Liu Haibo, Gan Ning, Chen Yinji, Ding Qingqing, Huang Jie, Lin Saichai, Cao Yuting, Li Tianhua
Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, China.
Department of Food Science and Engineering/Collaborative Innovation Center for Modern Grain Circulation and Safety, Nanjing University of Finance and Economics, Nanjing, China.
J Sep Sci. 2016 Sep;39(18):3578-85. doi: 10.1002/jssc.201600479. Epub 2016 Aug 16.
A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018-0.022 and 0.042-0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β2 -agonists residues in real food samples.
开发了一种基于一系列萃取净化盘的快速、特异性预处理方法,该萃取净化盘由分子印迹聚合物整体柱和C18吸附剂组成,用于特异性富集食品中的沙丁胺醇和克伦特罗残留。以沙丁胺醇为模板,通过一步合成法合成了分子印迹整体聚合物盘。它能同时特异性识别沙丁胺醇和克伦特罗。将整体聚合物盘和一系列C18盘与注射器组装在一起,形成一套用于萃取目标分子的定制装置。在一次运行中,沙丁胺醇和克伦特罗可被甲醇/乙酸/H2O特异性萃取、净化和洗脱。目标分子经硅烷化衍生化反应后,采用气相色谱-质谱联用仪进行检测。研究并讨论了溶剂解吸、样品pH值和再加载循环等参数。在优化的萃取和净化条件下,沙丁胺醇和克伦特罗的检测限和定量限分别为0.018 - 0.022 ng/g和0.042 - 0.049 ng/g。所描述的分析方法简便、快速且具有特异性;因此,在实际食品样品中β2-激动剂残留的高通量分析中可能具有高效性。