State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen 361005, China.
J Chromatogr A. 2009 Nov 13;1216(46):8240-5. doi: 10.1016/j.chroma.2009.05.031. Epub 2009 May 21.
A simple, rapid, and sensitive method for the quantitative monitoring of five sulfonamide antibacterial residues (SAs) in milk was developed by stir bar sorptive extraction (SBSE) coupling to high performance liquid chromatography with diode array detection. The analytes were concentrated by SBSE based on poly (vinylimidazole-divinylbenzene) monolithic material as coating. The extraction procedure was very simple, milk was diluted with water then directly sorptive extraction without elimination of fats and protein in samples was required. To achieve optimum extraction performance for SAs, several parameters, including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. Under the optimized experimental conditions, low detection limits (S/N=3) quantification limits (S/N=10) of the proposed method for the target compounds were achieved within the range of 1.30-7.90 ng/mL and 4.29-26.3 ng/mL from spiked milk, respectively. Good linearities were obtained for SAs with the correlation coefficients (R(2)) above 0.996. Finally, the proposed method was successfully applied to the determination of SAs compounds in different milk samples and satisfied recoveries of spiked target compounds in real samples were obtained.
建立了一种基于搅拌棒吸附萃取(SBSE)与高效液相色谱-二极管阵列检测联用技术,用于牛奶中 5 种磺胺类抗菌药物残留的简单、快速、灵敏的检测方法。以聚(4-乙烯基咪唑-二乙烯基苯)整体材料为涂层,通过 SBSE 对目标物进行浓缩。该萃取方法非常简单,只需要将牛奶用水稀释,无需去除样品中的脂肪和蛋白质,即可直接进行吸附萃取。为了获得最佳的萃取性能,对萃取和解析时间、解析溶剂、样品基质的离子强度和 pH 值等参数进行了考察。在优化的实验条件下,该方法对目标化合物的检测限(S/N=3)和定量限(S/N=10)分别在 1.30-7.90ng/mL 和 4.29-26.3ng/mL 的范围内,在所研究的范围内,磺胺类药物均具有良好的线性关系(R(2)>0.996)。最后,该方法成功地应用于不同牛奶样品中磺胺类化合物的测定,实际样品中目标化合物的加标回收率令人满意。