Li Xiaowei, Guo Ping, Shan Yawen, Ke Yuebin, Li Hui, Fu Qin, Wang Yingyu, Liu Tianhe, Xia Xi
Beijing Advanced Innovation Center for Food Nutrition and Human Health, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Jiangxi Research Institute for Food Inspection and Testing, Nanchang 330001, China.
J Chromatogr A. 2017 May 26;1499:57-64. doi: 10.1016/j.chroma.2017.03.055. Epub 2017 Mar 23.
This work reports the development of a multi-residue method for the identification and quantification of 82 veterinary drugs belonging to different chemical classes in swine waste lagoon. The proposed method applies a solid-phase extraction procedure with Oasis PRiME HLB cartridges that combines isolation of the compounds and sample clean-up in a single step. Analysis is performed by ultra-high performance liquid chromatography-tandem mass spectrometry, in one single injection with a chromatographic run time of only 9.5min. Linearity was studied in the range between 1 and 500μgkg using standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination higher than 0.99 for all the analytes except for cefapirin in matrix. The average recoveries were in the range of 60-110% for most of the compounds tested with inter-day relative standard deviations below 17%. More than 97% of the investigated compounds had less or equal to a 5μgkg quantitation limit in the studied matrix. Finally, the method was used with success to detect and quantify veterinary drugs residues in real samples with sulfonamides, quinolones, and tetracyclines being the most frequently determined compound groups.
本研究报道了一种多残留方法的开发，用于鉴定和定量猪粪污泻湖中的82种不同化学类别的兽药。所提出的方法采用Oasis PRiME HLB固相萃取柱，将化合物的分离和样品净化合并为一步。分析通过超高效液相色谱-串联质谱法进行，单次进样，色谱运行时间仅为9.5分钟。使用纯溶剂和基质存在下制备的标准品，在1至500μg/kg范围内研究线性，除基质中的头孢匹林外，所有分析物的测定系数均高于0.99。大多数测试化合物的平均回收率在60%-110%之间，日间相对标准偏差低于17%。在所研究的基质中，超过97%的被调查化合物的定量限小于或等于5μg/kg。最后，该方法成功用于检测和定量实际样品中的兽药残留，磺胺类、喹诺酮类和四环素类是最常检测到的化合物组。
