Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.
J Sep Sci. 2018 Feb;41(3):723-731. doi: 10.1002/jssc.201701205. Epub 2017 Dec 18.
A highly selective molecularly imprinted polymer sorbent was synthesized and employed for the simultaneous determination of six sulfonamide antibiotic residues (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, and sulfamethizole) in milk samples. Multi-analyte imprinted particles were used as a sorbent in solid-phase extraction. Sulfonamides were separated on a high-performance liquid chromatography column (Merck-Lichrospher RP18e, 5 μm 250 × 4 mm) and further identified and quantified by diode array detection. Several parameters including required loading of the molecularly imprinted polymer sorbent, mass of milk, volume, and type of elution solvent, as well as time for absorption and elution were investigated to obtain optimal experimental conditions. For comparison purpose, a non-imprinted polymer was applied under the optimum conditions. The validation study according to the European Union Decision 2002/657/EC was based on the investigation of linearity, selectivity, stability, limits of detection and quantitation, decision limit, detection capability, trueness, precision, and ruggedness according to Youden's approach. The decision limit and detection capability values in the milk were achieved from 101.9 to 113.5 μg/kg and from 114.4 to 135.4 μg/kg, respectively, depending on the target sulfonamide drug. Finally, the optimized protocol was successfully applied to commercial milk samples and human breast milk.
一种高选择性的分子印迹聚合物吸附剂被合成并用于同时测定牛奶样品中的六种磺胺类抗生素残留（磺胺、磺胺醋酰、磺胺嘧啶、磺胺噻唑、磺胺甲噁唑和磺胺二甲嘧啶）。多分析物印迹颗粒被用作固相萃取中的吸附剂。磺胺类药物在高效液相色谱柱（默克-利希罗普斯 RP18e，5μm 250×4mm）上分离，并用二极管阵列检测进一步鉴定和定量。研究了几个参数，包括分子印迹聚合物吸附剂的负载量、牛奶的质量、洗脱溶剂的体积和类型以及吸收和洗脱的时间，以获得最佳的实验条件。为了比较目的，在最佳条件下应用了非印迹聚合物。根据欧盟第 2002/657/EC 号决定进行的验证研究是基于对线性、选择性、稳定性、检测限和定量限、决策限、检测能力、准确度、精密度和稳健性进行调查，采用 Youden 方法。根据目标磺胺类药物的不同，牛奶中的决策限和检测能力值分别为 101.9 至 113.5μg/kg 和 114.4 至 135.4μg/kg。最后，优化的方案成功地应用于商业牛奶样品和人乳。
