超高效液相色谱法测定柑橘类水果干片中的3种呋喃香豆素  

Determination of 3 kinds of furanocoumarins in dried citrus slices by ultra performance liquid chromatography

作　　者：李兵[1] 戚燕 范赛[1] 陈东[1] 赵榕[1] LI Bing;QI Yan;FAN Sai;CHEN Dong;ZHAO Rong(Beijing Center for Disease Control and Prevention,Beijing 100013,China)

机构地区：[1]北京市疾病预防控制中心,北京100013

出　　处：《食品安全质量检测学报》2025年第9期216-222,共7页Journal of Food Safety and Quality

基　　金：中国食物成分监测项目(2020-609)。

摘　　要：目的 建立超高效液相色谱-二极管阵列检测器法同时测定柑橘类水果干片中的3种呋喃香豆素。方法 试样经粉碎后分两次采用40m L乙酸乙酯超声提取40min,再采用20m L乙酸乙酯分两次涡旋10min提取残渣,合并提取液,30°C旋蒸至干。采用Acquity UPLC HSS C18 SB色谱柱(2.1 mm×150 mm,1.8μm)分离,流速为0.3 mL/min,柱温30℃,检测波长为310 nm。流动相A为水和乙腈,梯度洗脱。结果 3种呋喃香豆素6’,7’-二羟基佛手素、环氧佛手柑素、佛手柑素分别在3.00~300.00μg/mL、4.32~432.00μg/mL、4.12~412.00μg/mL范围内具有良好的线性关系,相关系数大于0.999。检出限为0.09~0.17μg/g,定量限为0.31~0.57μg/g。在3个加标水平下,呋喃香豆素的平均回收率分别为94.4%~99.1%,相对标准偏差为2.7%~4.7%(n=6)。该方法能够使柑橘类水果干片中的3种呋喃香豆素在25min内很好地分离。在测定的18种柑橘类水果干片和干粉样品中,6’,7’-二羟基佛手素的含量范围为1.52~159.04μg/g,环氧佛手柑素的含量范围为49.57~60.09μg/g,佛手柑素的含量范围为1.49~248.71μg/g。结论 本方法具有良好的准确性和重复性,适用于柑橘类水果干片中3种呋喃香豆素含量的分析测定。Objective To establish an ultra performance liquid chromatography-photodiode array detector method to analysis 3 kinds of furanocoumarins in dried citrus slices.Methods The samples were ultrasonically extracted with 40 mL ethyl acetate for 40 min twice.Vortex-assisted extraction were then repeated twice using 20 mL of ethyl acetate for 10 min.The ethyl acetate extracts were combined,concentrated to dryness in a rotary evaporator at 30 °C.The determination was carried out using an Acquity UPLC HSS C18 SB column(2.1mm×150 mm,1.8 μm) with a flow rate of 0.3 mL/min,column temperature of 30 ℃,and detector wavelength of 310 nm.A gradient elution was performed with mobile phase A water and acetonitrile as mobile phase B.Results The 6',7'-dihydroxybergamottin,epoxybergamottin and bergamottin showed good linearity within 3.00~300.00 μg/mL,4.32–432.00 μg/mL and 4.12–412.00 μg/mL with correlation coefficients greater than 0.999.The limits of detection were 0.09–0.17 μg/g.The limits of quantitation were 0.31-0.57 μg/g.The average recoveries with 3 concentration levels were 94.4%-99.1%.The relative standard deviations were between 2.7% and 4.7%(n=6).This method could separate 3 kinds of furanocoumarins in dried citrus slices well in 25 minutes.The developed method was successfully applied to determine 3kinds of furanocoumarins in 18 kinds of dried citrus slices and powders.The content of 6',7'-dihydroxybergamottin was between 1.52 and 159.04 μg/g.The content of epoxybergamottin was between 49.57 and 60.09 μg/g.The content of bergamottin was between 1.49 and 248.71 μg/g.Conclusion The established method has good repeatability and high accuracy,and can be used for the 3 kinds of furanocoumarins determination in dried citrus slices.

关 键 词：柑橘类水果干片 呋喃香豆素 超高效液相色谱 

分 类 号：R284.1[医药卫生—中药学]