柑橘精油中呋喃香豆素的超高效液相色谱分析  

Determination of furocoumarines in citrus essential oil by ultra- high performance liquid chromatography

作　　者：茅富燕 庄伟强 黄健 乐之歆 胡坪[2] 

机构地区：[1]爱普香料集团股份有限公司,上海201809 [2]华东理工大学化学与分子工程学院,上海200237

出　　处：《日用化学工业》2014年第12期706-709,713,共5页China Surfactant Detergent & Cosmetics

摘　　要：建立了柑橘类精油中4种呋喃香豆素（异补骨脂素、补骨脂素、5-甲氧基补骨脂素和欧前胡素）的超高效液相色谱（UPLC）分析方法。样品经甲醇稀释定容,高速离心分离后,取上清液进样分析。采用Agilent Zorbax Eclipse Plus C18色谱柱（2.1 mm×50 mm,1.8μm）分离,以水-乙腈二元流动相梯度洗脱,流速0.3 m L·min^-1,检测波长300 nm。4种呋喃香豆素在0.5～100 mg·L^-1范围内呈良好线性,相关系数均达到0.999,检出限为1.5～3.0 mg·kg^-1,平均回收率为97.5%～105.6%,相对标准偏差为0.4%～2.9%（n=3）。采用已建立的方法对25批柑橘类精油样品进行测定,发现1个批次的甜圆柚油中含有5-甲氧基补骨脂素,质量分数为60.5 mg·kg^-1。An analysis method was established to determine four kinds of furocoumarines（ isopsoralen,psoralen,5- methoxy- psoralen and imperatorin） in citrus essential oil by ultra- high performance liquid chromatography（ UPLC） with a diode array detector（ DAD）. The essential oil sample was diluted with methanol. After centrifugal separation,the supernatant was directly analyzed by UPLC. The separation was performed on an Agilent Zorbax Eclipse Plus C18column（ 2. 1 mm × 50 mm,1. 8 μm）,with water-acetonitrile as the mobile phase in gradient elution mode at a flow rate of 0. 3 m L · min^-1. The detection wavelength was 300 nm. The results indicated that good linearity is obtained in the mass concentration range of0. 5- 100 mg · L^-1 with all correlation coefficients of 0. 999 for the four kinds of furocoumarines. The detection limits are 1. 5- 3. 0 mg·kg^-1. The recoveries at three spiked levels of four kinds of furocoumarines are ranged within 97. 5%- 105. 6%,with the relative standard deviations of 0. 4%- 2. 9%（ n = 3）.Furthermore,25 batches of citrus essential oil samples were determined using the established method and a batch of grapefruit oil was found containing 60. 5 mg·kg^-1 of 5- methoxy- psoralen.

关 键 词：柑橘精油 超高效液相色谱 异补骨脂素 补骨脂素 5-甲氧基补骨脂素 欧前胡素 

分 类 号：TQ651.2[化学工程—精细化工] O657.72[理学—分析化学]