摘要
[目的]优化并构建水包油包水(W/O/W)型乳状液膜体系,为有效分离富集烟草提取物中的高浓度烟碱及其开发利用提供参考依据.[方法]以降烟碱为模板分子,通过单因素试验对外水相pH、表面活性剂种类及用量、膜载体种类及用量、油内比、内水相HC1浓度、迁移时间及乳水比进行优化,在此基础上对外水相pH、膜载体D2EHPA用量、表面活性剂T154用量和内水相HC1浓度开展4因素5水平的正交试验筛选,采用紫外可见分光光度法和高效液相色谱法评价乳状液膜体系对烟草提取物中烟碱的分离效能,以此确定乳状液膜体系的最佳条件.[结果]正交试验中,4个因素对乳状液膜体系的萃取率影响排序:外水相pH=表面活性剂T154用量＞膜载体D2EHPA用量＞内水相HC1浓度.通过比较单因素试验和正交试验优化的乳状液膜分离体系对降烟碱的分离富集效率,确定单因素试验优化获得的乳状液膜体系条件最佳:表面活性剂为3％T154,膜载体为3％仲辛醇和5％D2EHPA,内水相为0.5 mol/L HC1,外水相pH为13,油内比10:8,乳水比2:25,迁移时间2.5 min;在该条件下,乳状液膜体系对0.05 mg/mL烟碱和降烟碱的萃取率分别达85.07％和91.42％,对烟草提取物中烟碱成分的分离富集效率可达74.80％,且分离所得样品中烟碱浓度为原样的2.17倍.[结论]优化所得乳状液膜体系能快速有效地分离富集烟草提取物中的高浓度烟碱,表现出较好的应用潜力.
Abstract
[Objective]To optimize and construct a water-in-oil-in-water(W/O/W)type emulsion liquid membrane system for the effective separation and enrichment of high-concentration nicotine in tobacco extracts,providing reference for its development and utilization.[Method]Using nicotine as a template molecule,single-factor experiments were con-ducted to optimize the pH of the external aqueous phase,types and amounts of surfactants,types and amounts of mem-brane carriers,ratio of oil phase to internal aqueous phase,HC1 concentration of internal aqueous phase,transfer time,and ratio of emulsion phase to external aqueous phase.Subsequently,a four-factor and five-level orthogonal test was per-formed on the pH of the external aqueous phase,the amount of membrane carrier D2EHPA,the amount of surfactant T154,and HC1 concentration of internal aqueous phase.The separation efficiency of the emulsion liquid membrane sys-tem for nicotine in tobacco extracts was evaluated using ultraviolet-visible spectroscopy and high-performance liquid chro-matography(HPLC)to determine the optimal conditions of the emulsion liquid membrane system.[Result]In the or-thogonal test,the influence of the 4 factors on the extraction rate of the emulsion liquid membrane system was ranked as follows:pH of external aqueous phase=amount of surfactant T154＞amount of membrane carrier D2EHPA＞HCl con-centration of internal aqueous phase.By comparing the separation and enrichment efficiencies of the emulsion liquid mem-brane system optimized by single-factor and orthogonal tests,the optimal conditions obtained from the single-factor test were determined to be:3％T154 as surfactant,3％sec-octanol and 5％D2EHPA as membrane carriers,0.5 mol/L HCl in the internal aqueous phase,pH 13 in the external aqueous phase,ratio of oil phase to internal aqueous phase of 10:8,ra-tio of emulsion phase to external aqueous phase of 2:25,and transfer time of 2.5 min.Under these conditions,the extrac-tion rates for 0.05 mg/mL nicotine and nornicotine reached 85.07％and 91.42％respectively by emulsion liquid membrane system,and the separation and enrichment efficiency for nicotine components in tobacco extracts reached 74.80％,with the nicotine concentration in the separated sample being as 2.17 times as that of the original sample.[Conclusion]The op-timized emulsion liquid membrane system can rapidly and effectively separate and enrich high-concentration nicotine from tobacco extracts,showing good potential for application.
维普
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