Li Xin, Wang Man-Man, Zheng Guo-Ying, Ai Lian-Feng, Wang Xue-Sheng
†School of Public Health, Hebei United University, Tangshan 063000, Hebei, China.
‡Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, Hebei, China.
J Agric Food Chem. 2015 Apr 29;63(16):4096-103. doi: 10.1021/acs.jafc.5b00739. Epub 2015 Apr 20.
A hydrophobic monolith (10 mm × 2.1 mm i.d.) was developed as a reusable online solid-phase extraction (SPE) sorbent coupled with LC-MS/MS for the rapid determination of five avermectin residues in foodstuffs of both plant and animal origin. The online SPE was achieved using a 10 mmol/L ammonium acetate solution as the loading solvent, and acetonitrile (MeCN) was selected for the washing step. After being transferred from the monolith into a C18 analytical column using MeCN, the analytes were analyzed by LC-MS/MS using MeCN/0.1% NH4OH (10:90, v/v) as the mobile phase. The detection limit was 2 μg/kg for five avermectins, and the recoveries in fresh pear, chili seed, bovine muscle, and milk ranged from 71.8% to 101.3% with relative standard deviations of less than 8.94%. The online SPE and determination were achieved within 15 min, and the monolithic extractor was reusable for more than 500 experiments.
开发了一种疏水整体柱（内径10 mm×2.1 mm）作为可重复使用的在线固相萃取（SPE）吸附剂，与液相色谱-串联质谱联用，用于快速测定动植物源性食品中的5种阿维菌素残留。在线固相萃取通过使用10 mmol/L醋酸铵溶液作为上样溶剂来实现，洗涤步骤选用乙腈（MeCN）。使用MeCN将分析物从整体柱转移至C18分析柱后，采用MeCN/0.1% NH4OH（10:90，v/v）作为流动相，通过液相色谱-串联质谱对分析物进行分析。5种阿维菌素的检出限为2 μg/kg，在新鲜梨、辣椒籽、牛肌肉和牛奶中的回收率为71.8%至101.3%，相对标准偏差小于8.94%。在线固相萃取和测定在15分钟内完成，整体柱萃取器可重复使用500多次实验。
