Li Jincheng, Zhou Ruidong, Yang Guangxin, Kouadio Fodjo Essy, Feng Tengwang, Sun Huiwu, Huang Dongmei, Kong Cong, Liu Huan
Key Laboratory of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture and Rural Affairs, Chinese Academy of Fishery Sciences, Beijing 100141, PR China.
College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, PR China.
Food Chem X. 2023 Aug 19;19:100846. doi: 10.1016/j.fochx.2023.100846. eCollection 2023 Oct 30.
In this study, a novel filter-press cleanup column was developed as a single-step cleanup approach for the rapid screening and quantification of 112 veterinary drugs in fish samples. Fish muscle samples were extracted with acetonitrile and ethyl acetate, sequentially. After concentration and reconstitution, -propylethylenediamine (PSA) sorbent, packed in filter-press column, allows rapid single-step cleanup operation, while UHPLC-Q-Orbitrap-HRMS provides high-precision mass information in multi-residue screening. Under optimum settings, the detection and quantification limits were validated at 0.5 and 2.0 μg·kg, for all analytes, respectively. The ranges of recoveries were from 35.3 to 138.4%. Most of these target analytes (82%) could be measured with recoveries between 60 and 130%, and intra-day RSDs ranging from 1.9 to 26.1%. This method was further applied to evaluate the residual of veterinary drugs in fish samples from four cities in China, and results demonstrated its practicability for multi-residue monitoring veterinary residues for food safety administration.
在本研究中,开发了一种新型压滤净化柱,作为一种单步净化方法,用于快速筛查和定量鱼类样品中的112种兽药。鱼肌肉样品依次用乙腈和乙酸乙酯萃取。浓缩并复溶后,填充在压滤柱中的丙基乙二胺(PSA)吸附剂可实现快速单步净化操作,而超高效液相色谱-四极杆-轨道阱-高分辨质谱(UHPLC-Q-Orbitrap-HRMS)在多残留筛查中提供高精度质量信息。在最佳设置下,所有分析物的检测限和定量限分别验证为0.5和2.0 μg·kg。回收率范围为35.3%至138.4%。这些目标分析物中的大多数(82%)回收率在60%至130%之间,日内相对标准偏差(RSD)在1.9%至26.1%之间,均可进行测定。该方法进一步应用于评估中国四个城市鱼类样品中兽药的残留情况,结果证明了其在食品安全管理中多残留监测兽药残留的实用性。