School of Environmental Engineering and Chemistry, Luoyang Institute of Science and Technology, No. 90, Wangcheng Avenue, Luoyang, 471023, P. R. China.
School of chemistry and chemical engineering, Henan Normal University, No. 46, East Section of Jianshe Road, Xinxiang, 453000, P. R. China.
J Sep Sci. 2022 Dec;45(24):4460-4468. doi: 10.1002/jssc.202200599. Epub 2022 Oct 25.
Exploiting adsorbents with highly efficient extraction performance is of great promise for extracting small organic molecules from biological samples. In this work, a novel Zn -immobilized chitosan@silica hybrid monolith was prepared through a simple self-assembly Zn -immobilization process. Exploited as an adsorbent in solid-phase micro-extraction for extracting trace β-agonists, the monolith exhibited high extraction efficiencies for salbutamol, clenbuterol, and ractopamine with the enrichment factors approaching 120, 85, and 52, respectively. These could be attributed to the effective interaction between Zn ions and the target molecule via coordination or other intermolecular interactions. Under optimized extraction operations, a sensitive determination was successfully developed coupling with high-performance liquid chromatography-ultraviolet detection. The linear range was 0.17-58.8, 0.12-68.5, and 0.18-65.5 ng/ml for salbutamol, clenbuterol, and ractopamine. The limits of detection of the β-agonists were from 0.04 to 0.07 ng/ml, and the limits of quantification were from 0.12 to 0.18 ng/ml. The recoveries of spiking in mutton samples were observed in the range of 85.9%-95.7%, with relative standard deviations <8.0% (n = 3). Application tests demonstrated this newly developed determination was practical, accurate, and convenient for detecting trace content β-agonists in meat.
利用具有高效萃取性能的吸附剂从生物样品中提取小分子有机化合物具有很大的前景。在这项工作中，通过简单的自组装 Zn 固定化过程制备了一种新型的 Zn 固定化壳聚糖@二氧化硅杂化整体柱。作为固相微萃取中的吸附剂，用于提取痕量β-激动剂，该整体柱对沙丁胺醇、克伦特罗和莱克多巴胺的萃取效率很高，富集因子分别接近 120、85 和 52。这可以归因于 Zn 离子与目标分子通过配位或其他分子间相互作用的有效相互作用。在优化的萃取操作条件下，成功地建立了与高效液相色谱-紫外检测相结合的灵敏测定方法。沙丁胺醇、克伦特罗和莱克多巴胺的线性范围分别为 0.17-58.8、0.12-68.5 和 0.18-65.5 ng/ml。β-激动剂的检出限为 0.04-0.07 ng/ml，定量限为 0.12-0.18 ng/ml。在羊肉样品中的加标回收率在 85.9%-95.7%之间，相对标准偏差 <8.0%（n=3）。应用测试表明，这种新开发的测定方法实用、准确、方便，可用于检测肉类中痕量β-激动剂。
