【摘要】 建立了超声提取-固相萃取纯化/正相高效液相色谱测定大豆及大豆油中磷脂酰胆碱(PC)、磷脂酰乙醇胺(PE)、磷脂酰肌醇(PI)的方法。考察了提取溶剂、超声功率、超声时间、提取温度及净化方式的影响,并研究了不同色谱固定相对磷酸甘油酯分离效果的影响。优化的实验条件为:以氯仿-甲醇(2∶1,体积比)为提取溶剂,1 500 W功率超声提取30 min;氨基固相萃取柱为纯化小柱;正己烷-异丙醇-1%HAc(8∶8∶1,体积比)为流动相。在该条件下,PC、PE、PI的线性范围分别为0.08～8.00、0.15～15.00、0.30～20.00 g.L-1,定量下限分别为0.021、0.050、0.060 g.L-1,检出限在8～23 mg.L-1之间,其在大豆和大豆油中的回收率为85%～108%。日内与日间精密度分别不大于4.7%和8.6%。更多还原

【Abstract】 A normal high performance liquid chromatography with UV detection was developed for the determination of phosphatidyl cholines(PC),phosphatidyl ethanolamines(PE) and phosphatidyl inositol(PI) in soybean and soybean oil samples.Effects of extraction solvent,ultrasonic power,ultrasonic time,extracting temperature and purification method on the extraction efficiency were investigated.Effects of different stationary phases on the separation efficiency were studied.The optimal extraction conditions were as follows:extraction solvent:chloroform-methanol(2 ∶ 1,by volume);ultrasonic extraction power:1 500 W;extraction time:30 min.The purification and separation of three phospholipid compounds were performed on an amine solid phase extraction column and a silica gel column with a mobile phase of hexane-isopropanol-1% HAc solution(8 ∶ 8 ∶ 1,by volume).Under the optimized conditions,the linear ranges for the PC,PE and PI were in the range of 0.08-8.00,0.15-15.00,0.30-20.00 g·L-1,respectively.The limits of quantitation for the PC,PE and PI were 0.021,0.050,0.060 g·L-1,respectively,and the limits of detection were in the range of 8-23 mg·L-1.The recoveries of three phospholipids in fortified soybean and soybean oil sample ranged from 85% to 108%.The intra-day RSDs and inter-day RSDs of three phospholipid compounds were no more than 4.7% and 8.6%,respectively.更多还原