分散液相微萃取-HPLC法用于大鼠血浆中对香豆酸测定

Determination of p-coumaric acid in rat plasma by dispersive liquid-liquid microextraction-HPLC

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.