分析测试学报2011,Vol.30Issue(6):618-623,6.DOI:10.3969/j.issn.1004-4957.2001.06.005
液-液微萃取/高效液相色谱-质谱测定五指毛桃水提取液中的补骨脂素与佛手内酯
Determination of Psoralen and Bergapten in Radix fici hirtae by Liquid - Liquid Microextraction Coupled with Liquid Chromatography- Mass Spectrometry
摘要
Abstract
A high performance liquid chromatography coupled with electro-spray ionization-tandem mass spectrometric ( HPLC - ESI MSn ) method was developed for the simultaneous determination of psoralen and bergapten in aqueous extraction from Radix fici hirtae. The separation of psoralen and bergapten was performed on a Hypersil C1s column( 150 mm ×4. 6 mm, 5 μm), using water - methanol (50: 50)as mobile phase at a flow rate of 0. 80 mL · min- 1 The detection was carried out at room temperature with a detection wavelength of 300 nm(PDA) and an injection volume of 10 μL. The influencing factors for liquid - liquid microextraction ( LLME ) were investigated. Under the optimized conditions, the calibration curves were linear in the range of 0. 55 -2 200 μg · L-1 for psoralen and 1.00 - 4 000 μg · L - 1 for bergapten, with correlation coefficients of 0. 999 9 and 0. 999 2, respectively. The limits of detection(S/N=3) were 0. 13 lμg · L-1 and 0. 18 μg · L-1, and the limits of quantitation(S/N= 10) were 0. 43 μg · L-1 and 0. 60 μg · L-1 , respectively. The relative standard deviations(RSDs, n =5) of 110 μg · L-1 psoralen and 100 μg · L-1 bergapten were both less than 1%. The recoveries of psoralen and bergapten were 100% and 101% , respectively. The results demonstrated that LLME combined with LC - MS was a rapid, convenient and efficient method for the determination of herbal compositions, and could provide the basis for the quantitation detection of psoralen and bergapten in aqueous sample from Radix fici hirtae.关键词
五指毛桃/液-液微萃取/高效液相色谱-质谱/补骨脂素/佛手内酯Key words
Radix fici hirtae/ liquid - liquid microextraction ( LLME )/ high performance liquid chromatography - mass spectrometry( HPLC - MS)/ psoralen/ bergapten分类
化学化工引用本文复制引用
陶敬奇,闻莹莹,王辉,王三永,陈洪伟..液-液微萃取/高效液相色谱-质谱测定五指毛桃水提取液中的补骨脂素与佛手内酯[J].分析测试学报,2011,30(6):618-623,6.基金项目
广东省食品工业研究所开放实验室项目资助(FIPL-07-006) (FIPL-07-006)