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

中文关键词:  柑橘类水果干片  呋喃香豆素  超高效液相色谱

英文关键词:dried citrus slices  furanocoumarins  ultra performance liquid chromatography

中文摘要:

      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40 mL乙酸乙酯超声提取40 min, 再采用20 mL乙酸乙酯分两次涡旋10 min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, 1.8 μm)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3.00~300.00 μg/mL、4.32~432.00 μg/mL、4.12~412.00 μg/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0.09~0.17 μg/g, 定量限为0.31~0.57 μg/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25 min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1.52~159.04 μg/g, 环氧佛手柑素的含量范围为49.57~60.09 μg/g, 佛手柑素的含量范围为1.49~248.71 μg/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。

英文摘要:

      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 3 kinds 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.