School of Environmental Engineering and Chemistry, Luoyang Institute of Science and Technology, Luoyang 471023, China.
School of Environmental Engineering and Chemistry, Luoyang Institute of Science and Technology, Luoyang 471023, China.
Food Chem. 2021 Sep 1;355:129662. doi: 10.1016/j.foodchem.2021.129662. Epub 2021 Mar 22.
A facile in-tube solid phase microextraction (in-tube SPME) procedure was developed to enrich ractopamine before HPLC-UV analysis. This was achieved by employing amide groups modified polysaccharide-silica hybrid monolith as an efficient sorbent. The monolith was synthesized by a simple reaction with agarose oxide and tetramethoxylisane, followed by the modification of amide groups via subsequent ring opening, "thiol-ene" click and dehydration reactions. Under the optimized extraction conditions, the enrichment factors for ractopamine, dopamine, clenbuterol, para-methylphenol and phenol were determined to be 50.5, 32.2, 4.8, 2.1 and 1.8, respectively. The monolithic column has ideal selectivity for ractopamine. Coupled with HPLC-UV, this method demonstrated a linearity within 2.0-800 ng/g for ractopamine with spiking in pork muscles (R = 0.9958). The LOD was 0.64 ng/g (S/N = 3) and recoveries ranged from 85.2 to 108.1% (n = 3). This approach provides a feasible way for analysis of trace ractopamine in biological samples.
建立了一种简单的管内固相微萃取（in-tube SPME）方法，用于在 HPLC-UV 分析之前富集莱克多巴胺。该方法通过采用酰胺基修饰的多糖-二氧化硅杂化整体柱作为高效吸附剂来实现。整体柱通过与氧化琼脂糖和四甲氧基硅烷的简单反应合成，然后通过随后的开环、“硫醇-烯”点击和脱水反应来修饰酰胺基。在优化的萃取条件下，莱克多巴胺、多巴胺、克伦特罗、对甲基苯酚和苯酚的富集因子分别为 50.5、32.2、4.8、2.1 和 1.8。该整体柱对莱克多巴胺具有理想的选择性。与 HPLC-UV 结合，该方法在猪肉肌肉中莱克多巴胺的线性范围为 2.0-800 ng/g（R = 0.9958）。LOD 为 0.64 ng/g（S/N = 3），回收率在 85.2%至 108.1%之间（n = 3）。该方法为生物样品中痕量莱克多巴胺的分析提供了一种可行的方法。
