[关键词]
[摘要]
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 mL,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。
[Key word]
[Abstract]
Objective To study on the scavenging rules and optimum processing condition of heavy metals Pb, Cd, Hg, and Cu removal in Acanthopanax senticosus extract (ASE) with alkyl thiourea functionalized silica (ATFS). Methods ASE was simulated as study object of excessive harmful elements Pb, Cd, Hg, and Cu.The scavenging mass, scavenging time, shaking speed and scavenging temperature were investigated by static scavenging way and the diameter ratio, sample solution, washing speed and washing temperature were investigated by dynamic scavenging way influence to metal removal rate. The best process of static and dynamic was chosen by orthogonal experiment; Eleutheroside B and eleutheroside E were as the effective constituents in ASE, solid contents and HPLC fingerprint similarity were as investigated index, the change of chemical composition in ASE to heavy metals removal from aqueous solution before and after treatment was evaluated. Results Compared with unmodified silica gel (SG), static absorption and dynamic absorption had a high removal rate of heavy metals, the scavenging speed was relative fast, the best static scavenging process of harmful elements in ASE were: The ratio of TCME mass and adsorbent was 80:1, shaking speed was 260 times/min, scavenging time was 600 min, scavenging temperature was 45 ℃; The best dynamic scavenging process: Diameter ratio was 1:20, sample volume was 100 mL, washing speed was 3 BV/h, washing temperature was 15 ℃; The change rate of eleutheroside B and eleutheroside E before and after heavy metal elements in ASE dislodged were less than 2.00%, loss ratio of solid contents was 0.18%, fingerprint similarity was more than 99.9%. Conclusion The method can be used to satisfy the high efficiency of selective removal of harmful elements in ASE and the effective composition of almost no effect, the method is simple and easy, so it can be recommended for pretreatment of harmful elements in traditional Chinese medicine extracts and this way provides a new thought and research technique to decrease the contents of harmful elements.
[中图分类号]
[基金项目]
贵州省中医药管理局项目(QZYY-2015-081)