State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, P.O. Box 1009, Xiamen, 361005, China.
Anal Bioanal Chem. 2013 Aug;405(21):6885-9. doi: 10.1007/s00216-013-7124-6. Epub 2013 Jun 19.
A highly sensitive method was developed for the simultaneous determination of ten sulfonamides in pork and chicken samples by monolith-based stir bar sorptive extraction (SBSE) coupled to high-performance liquid chromatography tandem mass spectrometry. The samples were freeze-dried and extracted by acetonitrile, then enriched and further extracted by SBSE which was based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) as coating. To achieve optimum extraction performance of SBSE for sulfonamides, several parameters, including pH value and ionic strength in the sample matrix and extraction and desorption time, were investigated in detail. Under the optimal conditions, the limits of detection (S/N = 3) for target sulfonamides were 1.2-6.1 ng/kg in pork and 2.0-14.6 ng/kg in chicken, respectively. Real samples spiked at the concentration of 0.5 and 5.0 μg/kg showed recoveries above 55% and relative standard deviations below 12%. At the same time, the extraction performances of target sulfonamides on SBSE-VPMB were compared with other SBSE based on porous monolith and commercial SBSE.
建立了一种基于整体柱搅拌棒吸附萃取(SBSE)与高效液相色谱-串联质谱联用测定猪肉和鸡肉中十种磺胺类药物残留的分析方法。样品经冷冻干燥后,以乙腈提取,再用基于聚(邻苯二甲酰亚胺-co-N,N-亚甲基双丙烯酰胺)整体柱(SBSE-VPMB)的 SBSE 进行浓缩和进一步萃取。为了实现 SBSE 对磺胺类药物的最佳萃取性能,详细考察了样品基质中 pH 值和离子强度以及萃取和洗脱时间等参数。在最佳条件下,十种磺胺类药物在猪肉和鸡肉中的检出限(S/N=3)分别为 1.2-6.1 ng/kg 和 2.0-14.6 ng/kg。在 0.5 和 5.0 μg/kg 浓度水平下进行加标回收实验,回收率均在 55%以上,相对标准偏差均小于 12%。同时,还比较了目标磺胺类药物在 SBSE-VPMB 上的萃取性能与其他基于多孔整体柱和商品化 SBSE 的萃取性能。