Wu Kesheng, Guo Liang, Xu Wei, Xu Hengyi, Aguilar Zoraida P, Xu Guomao, Lai Weihua, Xiong Yonghua, Wan Yiqun
State Key Laboratory of Food Science and Technology, Nanchang University, 235 Nanjing East Road, Nanchang 330047, PR China; Jiangxi Institute of Veterinary Drug and Feedstuff control, Nanchang 330047, PR China.
State Key Laboratory of Food Science and Technology, Nanchang University, 235 Nanjing East Road, Nanchang 330047, PR China.
Talanta. 2014 Nov;129:431-7. doi: 10.1016/j.talanta.2014.06.007. Epub 2014 Jun 14.
A magnetic solid-phase extraction method (MSPE) was developed to pre-concentrate and cleanup clenbuterol (CLE) from pork muscle. Novel sulfonated polystyrene magnetic nanobeads (spMNBs) were synthesized via a one-pot emulsion copolymerization method by using divinylbenzene, styrene, and sodium styrene sulfonate in the presence of oleic acid-modified and 10-undecylenic acid-modified magnetic ferrofluid. The resulting spMNBs exhibited high adsorption efficiency for CLE and for 10 other common beta-adrenergic agonists, namely, brombuterol, ractopamine, tulobuterol, bambuterol, cimbuterol, mabuterol, clorprenaline, penbutolol, salbutamol, and cimaterol. The adsorption behavior of the spMNBs for CLE was described by the Langmuir equation with a maximum adsorption capacity of 0.41 mg/g. Under the optimized parameters, the extraction of CLE from 0.5 g of pork muscle required 25mg of the spMNBs at a shortened adsorption time (0.5 min). The proposed MSPE was coupled with colloidal gold nanoparticle-based immunochromatographic assay (MSPE-AuNPIA) for the quantitative detection of CLE residue in pork muscle. The limit of detection and limit of quantification for the pork muscle were 0.10 and 0.24 ng/g, respectively. The intra-day and inter-day assay recoveries at three CLE spiked concentrations ranged from 92.5% to 98.1%, with relative standard deviations ranging from 3.2% to 13.0%. The results of MSPE-AuNPIA were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The CLE values obtained with MSPE-AuNPIA agreed with those obtained with LC-MS/MS.
开发了一种磁性固相萃取方法(MSPE),用于从猪肌肉中预富集和净化克伦特罗(CLE)。通过一锅法乳液共聚法,在油酸改性和10-十一烯酸改性的磁性铁流体存在下,使用二乙烯基苯、苯乙烯和苯乙烯磺酸钠合成了新型磺化聚苯乙烯磁性纳米珠(spMNBs)。所得的spMNBs对CLE以及其他10种常见的β-肾上腺素能激动剂表现出高吸附效率,这10种激动剂分别为溴布特罗、莱克多巴胺、妥布特罗、班布特罗、西马特罗、马布特罗、氯丙那林、喷布洛尔、沙丁胺醇和西马特罗。spMNBs对CLE的吸附行为符合朗缪尔方程,最大吸附容量为0.41 mg/g。在优化参数下,从0.5 g猪肌肉中提取CLE需要25 mg的spMNBs,吸附时间缩短至0.5分钟。所提出的MSPE与基于胶体金纳米颗粒的免疫色谱分析法(MSPE-AuNPIA)联用,用于定量检测猪肌肉中的CLE残留。猪肌肉的检测限和定量限分别为0.10和0.24 ng/g。在三个加标浓度下,日内和日间测定回收率在92.5%至98.1%之间,相对标准偏差在3.2%至13.0%之间。MSPE-AuNPIA的结果通过液相色谱-串联质谱法(LC-MS/MS)进行了确认。MSPE-AuNPIA获得的CLE值与LC-MS/MS获得的值一致。