Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, São João del-Rei, Minas Gerais 36301-160, Brazil.
Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, São João del-Rei, Minas Gerais 36301-160, Brazil.
J Chromatogr A. 2024 Apr 12;1720:464809. doi: 10.1016/j.chroma.2024.464809. Epub 2024 Mar 10.
An ultrafast, efficient, and eco-friendly method combining magnetic solid phase extraction and capillary electrophoresis with diode array detection have been developed to determine ractopamine residues in food samples. A restricted access material based on magnetic and mesoporous molecularly imprinted polymer has been properly synthesized and characterized, demonstrating excellent selectivity and high adsorbent capacity. Short-end injection capillary electrophoresis method was optimized: 75 mM triethylamine pH 7 as BGE, -20 kV, 50 mbar by hydrodynamic injection during 8 s, and capillary temperature at 25 °C; reaching ultrafast ractopamine analysis (∼0.6 min) with good peak asymmetry, and free from interfering and/or baseline noise. After sample preparation optimization, the conditions were: 1000 µL of sample at pH 6, 20 mg of adsorbent, stirring time of 120 s, 250 µL of ultrapure water as washing solvent, 1000 µL of methanol: acetic acid (7: 3, v/v) as eluent, and the adsorbent can be reused four times. In these conditions, the analytical method showed recoveries around to 100 %, linearity ranged from 9.74 to 974.0 µg kg, correlation coefficient (r) ≥ 0,99 in addition to adequate precision, accuracy, and robustness. After proper validation, the method was successfully applied in the analysis ractopamine residues in bovine milk and bovine and porcine muscle.
一种结合了磁性固相萃取和毛细管电泳与二极管阵列检测的超快速、高效、环保的方法已被开发出来,用于检测食品样品中的莱克多巴胺残留。一种基于磁性和介孔分子印迹聚合物的受限进入材料已被适当合成和表征,表现出优异的选择性和高吸附容量。短端进样毛细管电泳法进行了优化:BGE 为 75 mM 三乙胺 pH7,-20 kV,50 mbar 通过 8 s 内的水力进样,毛细管温度为 25°C;达到超快速莱克多巴胺分析(约 0.6 分钟),峰形不对称性良好,无干扰和/或基线噪声。在样品制备优化后,条件为:pH6 的 1000 µL 样品、20 mg 吸附剂、搅拌时间 120 s、250 µL 超纯水作为洗涤溶剂、1000 µL 甲醇:乙酸(7:3,v/v)作为洗脱液,吸附剂可重复使用四次。在此条件下,分析方法的回收率约为 100%,线性范围为 9.74 至 974.0 µg kg,相关系数(r)≥0.99,此外还具有足够的精密度、准确度和稳健性。经过适当验证,该方法成功应用于牛奶奶和牛、猪肌肉中莱克多巴胺残留的分析。