反相离子对液相色谱分离-柱后衍生化学发光检测痕量金属离子

Determinationn of Trace Amount of Metal Ions by Reversed-Phase Ion-Pair Liquid Chromatography with Post-Column Derivatization Chemiluminescence Detection

报道了反相离子对液相色谱-柱后衍生化学发光检测方法分离测定痕量的钴(Ⅱ)、铁(Ⅱ)、铜(Ⅱ)、铁(Ⅲ)及铬(Ⅲ).利用弱络合性的乳酸作为淋洗剂,加入适量的十二烷基磷酸钠作对离子试剂,研究了分离条件、发光条件及二者的匹配方式等因素对分离检测的影响.测定线性范围分别为(g/mL):Cr(Ⅲ)5.0×10^(-9)～1.0×10^(-5);Fe(Ⅱ)2.0×10^(-9)～1.0×10^(-5);Fe(Ⅲ〕8.0×10^(-9)～1.0×10^(-5);Cu(Ⅱ)8.0×10^(-11)～1.0×10^(-5)及Co(Ⅲ)1.0×10^(-11)～1.0×10^(-5).检出限分别为:10pg Cr(Ⅲ),0.4pg Fe(Ⅱ),20pg Fe(Ⅲ),1.0pg Cu(Ⅱ)及0.01 pg Co(Ⅱ).

The separation and determination of Cr( Ⅲ ), Fe( Ⅱ ) , Fe( Ⅲ), Cu( Ⅱ ) , and Co( Ⅱ ) were demonstrated by reversed-phase ion-pair liquid chromatography with chemiluminescence detection. A reversed-phase column (YWQ-C18, 10 μm, 150×4. 0 mm i. d. ) was used. The ion-pair ion was sodium dodecyl sulfate (SDS) and the eluent was lactic acid. The Chemiluminescence system used was luminol-KOH-H2O2-Brij 35 system. The separation and detection conditions were studied. In the optimization condition the metal ions could be determined in the range from 1. 0×10-11 to 1. 0×10-5g/mL with the detection limits of 10 pg Cr( Ⅲ ), 0. 4 pg Fe ( Ⅱ ), 20 pg Fe( Ⅲ ) , 1. 0 pg of Cu( Ⅱ ), and 0. 01 pg Co( Ⅱ ), respectively.