刘健艺,左莉华,贾欣欣,郭兴杰
LIU Jian-yi,ZUO Li-hua,JIA Xin-xin,GUO Xing-jie(School of Pharmacy

• 1:沈阳药科大学药学院

摘要(Abstract)：

目的建立了分散液相微萃取与高效液相色谱联用技术测定大鼠血浆中对香豆酸浓度。方法微萃取条件为:20μL 1-己基-3-甲基咪唑六氟磷酸盐离子液体(1-hextyl-3-methylimidazoliumhexafluorophosphate,[C6MIM][PF6])作萃取剂,80μL乙腈作分散剂,0.5 mol.L-1硫酸作酸化剂,萃取时间为1 min。结果在优化的萃取条件下,血浆中对香豆酸质量浓度在0.012～2.400 mg.L-1内,线性关系良好(相关系数r=0.997 5),日内和日间精密度(RSD%)<9%(n=6),相对回收率为96.7%～101.6%,提取回收率为59.0%～70.4%。结论该方法适于血浆中对香豆酸浓度的测定。
Objective To establish an novel method for determination of p-coumaric acid in rat plasma by dispersive liquid-liquid microextraction coupled with high performance liquid chromatography(DLLME-HPLC).Methods The optimal conditions of dispersive liquid-liquid microextraction were as follow:ionic liquids of 1-hexyl-3-methylimidazolium hexafluorophosphate20 μL as extraction solvent,acetonitrile 80 μL as dispersive solvent,0.5 mol · mL-1H2SO4 solution as acidifying agent;extraction time was 1 min.Results Under the optimized conditions,the linear range of p-coumaric acid was 0.012-2.4 μg · mL-1(r=0.997 5),the limit of detection was 0.03 ng,relative recoveries were 96.7%-101.6% with both intra-day and inter-day RSDs less than 9%,extraction recoveries were 62.9-70.4%.Conclusions The method is sensitive and fast for determination of p-coumaric acid in rat plasma,and can provide a high degree of enrichment.

关键词(KeyWords)： 分散液相微萃取;离子液体;高效液相色谱法;对香豆酸;血浆
dispersive liquid-liquid microextraction;ionic liquids;high performance liquid chromatography;p-coumaric acid;plasma

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 刘健艺,左莉华,贾欣欣,郭兴杰
LIU Jian-yi,ZUO Li-hua,JIA Xin-xin,GUO Xing-jie(School of Pharmacy

DOI: 10.14066/j.cnki.cn21-1349/r.2012.07.013

参考文献(References)：

• [1]REZAZZ M,ASSADI Y,HOSSEINI M R M,et al.De-termination of organic compounds in water using disper-sive liquid-liquid microextraction[J].J Chrom atogr A,2006(1-2):1-9.
• [2]张明勇,洪战英,范国荣.分散液相微萃取技术及其在生物样品分析中的应用进展[J].中国新药杂志,2011,20(5):429-431.
• [3]冉桂梅,何彬,姚国灿,等.白花蛇舌草注射液中对香豆酸的药代动力学研究[J].药物分析杂志,2005,25(7):759-761.
• [4]CUI Yan,LI Qing,ZHANG Ming,et al.LC-MS Deter-minnation and pharmacokinetics of p-coumaric acid inrat plasma after oral administration of p-coumaric acidand freeze-dried red wine[J].Agric Food Chem,2010,58:12083-12088.
• [5]臧晓欢,吴秋华,张美月,等.分散液相微萃取技术研究进展[J].分析化学,2009,37(2):161-168.
• [6]HADI F A,PARVIZ N A B,RASSOUL D C,et al.De-velopment of dispersive liquid-liquid microextractioncombined with gas chromatography-mass spectrometryas a simple,rapid and highly sensitive method for thedetermination of phthalate esters in water samples[J].JChromatogr A,2007,1172:105-112.
• [7]ZANG Xiao-huan,WU Qiu-hua,ZHANG Mei-yue,etal.Developments of dispersive liquid-liquid microex-traction technique[J].J Chin Anal Chem,2009,37(2):161-168.
• [8]杜甫佑,肖小华,李攻科,等.离子液体在样品预处理中的应用[J].化学通报,2007(9):647-654.
• [9]ABDOLMOHAMMAD-ZADEH H,SADEGHI G H.Anovel microextraction technique based on 1-hexylpyri-dinium hexafluorophosphate ionic liquid for the precon-centration of zinc in water and milk samples[J].Ana-lytica Chimica Acta,2009,649:211-217.
• [10]AGUILERA-HERRADOR H,LUCENA R,CARDENASS,et al.The roles of ionic liquids in sorptive microex-traction technique[J].Trends in Analytical Chemistry,2010,29(7):602-616.
• [11]YUN Chang-fan,ZHENG Liang-hu,MEI Lan-chen,etal.Ionic liquid based dispersive liquid-liquid microex-traction of aromatic amines in water samples[J].Chi-nese Chemical Letters,2008,19:985-987.
• [12]叶烨,相秉仁,项素云.单液滴微苹取技术及其在色谱分析中的应用[J].药学进展,2006,30(3):109-113.
• [13]MARIA R P,MIGUEL A B L,RUT F T,et al.Hollowfiber-based liquid phase microextraction(HF-LPME)asa new approach for the HPLC determination of fluoro-quinolones in biological and environmental matrices[J].Jouranl of Pharmaceutical and Biomedical Analy-sis,2011,55:332-341.
• [14]MARTA C V,RAFAEL L,SOLEDAD C,et al.One-step in-syringe ionic liquid-based dispersive liquid-liq-uid microextraction[J].Journal of Chromatography A,2009,1216:6459-6465.