提出了一种亲水有机溶剂(乙醇、正丙醇、四氢呋喃等)气浮浮选(双水相气浮浮选)分离,富集光度法测定污水中痕量土霉素(OTC)的新型绿色高效分析方法。利用自制的浮选装置,选择四氢呋哺作溶剂,氯化钠作分相剂,氢氧化钠溶液调节酸度,将Ni(Ⅱ)与OTC形成的疏水性缔合物浮选至有机相,浮选完毕后经分光光度法分析,线性范围为1.1×10^-7-9.7×10^-6mol/L,线性回归方程为A=2.038×10^5C(mol/L)+0.005,相关系数为0.9996,检出限为7.36×10^-8mol/L,回收率为99.8%-100.4%,表观摩尔吸光率ε=2.38×10^5L/mol·cm,适用于污水中痕量土霉素的分离/富集及分析测定。
A novel and green method for separating and enriching trace OTC in sewage by aqueous two-phase gas floatation spectrophotometry was proposed. Hydrophobic complex composed of Ni( Ⅱ ) and OTC was floated into organic phase under the optimal conditions of pH 9, home made floatation equipment, tetrahydrofuran as organic solvent and sodium chloride as separating phase reagent. The data was obtained by spectrophotometry after floatation, with linear regression equation as 2.038×10^5C (mol/L)+0.005, linear range from 1.1×10^-7 to 9.7×10^-5mol/L, correlation coefficient better than 0.9996, relative recovery 99.8%-100.4% and detection limit 7.36×10^-8mol/L. It can be applied to analysis of trace OTC in sewage.