therefore, we constructed a new limit test method to rapidly determine the levels of sulfonamide
residues. Six sulfonamides were detected using the latest method called TLC-SERS, namely, sulfamethasone (A), sulfamethazine (B), sulfadoxine (C), sulfamethoxydiazine (D), sulfamethoxazole (E), and sulfathiazole (F). The optimal conditions for SERS detection were investigated for these six drugs, and the separation effects of different TLC spreaders on them were compared. Then, we successfully established a separation system using dichloromethane-methanol-ammonia in a ratio of 5:1:0.25 (v/v/v), which provided good separation effects on the six drugs. The
residues were preliminarily separated via TLC. A silver sol solution was added to the spot on the silica gel G plate at the corresponding specific shift values, and SERS detection was performed. The sample solution was placed on the spot under a 532 nm laser, and the SERS spectrum was collected and analyzed for the six sulfonamides. The results showed obvious variations in the SERS spectrum among the six sulfonamides, with the LODs being 12.5, 6.4, 6.3, 7.1, 18.8, and 6.2 ng/mL from A to F, respectively, and an RSD of <3.0%. Within 48 h, the SERS signal for each sulfonamide drug was kept stable, with an RSD of <3.0%. The detection results of 20 samples using the TLC-SERS method were consistent with those obtained by UPLC-MS/MS. The established TLC-SERS method is simple and fast, providing a useful reference for the rapid detection of residue limits in food.