作　　者： ; ; ; ; ;

机构地区： 淮阴工学院

出　　处： 《光谱实验室》 2011年第5期2708-2712,共5页

摘　　要： 建立了用离子印迹壳聚糖/凹凸棒石(MICA)分离富集-火焰原子吸收光谱法(FAAS)测定中药中痕量铅的新方法。在动态吸附条件下,系统地研究了溶液pH值、流速、洗脱条件和干扰离子对痕量铅分离富集的影响;在pH 4.5,上样流速为0.60mL/min的条件下,铅能被MICA定量富集;吸附的铅可用1.0mol/L HCl-0.1mol/L甲基异丁酮的乙醇溶液在流速为0.96mL/min条件下完全洗脱;优化条件下,MICA对铅的动态吸附容量为36.78mg/g。线性范围为0—1.28mg/L,r=0.9997,检出限(3σ,n=11)为0.73μg/L,相对标准偏差为1.69%(n=6,ρ=0.08mg/L),回收率在97.5%—101.4%之间。该方法操作简便、线性关系良好、灵敏度和精密度高,实际中药中痕量铅的测定结果满意。 A new method for the determination of trace lead（Ⅱ） in traditional Chinese medicine by FAAS-separation and concentration with MICA was established.Under dynamic adsorbtion conditions,the effects of optimal pH of the solution,flow rate,elution conditions and interfering ion on separation and concentration of trace lead（Ⅱ） were investigated by the numbers.Lead can quantificationally gathered at pH value of 4.5 with injection velocity of 0.60 mL/min,and adsorbed lead can get entire elution by 1.0mol/L HCl-0.1mol/L methyl isobutyl ketone alcohol with flow rate of 0.96mL/min,while the dynamic adsorption capacity of MICA on lead was 36.78 mg/g under the optimal conditions.The linear range was from 0 to 1.28mg/L with correlation coefficient of 0.9997,and the detection limit was 0.73μg/L（3σ,n=11）,and recovery was between 97.5% and 101.4% with RSD of 1.69%（n=6,ρ=0.08mg/L）.The method has simple operation,good linear relationship with high sensitivity and precision,and that can be applied to the determination of trace lead（Ⅱ） in traditional Chinese medicine with satisfactory results.

关 键 词： 印迹技术 凹凸棒石黏土 壳聚糖 分离富集 火焰原子吸收光谱法 铅

领　　域： [理学] [理学]