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机构地区:[1]华西医科大学公共卫生学院,四川成都610041
出 处:《色谱》2000年第5期436-438,共3页Chinese Journal of Chromatography
基 金:卫生部基金!资助项目批准号 94 2 1 77
摘 要:研究了meso 四 (对羟基苯基 )卟啉为柱前衍生化试剂与Cd2 +,Pb2 +,Cu2 +和Zn2 +离子的配合反应条件及配合物在C1 8色谱柱上的分离条件 ,建立了反相高效液相色谱快速分离光度检测Cd2 +,Pb2 +,Cu2 +和Zn2 +的新方法。配合物和试剂在 1 5min内出峰完毕。 4种离子的检出限为 :Cd2 +0 0 2ng ,Pb2 +0 0 2ng ,Cu2 +0 0 2ng ,Zn2 +0 1 2ng ;线性范围为 :Cd2 +0 8μg/L~ 1 50 μg/L ,Pb2 +0 8μg/L~ 30 0 μg/L ,Cu2 +0 8μg/L~ 50 0 μg/L ,Zn2 +5 0 μg/L~ 1 0 0 0 μg/L ;方法的日内相对标准偏差为 :2 8%~ 4 8%,测定低、中、高 3个浓度的日间相对标准偏差为 3 7%~ 9 7%。HPLC was used in the investigation of the reaction behavior of Cd\+\{2+\}, Pb\+\{2+\}, Cu\+\{2+\} and Zn\+\{2+\} with meso tetrakis (4 hydroxy phenyl)porphine (THPP) and chromatographic behavior of their complexes The reaction and chromatographic separation parameters were optimized and a method for the simultaneous determination of Cd\+\{2+\}, Pb\+\{2+\}, Cu\+\{2+\} and Zn\+\{2+\} by reversed phase high performance liquid chromatography with THPP as pre column derivatization reagent was established The metal THPP complexes formed in 0 1 mol/L borate buffer (pH 10 5) by heating in 60 ℃ water bath for 20 min and were extracted into ethyl acetate benzene mixture The metal THPP complexes and THPP were separated on a Prodigy ODS, 5 μm, 250 mm×4.6 mm i.d. column with methanol 0 05 mol/L borate buffer(90∶10,V/V) (pH 8 0) as eluent and detected at 437 nm (Cd 2+ and Zn 2+ ), 465 nm (Pb 2+ ) and 416 nm (Cu 2+ ) The detection limits of the four metal ions in 5 μL injection solution were Cd 2+ \{0 02\} ng, Pb 2+ \{0 02\} ng, Cu 2+ \{0 02\} ng,and Zn 2+ \{0 12\} ng, and the linear ranges were Cd 2+ 8 ng 1 5 μg, Pb 2+ 8 ng 3 0 μg, Cu 2+ 8 ng 5 0 μg, and Zn 2+ 50 ng 10 μg in 10 mL reaction solution The intra day repeatability (as RSDs) was in the range of 2 8% 4 8% and the inter day reproducibility was in the range of 3 7% 9 7%
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