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2.5μg/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 000μg/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.
引文
[1] Bai Y X,Bao G H,Liao Ning Journal of Traditional Chinese Medicine,2007,34(1):1132 白玉霞,包桂花,辽宁中医杂志,2007,34(1):1132
[2] Bai C J,Li J W,Wang L J,et al.Chinese Pharmaceutical Affairs,2003,17(4):234 白春洁,李敬伟,王丽君,等.中国药事,2003,17(4):234
[3] Hu M Z,Lian X H,Liu H,et al.Chinese Journal of Chromatography,2017,35(11):1145 胡明珠,连显会,刘晗,等.色谱,2017,35(11):1145
[4] Feng J J,Sun M,Bu Y N,et al.Anal Bioanal Chem,2016,408:1679
[5] Asadi M,Dadfarnia S,Shabani A M H,et al.Food Anal Methods,2016,9:2762
[6] Wang K,Li N,Lei L,et al.Anal Bioanal Chem,2016,408:3359
[7] Saraji M,Maleki B,Khayamian T,et al.Chromatographia,2017,80:951
[8] Ghiasvand A R,Heidari N.Chromatographia,2016,79:1187
[9] Barahona F,Gjelstad A,Pedersen-Bjergaard S,et al.J Chromatogr A,2010,1217:1989
[10] Zhou B,Huang D S,Xu S J,et al.Adv Mater Res,2014,830:319