建立了一种新型分离方法——双水相气浮浮选光度法,使其处理环境水样中痕量土霉素(OTC)残留物,研究了其工作原理,并用高效液相色谱法对该方法的可靠性进行了验证。利用自制的双水相气浮浮选装置,选择四氢呋喃作亲水有机溶剂、质量分数为10%的NaCl溶液作分相剂,NaOH溶液调节pH,将Cu^2+与OTC形成的疏水配合物浮选至有机相,实现OTC与水样分离。浮选完毕后,经紫外-可见分光光度法分析,线性回归方程为A=1.532×10^5c+0.1230(其中:A为有机相的吸光度;c为水样的OTC摩尔浓度,mol/L),相关系数为0.9998,该方法的线性范围为4.8×10^-7~7.3×10^-5mol/L,OTC加标回收率为99.5%~100.1%。
The paper presents a novel and green analytical method for measurement of trace level oxytetracycline (OTC) in water samples. An aliquot of CuSO4 solution was added to the sample to form hydrophobic Cu^2+ -OTC complex which was separated and concentrated by solvent (tetrahydrofuran) extraction and gas floatation before measurement by the HPLC; NaCl, NaOH were employed to provide the optimal ionic strength for extraction/floatation at pH of 8. The method is accurate, highly reproducible and applicable over a wide concentration range (4.8 × 10^-7 to 7.3× 10^-5 tool/L) with a very low detection limit of 5.1 × 10^-8 mol/L.