摘要
针对6份不同品种的柚子皮,采用甲醇超声提取,Oasis HLB固相萃取柱净化,Waters XBrigde C18色谱柱分离,以乙腈和0.05 mol/L乙酸铵溶液(含0.1 %甲酸)为流动相进行梯度洗脱,采用多反应监测(multiple reaction monitoring, MRM)检测,建立液相色谱-质谱法(liquid chromatography-mass spectrometry, LC-MS/MS)测定柚子皮中香豆素类物质组成及含量的检测方法。结果表明:在0.010 μg/mL^1.0 μg/mL范围内,8种香豆素及其衍生物具有良好的线性关系(R2≥0.999 5);方法检出限在3.0 μg/kg^4.5 μg/kg,定量限在10.0 μg/kg^15.0 μg/kg;加标回收率在90.4 %~98.5 %,相对标准偏差在0.9 %~4.1 %;在柚子皮中检出7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4-甲基香豆素、醋硝香豆素,其中7-甲氧基香豆素含量较高,含量在11.4 μg/kg^123.7 μg/kg,该成分可能与柚子具有暖胃、化痰、润化喉咙等食疗作用相关,这为柚子皮综合开发利用提供参考。
Liquid chromatography-mass spectrometry (LC-MS/MS) was established to determine the composition and content of coumarins in 6 different varieties of grapefruit skin of Citrus maxima, by ultrasonic extraction with methanol, and Oasis HLB solid phase extraction column purification with Waters XBrigde C18 column separation, and gradient with acetonitrile and 0.05 mol/L ammonium acetate solution (containing 0.1 % formic acid) as mobile phase elution, and detected by multiple reaction monitoring (MRM). The results showed that 8 coumarins and their derivatives had a good linear relationship (R2≥0.999 5) in the range of 0.010 μg/mL to 1.0 μg/mL. The detection limit of the method was from 3.0 μg/kg to 4.5 μg/kg, and the limit of quantification was from 10.0 μg/kg to 15.0 μg/kg;the recoveries were from 90.4 % to 98.5 %, and the relative standard deviations were from 0.9 % to 4.1 %. 7-methylcoumarin, 7-methoxycoumarin, 7-ethoxy-4-methylcoumarin, acenocoumarol were detected in grapefruit skin of Citrus maxima. Among them, the content of 7-methoxyc-oumarin was relatively high, and the content was 11.4 μg/kg -123.7 μg/kg. This ingredient may be related to the therapeutic effect of grapefruit with warm stomach, phlegm and moisturizing throat, which provides compr-ehensive development and utilization of grapefruit skin of Citrus maxima.
作者
郝元元
HAO Yuan-yuan(Ulanqab Vocational College , Ulanqab 012000, Inner Mongolia, China)
出处
《食品研究与开发》
CAS
北大核心
2019年第16期146-152,共7页
Food Research and Development
关键词
液相色谱-质谱法
柚子皮
香豆素
衍生物
测定
liquid chromatography-mass spectrometry
grapefruit skin of Citrus maxima
coumarin
derivative
determination
