School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, P. R. China.
J Sep Sci. 2019 Jul;42(13):2255-2262. doi: 10.1002/jssc.201801009. Epub 2019 May 15.
This study presents a simple and green dispersive micro-solid phase extraction method for preconcentration of acidic quinolones from honey prior to high performance liquid chromatography determination. A two-dimensional nanostructured zinc-aluminum layered double hydroxide was synthesized and used as the sorbent for dispersive micro-solid phase extraction. Its different characteristics from conventional sorbents is that it is dissolvable in acidic solution (pH < 4). After the extraction, the analyte elution step was omitted and thus the use of organic solvents was avoided. The key parameters influencing the extraction efficiency such as the amount of sorbent, pH of sample solution, vortex time, type and volume of acidic solution were investigated and optimized. The method exhibited low limits of detection (3.0-5.0 ng/g), good linearity (10-2000 ng/g) with coefficients of determinations higher than 0.9991, acceptable precision (RSD<9.1%) and accuracy (RE<5.8%). The proposed method is fast, efficient, eco-friendly, and suitable for the determination of acidic quinolones in honey samples.
本研究提出了一种简单、绿色的分散微固相萃取方法,用于在高效液相色谱测定前从蜂蜜中预浓缩酸性喹诺酮类药物。合成了二维纳米结构的锌铝层状双氢氧化物,并将其用作分散微固相萃取的吸附剂。与传统吸附剂不同的是,它可溶于酸性溶液(pH < 4)。萃取后,省略了洗脱步骤,避免了有机溶剂的使用。考察并优化了影响萃取效率的关键参数,如吸附剂用量、样品溶液 pH 值、涡旋时间、酸性溶液的类型和体积。该方法的检出限低(3.0-5.0 ng/g),线性良好(10-2000 ng/g),相关系数大于 0.9991,精密度(RSD<9.1%)和准确度(RE<5.8%)均令人满意。该方法快速、高效、环保,适用于蜂蜜样品中酸性喹诺酮类药物的测定。