Zhang Honglian, Zhang Min, Li Li, Dong Wei, Ren Qiyong, Xu Feng, Wang Yuanrui, Xu Tao, Liu Jicheng
School of Pharmacy, Qiqihar Medical University, Qiqihar 161006, China.
Qiqihar Institute for Food and Drug Control, Qiqihar 161006, China.
Molecules. 2023 Sep 6;28(18):6473. doi: 10.3390/molecules28186473.
Residual quinolones in food that exceed their maximum residue limit (MRL) are harmful to human health. However, the existing methods used for testing these residues have limitations; so, we developed a new limit test method called TLC-SERS to rapidly determine the levels of residues of the following: enrofloxacin (A), ciprofloxacin (B), ofloxacin (C), fleroxacin (D), sparfloxacin (E), enoxacin (F), gatifloxacin (G), and nadifloxacin (H). The residues ware preliminarily separated via TLC. The tested compounds' position on a thin-layer plate were labeled using their relative R under 254 nm ultraviolet light, and an appropriate amount of nanometer silver solution was added to the position. The silver on the plate was irradiated with a 532 nm laser to obtain the SERSs of the compounds. The results show significant differences in the SERS of the eight quinolones: the LODs of H, A, D, E, C, G, F, and B were 9.0, 12.6, 8.9, 19.0, 8.0, 8.7, 19.0, and 12.6 ng/mL, respectively; and the RSD was ≤4.9% for the SERS of each quinolone. The limit test results of 20 samples are consistent with those obtained via UPLC-MS/MS. The results indicate that TLC-SERS is a specific, sensitive, stable, and accurate method, providing a new reference for the rapid limit test of harmful residues in foods.
食品中残留的喹诺酮类药物若超过其最大残留限量(MRL),会对人体健康有害。然而,现有的检测这些残留的方法存在局限性;因此,我们开发了一种名为薄层色谱-表面增强拉曼光谱法(TLC-SERS)的新限量检测方法,以快速测定以下药物的残留水平:恩诺沙星(A)、环丙沙星(B)、氧氟沙星(C)、氟罗沙星(D)、司帕沙星(E)、依诺沙星(F)、加替沙星(G)和那氟沙星(H)。残留药物先通过薄层色谱进行初步分离。在254nm紫外光下,利用被测化合物的相对比移值(Rf)在薄层板上标记其位置,并在该位置加入适量的纳米银溶液。用532nm激光照射板上的银,以获得化合物的表面增强拉曼光谱(SERS)。结果表明,8种喹诺酮类药物的SERS存在显著差异:H、A、D、E、C、G、F和B的检测限分别为9.0、12.6、8.9、19.0、8.0、8.7、19.0和12.6 ng/mL;每种喹诺酮类药物SERS的相对标准偏差(RSD)≤4.9%。20个样品的限量检测结果与超高效液相色谱-串联质谱法(UPLC-MS/MS)的结果一致。结果表明,TLC-SERS是一种特异、灵敏、稳定且准确的方法,为食品中有害残留的快速限量检测提供了新的参考。