萃淋树脂微色谱柱分离富集-苯基荧光酮光度法测定中草药中痕量锗和钼

Spectrophotometric Determination of Trace Germanium and Molybdenum in Chinese Herbal Medicine after Continuous Enrichment and Separation Using the Micr-column Packed with Extraction-elution Resin

研究了在微色谱柱中以CL—TBP萃淋树脂为固定相，运用零空床体积洗脱技术，反相萃取分离痕量Ge、Mo。洗脱体积仅1．0～1．2mL便可实现两元素的连续分离。洗脱液用苯基荧光酮-溴化十六烷基三甲基溴化铵（PF-CTMAB）光度法进行测定。该树脂对Ge、Mo的动态吸附容量分别为34．8mg／g和67．4mg／g，加标回收率分别为91．4％～98．6％和96．6％～101.3％，相对标准偏差（RSD）分别在2．53％～5．74％和1．91％～4．12％之间。方法用于中草药中痕量Ge、Mo的测定，结果满意。

In the decompressed microchromatographic column packed with tributyl phosphate （TBP） extraction-eluting resin as the stationary phase under negative pressure, Ge and Mo can be separated using reversed-phase extraction chromatography by the eluting-technology of zero dead volume. Ge and Mo were eluted continually with Qnly about 1 mL eluting-liquids, respectively. The eluted samples were determined with PF-CTMAB spectrophotometry. The saturated adsorption capacities of Ge and Mo on the resin reached 34. 8 mg/g and 67. 4 mg/g. The recoveries were 91. 4%～98. 6% and 96. 6%～101.3%, and the RSDs were 2. 53%～5. 74% and 1.91%～4.12%, respectively. The method has been successfully applied to the determination of trace Ge and Mo in Chinese herbal medicine.