高效液相色谱-串联质谱法测定蜂胶中咖啡酸苯乙酯

HPLC-MS/MS Determination of Phenylethyl Caffeate in Propolis

摘要: 采用高效液相色谱-串联质谱法测定蜂胶中的咖啡酸苯乙酯。蜂胶样品经甲醇超声提取。以Sepax GP-C18色谱柱为分离柱,以各含(φ) 0.5%甲酸的甲醇和5 mmol·L-1乙酸铵溶液按体积比为80比20的混合液作为流动相进行分离。采用电喷雾负离子源多反应监测模式检测。咖啡酸苯乙酯的质量浓度在0.2~500 μg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.003 g·kg-1。在0.01,0.1,1.0 g·kg-1 3个浓度水平进行加标回收试验,回收率在73.0%~98.1%之间,相对标准偏差(n=5)不大于3.5%。

Abstract: HPLC-MS/MS was applied to the determination of phenylethyl caffeate in propolis. The propolis sample was extracted ultrasonically with methanol. Sepax GP-C18 column was used as stationary phase, and a mixture of methanol and 5 mmol·L-1 NH4OAc solution, (both of which containing 0.5% by vol. of formic acid), mixed in the volumic ratio of 80 to 20 was used as mobile phase in the separation. ESI- as well as multi-reaction monitoring was adopted in MS/MS. Linear relationship between values of peak area and mass concentration of phenylethyl caffeate was kept in the range of 0.2-500 μg·L-1, with detection limit (3S/N) of 0.003 g·kg-1. Tests for recovery were made by addition of standard solutions at concentration levels of 0.01, 0.1, 1.0 g·kg-1, values of recovery found were in the range of 73.0%-98.1% with RSD′s (n=6) no more than 3.5%.