离子液体分散液相微萃取对苯丙烯酸类化合物的浓缩及作用机制

Mechanism and Concentration of Phenylpropionic Acids by Ionic Liquid Dispersive Liquid Phase Microextraction

研究了离子液体分散液相微萃取(ILDLPME)机理,建立了简单、快速、灵敏的ILDLPME-HPLC(高效液相色谱)同时测定中药白附子中5种低丰度苯丙烯酸类化合物含量的方法,对不同产地白附子的质量进行了比较和评价.在最佳的ILDLPME-HPLC条件下,测得咖啡酸的线性范围为1.28×10-3～2.60μg/mL,对羟基桂皮酸及阿魏酸的线性范围为1.28×10-4～2.60μg/mL,桂皮酸及对甲氧基桂皮酸的线性范围为1.28×10-3～4.00μg/mL,检出限分别为0.13,0.01,0.01,0.13和0.13 ng/mL,日内精密度RSD<7.9%,日间精密度RSD<9.7%,药材中分析物的回收率在86.9%～112.6%之间,ILDLPME对5种分析物的富集倍数分别在56.0～159.3倍之间.结合5种苯丙烯酸类化合物ILDLPME萃取前后紫外光谱的变化,提出了ILD-LPME萃取苯丙烯酸羧基-离子液体电荷转移超分子(CTSMCIL)机理.本研究为建立中药白附子的质量控制方法提供了理论依据和实验基础.

The ionic liquid dispersive liquid phase microextraction（ILDLPME） was developed and its mechanism was investigated;ILDLPME coupled with high performance liquid chromatography（HPLC） was introduced for the determination and evaluation of five kinds of low abundance phenylpropionic acid compounds of Rhizoma typhonii from different origins.The main parameters affecting the performance of ILDLPME were optimized.Under the optimized parameters,the linear ranges were 1.28×10-3—2.60 μg/mL for caffeic acid,1.28×10-4—2.60 μg/mL for p-hydroxycinnamic acid and ferulic acid,1.28×10-3—4.00 μg/mL for cinnamic acid and p-methoxycinnamic acid,respectively;the limits of detection were 0.13,0.01,0.01,0.13 and 0.13 ng/mL,respectively;the intra and inter RSD were less than 9.7%,the mean recoveries of analytes in traditional Chinese medicines were between 86.9% and 112.6%,the enrichment factors were in the range of 56.0—159.3 for ILDLPME.By analysis and comparison the UV spectra of phenylpropionic acids before and after ILDLPME,the extraction mechanism of the charge transfer superamolecule of carboxyl-ionic liquid（CTSMCIL） was proposed.CTSMCIL-HPLC provide dependably theoretic foundation and experimental evidence for establishing quality control method in Rhizoma typhonii.