中空纤维膜液相微萃取-超高效液相色谱测定蒙药毛勒日-达布斯-4汤中两种生物碱  

Determination of two alkaloids in Mongolian medicine Mauleri-Dabusi-4 soup by hollow fiber liquid phase micro-extraction coupled with ultra-high performance liquid chromatography

作　　者：宝贵荣[1,2] 孟和[3] 李优鑫[2] 包建民[2] BAO Guirong;MENG He;LI Youxin;BAO James Jianmin(Department of Biochemistry Engineering, Hohhot Vocational College, Hohhot 010051, China;School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072, China;College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, China)

机构地区：[1]呼和浩特职业学院生物化学工程学院,内蒙古呼和浩特010051 [2]天津大学药物科学与技术学院,天津300072 [3]内蒙古大学化学化工学院,内蒙古呼和浩特010021

出　　处：《色谱》2019年第6期644-648,共5页Chinese Journal of Chromatography

基　　金：内蒙古自然科学基金项目(2018MS02007)~~

摘　　要：建立了将中空纤维膜液相微萃取(HF-LPME)技术与超高效液相色谱(UPLC)技术联用检测蒙药毛勒日-达布斯-4汤中2种生物碱(胡椒碱和荜茇宁)的分析方法。通过考察该HF-LPME方法的影响参数,优化了萃取实验条件。HF-LPME优化条件如下:空隙率大于50%的偏氟乙烯中空纤维膜,萃取溶剂为正辛醇,氯化钠质量浓度为10 g/L,室温振荡,振荡速度为173 r/min ,萃取时间为128 min。结果表明:该HF-LPME-UPLC方法对胡椒碱和荜菝宁的检出限(LOD)分别为2.2和2.5 μg/L ,相对标准偏差不大于7.8%( n =5)。胡椒碱和荜菝宁分别在100~ 8 500 和8.3~ 5 000 μg/L 范围内具有良好的线性关系,胡椒碱和荜茇宁的富集倍数分别为59和65。该方法简便、快速、准确、环保,适用于蒙药中胡椒碱和荜菝宁含量的测定。In this study, a method combining hollow fiber liquid phase micro-extraction (HF-LPME) and ultra-high performance liquid chromatography (UPLC) was developed for the determination of two alkaloids (piperine and piperlonguminine) in Mongolian medicine Mauleri-Dabusi-4 Soup. The parameters affecting the micro-extraction efficiency were evaluated and optimized . The optimum conditions were as follows: polyvinylidence fluoride HF (54% pore size);10 g/L NaCl;30 μL octanol as extraction solvent;173 r/min stirring rate of extraction;and 128 min extraction time. The extracted drug was detected by UPLC. The calibration curves obtained good linear relationship in the concentration ranges of 100- 8 500 and 8.3- 5 000 μg/L for piperine and piperlonguminine, respectively. The enrichment factors of the method for piperine and piperlonguminine were achieved to be 59 and 65. The limits of detection were 2.2 μg/L for piperine and 2.5 μg/L for piperlonguminine. The method was successfully applied for the determination of alkaloids in Mongolian medicine Mauleri-Dabusi-4.

关 键 词：中空纤维膜液相微萃取 超高效液相色谱 生物碱 毛勒日达布斯 4 蒙药 

分 类 号：O658[理学—分析化学]