Department of Pharmacology, College of Veterinary Medicine, South China Agricultural University, Guangzhou, Guangdong, PC 510642, People's Republic of China.
Anal Chim Acta. 2011 Apr 1;690(2):269-74. doi: 10.1016/j.aca.2011.02.029. Epub 2011 Feb 18.
A simple, sensitive and reproducible molecularly imprinted solid-phase extraction (MISPE) coupled with high performance liquid chromatographic method was developed for monitoring tilmicosin in feeds. The polymers were prepared using tylosin as mimic template molecule, methacrylic acid as functional monomer and ethylene glycol dimethacrylate as cross-linking monomer, and chloroform as a solvent by bulk polymerization. Under the optimum MISPE conditions, the novel polymer sorbent can selectively extract and enrich tilmicosin from variety of feeds. The MISPE cartridge was better than non-imprinted, C(18) and HLB cartridges in terms of both recovery and precision. Mean recoveries of tilmicosin from five kinds of feeds spiked at 1, 10 and 50 mg kg(-1) ranged from 76.9% to 95.6%, with intra-day and inter-day relative standard deviation less than 7.6%. The linearity was ranged from 1.0 to 100 mg L(-1) for matrix standard solution (r=0.9990). The limit of detection was approximately 0.35 mg kg(-1) and the limit of quantification was approximately 0.98 mg kg(-1). There was cleaner chromatogram by using MISPE than C(18) and HLB SPE.
建立了一种简单、灵敏、重现性好的分子印迹固相萃取（MISPE）-高效液相色谱法，用于饲料中替米考星的监测。将泰乐菌素作为模拟模板分子、甲基丙烯酸作为功能单体、乙二醇二甲基丙烯酸酯作为交联单体，氯仿作为溶剂，通过本体聚合制备聚合物。在最佳的 MISPE 条件下，新型聚合物吸附剂可从多种饲料中选择性提取和富集替米考星。与非印迹、C(18)和 HLB 柱相比，MISPE 柱在回收率和精密度方面都有优势。替米考星在五种饲料中的添加水平为 1、10 和 50mg/kg 时的平均回收率为 76.9%至 95.6%，日内和日间相对标准偏差均小于 7.6%。基质标准溶液的线性范围为 1.0-100mg/L（r=0.9990）。检测限约为 0.35mg/kg，定量限约为 0.98mg/kg。与 C(18)和 HLB SPE 相比，MISPE 可获得更清洁的色谱图。
