摘要
用二甲酚橙作柱前衍生试剂 ,在C18色谱柱上 ,以乙腈 水 (12∶88)作流动相 ,六次甲基四胺为对离子试剂 ,反相离子对高效液相色谱法快速分离测定人发中痕量锌和铜。配合物和试剂在8min内出峰完毕 ,于波长 5 75nm处检测 ,检出限分别为Zn2 + 0 .0 1ng·ml- 1,Cu2 + 1.3 0ng·ml- 1。用于人发样品中锌和铜的测定 ,结果满意。
Complexes of zinc (Ⅱ) and copper (Ⅱ) with xylenol orange (XO) can be separated and determined by the reverse phase, ionpair HPLC method. Micro amounts of zinc (Ⅱ) and copper(Ⅱ) are reacted with XO in a hexamine buffer solution of pH 5.4, and the volume of the sample solution is made up to 10ml. Twenty μl of sample solution is injected into the chromatograph, ZnOX - and CuOX - ions are separated on the Novapak C 18 column. A solution of acetonitrile and water in the ratio of 12 to 88 by volume, containing 28.5mmol·L -1 of hexamine (pH 5.4) as ion pairing reagent, is used as the mobile phase. The separation is completed within 8min. Photometric detection is made at 575nm. The detection limits for zinc (Ⅱ) and copper (Ⅱ) are found to be 0.01ng·ml -1 and 1.3ng·ml -1 respectively. The proposed method has been applied to the determination of trace amounts of zinc and copper in human hair, giving RSD′s of 1.0% (for Cu) and 1.2% (for Zn), and average recoveries of 96.7% (for Cu) and 104.7% (for Zn).
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2001年第9期403-404,408,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)