色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
8期
792-798
,共7页
李桂珍%唐为扬%曹伟敏%王倩%朱涛
李桂珍%唐為颺%曹偉敏%王倩%硃濤
리계진%당위양%조위민%왕천%주도
固相萃取法%低共熔溶剂%印迹分子聚合物%咖啡酸%山楂
固相萃取法%低共鎔溶劑%印跡分子聚閤物%咖啡痠%山楂
고상췌취법%저공용용제%인적분자취합물%가배산%산사
solid-phase extraction( SPE)%deep eutectic solvents%molecularly imprinted polymers( MIPs)%caffeic acid%hawthorn
在相同的实验条件下,分别合成了以咖啡酸为模板的印迹分子聚合物和无模板分子聚合物。使用场发射扫描电镜法和吸附实验表征这两种聚合物材料的孔状结构和选择性吸附性能。然后利用印迹分子聚合物、无模板分子聚合物、C18萃取小柱这3种材料结合固相萃取法纯化山楂提取物中的咖啡酸,提取率分别为3.46、1.01、1.17μg/g。为了优化固相萃取过程,实验研究了不同洗脱剂的影响。分别利用用氯化胆碱和甘油、氯化胆碱和尿素(摩尔比均为1:2)合成出两种低共熔溶剂。甲醇与这两种低共熔溶剂分别以不同的体积比混合作为洗脱剂,用于优化咖啡酸的固相萃取过程。实验结果表明,印迹分子聚合物是一种良好的固相萃取材料;当甲醇和甘油基低共熔溶剂在体积比为3:1混合时,表现出最好的洗脱能力,得到咖啡酸的回收率为82.32%。
在相同的實驗條件下,分彆閤成瞭以咖啡痠為模闆的印跡分子聚閤物和無模闆分子聚閤物。使用場髮射掃描電鏡法和吸附實驗錶徵這兩種聚閤物材料的孔狀結構和選擇性吸附性能。然後利用印跡分子聚閤物、無模闆分子聚閤物、C18萃取小柱這3種材料結閤固相萃取法純化山楂提取物中的咖啡痠,提取率分彆為3.46、1.01、1.17μg/g。為瞭優化固相萃取過程,實驗研究瞭不同洗脫劑的影響。分彆利用用氯化膽堿和甘油、氯化膽堿和尿素(摩爾比均為1:2)閤成齣兩種低共鎔溶劑。甲醇與這兩種低共鎔溶劑分彆以不同的體積比混閤作為洗脫劑,用于優化咖啡痠的固相萃取過程。實驗結果錶明,印跡分子聚閤物是一種良好的固相萃取材料;噹甲醇和甘油基低共鎔溶劑在體積比為3:1混閤時,錶現齣最好的洗脫能力,得到咖啡痠的迴收率為82.32%。
재상동적실험조건하,분별합성료이가배산위모판적인적분자취합물화무모판분자취합물。사용장발사소묘전경법화흡부실험표정저량충취합물재료적공상결구화선택성흡부성능。연후이용인적분자취합물、무모판분자취합물、C18췌취소주저3충재료결합고상췌취법순화산사제취물중적가배산,제취솔분별위3.46、1.01、1.17μg/g。위료우화고상췌취과정,실험연구료불동세탈제적영향。분별이용용록화담감화감유、록화담감화뇨소(마이비균위1:2)합성출량충저공용용제。갑순여저량충저공용용제분별이불동적체적비혼합작위세탈제,용우우화가배산적고상췌취과정。실험결과표명,인적분자취합물시일충량호적고상췌취재료;당갑순화감유기저공용용제재체적비위3:1혼합시,표현출최호적세탈능력,득도가배산적회수솔위82.32%。
Molecularly imprinted polymers( MIPs)with caffeic acid as template and non-imprinted polymers (NIPs)materials were prepared in the same procedure. Field emission scanning electron microscopy( FE-SEM)and adsorption capacity test were used to evaluate characteristic of the new materials. MIPs,NIPs and C18 were used for rapid purification of caffeic acid from hawthorn with solid-phase extraction( SPE),and extract yields of caffeic acid with the proposed materials were 3. 46 μg/g,1. 01 μg/g and 1. 17 μg/g,respec-tively. To optimize the MIPs-SPE procedures,different kinds of elution solutions were studied. Deep eutectic solvents( DESs)were prepared by choline chloride( ChCl)-glycerol( 1/2,n/n)and choline chloride-urea( 1/2,n/n). Methanol was mixed with the two kinds of DESs( glycerol-based DESs,urea-based DESs)in different ratios(0. 5:1,1:1,2:1,3:1,4:1,5:1,v/v),and they were used to investigated as elution solutions in the above MIPs-SPE procedures. The results showed that MIPs were potential SPE materials, and methanol/glycerol-based DESs( 3:1,v/v)had the best elution capability with the recovery of 82. 32%.