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采用硝基苯胲铵盐(铜铁试剂)、吡咯烷基二硫代甲酸铵(APDC)为络合剂,T riton X-114为表面活性剂的浊点萃取体系分别富集药物胶囊中的痕量Cr(Ⅲ)和总铬,富集后的Cr(Ⅲ)和总铬用石墨炉原子吸收光谱法进行测定。讨论了溶液pH值、表面活性剂浓度、络合剂浓度、平衡温度、平衡时间等对浊点萃取效率的影响。在优化的实验条件下,铬(Ⅵ)的检出限为0.031Lg/L,相对标准偏差为1.2%(C=2.0Lg/L,n=6),加标回收率为98.4%—102.1%。应用该法测定药物胶囊中的痕量Cr(Ⅵ),结果令人满意。
Nitrobenzamide ammonium salt (copper and iron reagent), ammonium pyrrolidine dithiocarbamate (APDC) as complexing agent, Triton X-114 as the surfactant cloud point extraction system were enriched in drug capsules Trace Cr (Ⅲ) and total chromium, Cr (Ⅲ) after enrichment and total chromium were determined by graphite furnace atomic absorption spectrometry. The effects of pH value, surfactant concentration, complexing agent concentration, equilibrium temperature and equilibrium time on the extraction efficiency of cloud point were discussed. The detection limit of chromium (Ⅵ) was 0.031Lg / L and the relative standard deviation was 1.2% (C = 2.0Lg / L, n = 6) under optimized conditions. The recoveries were in the range of 98.4% -102.1% . The method for determination of trace Cr (Ⅵ) in pharmaceutical capsules shows satisfactory results.