College of Food Science Sciences, Shanxi Normal University, Taiyuan 030000, China.
Tianjin Key Laboratory of Risk Assessment and Control Technology for Environment and Food Safety, Tianjin Institute of Environmental and Operational Medicine, Tianjin 300050, China.
Molecules. 2023 Jul 10;28(14):5307. doi: 10.3390/molecules28145307.
Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10-200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples.
抗生素药物残留会对人体产生不良影响。林可霉素是一种常见的兽药，可在动物源食品中形成残留。然而，检测实际样品中痕量林可霉素残留水平具有挑战性。在此，开发了一种简单的固相萃取（SPE）方法，用于在高效液相色谱-串联质谱法（HPLC-MS/MS）检测前从牛奶样品中富集林可霉素。SPE 中使用的吸附剂是通过溶剂热合成方法制备的基于 Cu 的金属有机骨架（Cu-MOF）。使用扫描电子显微镜（SEM）、傅里叶变换红外光谱（FT-IR）、X 射线衍射（XRD）、差示热重分析（TG-DTA）和 N2 吸附-解吸实验对制备的 MOFs 进行了表征。研究了吸附容量（吸附平衡、萃取时间、pH 值）和洗脱溶剂参数。在优化的 HPLC-MS/MS 方法条件下，林可霉素在 10-200 g/L 的线性范围内检测，检测限为 0.013 ng/mL。商业牛奶样品中添加了林可霉素，回收率在 92.3%至 97.2%之间。因此，该方法可成功用于从牛奶样品中富集和测定林可霉素。
