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

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1.0~1.2 mL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34.8 mg/g和67.4 mg/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。

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

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 only 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.