Wu Ci, Ning Xingshuang, Chen Xi, Ma Junfeng, Zhao Qun, Zhao Li, Zhu Guozhi, Shi Song
Liaoning Academy of Inspection and Quarantine Dalian 116000 China
Department of Oncology, Lombardi Comprehensive Cancer Center, Georgetown University, Technology Centre of Dalian Customs District Washington DC 20057 USA.
RSC Adv. 2021 Aug 31;11(46):28925-28933. doi: 10.1039/d1ra04481h. eCollection 2021 Aug 23.
A simple, accurate, and highly sensitive analytical method was developed in this study for the determination of ten β-agonists and five β-blockers in milk. In this method, new adsorbent phosphonic acid-functionalized porous organic polymers were synthesized through a direct knitting method. The synthesis procedure of the materials and the extraction conditions (such as the composition of loading buffer and eluent) were optimized. Benefitting from the high surface area (545-804 m g), multiple functional framework and good porosity, the phosphonic acid-functionalized porous organic polymers showed a high adsorption rate and high adsorption capacity for β-agonists (224 mg g and 171 mg g for clenbuterol and ractopamine, respectively). The analytes were quantified by ultra-high-performance liquid chromatography coupled to high-resolution tandem mass spectrometry. It showed a good linearity (with ranging from 0.9950 to 0.9991 in the linear range of 3-5 orders of magnitude), with low limits of quantification ranging from 0.05 to 0.25 ng g. The limits of detection of the method for the analytes were measured to be in the range of 0.02 to 0.1 ng g. The recoveries of target analytes from real samples on the material were in the range of 62.4-119.4% with relative standard deviations of 0.6-12.1% ( = 4). Moreover, good reproducibility of the method was obtained with the interday RSD being lower than 11.7% ( = 5) and intraday RSD lower than 12.2% ( = 4). The proposed method was accurate, reliable and convenient for the simultaneous analysis of multiple β-agonists and β-blockers. Finally, the method was successfully applied for the analysis of such compounds in milk samples.
本研究开发了一种简单、准确且高度灵敏的分析方法，用于测定牛奶中的十种β-激动剂和五种β-阻滞剂。在此方法中，通过直接编织法合成了新型吸附剂膦酸功能化多孔有机聚合物。对材料的合成过程和萃取条件（如加载缓冲液和洗脱液的组成）进行了优化。得益于高比表面积（545 - 804 m²/g）、多功能框架和良好的孔隙率，膦酸功能化多孔有机聚合物对β-激动剂表现出高吸附速率和高吸附容量（克伦特罗和莱克多巴胺的吸附容量分别为224 mg/g和171 mg/g）。通过超高效液相色谱与高分辨率串联质谱联用对分析物进行定量。其线性良好（在3 - 5个数量级的线性范围内，r值在0.9950至0.9991之间），定量下限低至0.05至0.25 ng/g。该方法对分析物的检测限在0.02至0.1 ng/g范围内。目标分析物在该材料上从实际样品中的回收率在62.4% - 119.4%之间，相对标准偏差为0.6% - 12.1%（n = 4）。此外，该方法具有良好的重现性，日间相对标准偏差低于11.7%（n = 5），日内相对标准偏差低于12.2%（n = 4）。所提出的方法准确、可靠且便于同时分析多种β-激动剂和β-阻滞剂。最后，该方法成功应用于牛奶样品中此类化合物的分析。
