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目的研究烷基硫脲功能化硅胶(alkyl thiourea functionalised silica,ATFS)去除刺五加提取物(Acanthopanax senticosus extract,ASE)中重金属Pb、Cd、Hg、Cu的吸附规律和最佳工艺。方法以ASE(单方药材)模拟重金属元素Pb、Cd、Hg、Cu超标作为研究对象,通过静态吸附方式考察吸附剂用量、吸附时间、振荡频率和吸附温度对脱除率的影响,通过动态吸附方式考察径高比、上样量、洗脱体积流量和洗脱温度对脱除率的影响,分别通过正交试验优选动、静态最佳吸附工艺;以ASE中指标成分刺五加苷B和刺五加苷E量、药液含固量和HPLC指纹图谱相似度作为考察指标,评价ASE脱除重金属前后化学成分的变化情况。结果与空白硅胶比,ATFS静态吸附和动态吸附均具有较高的重金属脱除率,且静态吸附速度较快,最佳静态吸附工艺条件:药材量与吸附剂量之比为80∶1,振荡频率为260次/min,吸附时间为600 min,吸附温度为45℃;最佳动态吸附工艺条件:径高比为1∶20,上样量为100 m L,洗脱体积流量为3 BV/h,洗脱温度为15℃;重金属元素脱除前后刺五加中指标成分刺五加苷B和刺五加苷E变化率均小于2.00%;含固量损失率为0.18%;指纹图谱相似度达99.9%以上。结论该方法可以满足选择性地高效脱除ASE中重金属元素,且对有效成分几乎无影响,操作简便、易行,可被推荐用于中药提取物中重金属元素超标时的前处理,为降低中药提取物中重金属元素量开辟了一条新的思路和研究方法。
Objective To study the adsorption and removal of heavy metals Pb, Cd, Hg and Cu in Acanthopanax senticosus extract (ASE) by alkyl thiourea functionalised silica (ATFS). Methods ASE (unilateral medicine) was used to simulate the excessive Pb, Cd, Hg and Cu in the heavy metals. The influence of the amount of adsorbent, adsorption time, oscillation frequency and adsorption temperature on the removal rate was investigated by static adsorption method. The effects of the ratio of height and diameter, sample volume, elution volume flow rate and elution temperature on the removal rate were investigated. The optimal adsorption process was optimized by orthogonal test. The content of pentagluctin E, the solid content of liquid and the similarity of HPLC fingerprints were used as indexes to evaluate the changes of chemical components before and after ASE removal of heavy metals. Results Compared with blank silica gel, both static adsorption and dynamic adsorption of ATFS have higher removal rates of heavy metals and faster static adsorption rate. The optimal static adsorption conditions are as follows: the ratio of the amount of drug to the adsorbent is 80: 1, the oscillation frequency Was 260 times / min, the adsorption time was 600 min and the adsorption temperature was 45 ℃. The optimum conditions for dynamic adsorption were as follows: the aspect ratio was 1:20, the sample volume was 100 mL, the elution volume flow rate was 3 BV / h , And the elution temperature was 15 ℃. The change rates of acanthopanax B and acanthopanax E in the acanthopanax senticosus before and after the removal of heavy metal elements were all less than 2.00%, and the loss rate of solid was 0.18%. The fingerprint similarity Up to 99.9%. Conclusion This method can meet the selective and efficient removal of heavy metal elements in ASE with little effect on the active ingredients. It is simple and easy to operate and can be recommended for the pretreatment of heavy metal elements in Chinese herbal extracts. The amount of heavy metal elements in the extract has opened up a new way of thinking and research methods.