LLE-UPLC-FLD法测定橄榄油中羟基酪醇和酪醇的含量

Determination of the contents of tyrosol and hydroxytyrosol in olive oil by liquid-liquid extraction and UPLC-FLD

建立了液液萃取-超高效液相色谱串联荧光检测器(LLE-UPLC-FLD)快速分离和测定橄榄油中羟基酪醇和酪醇含量的方法。橄榄油样品经乙醇提取后,以0.2%(v/v)甲酸乙腈溶液和0.2%(v/v)甲酸水为流动相,梯度洗脱,采用BEH(50 mm×1.0 mm,1.7μm)色谱柱,柱温为35℃,流速为0.15 m L/min,进样量为2.0μL,使用荧光检测器在激发波长为300 nm,发射波长为350 nm下进行检测,整个分析过程仅需10 min。羟基酪醇和酪醇的检出限(S/N=3)及定量限(S/N=10)分别为0.11,0.13和0.31,0.39μg/g,2种组分按高、中、低3个浓度水平加标回收率均高于89.52%;在最优条件下,对20批不同产地橄榄油中的羟基酪醇和酪醇进行检测,羟基酪醇和酪醇的含量范围分别在1.28~20.34及1.03~21.22μg/g之间;该法简便快速,重复性良好,结果准确可靠,可用于橄榄油中酪醇和羟基酪醇含量的测定。

This study was established a method of uhra performance liquid chromatography tandem fluorescence detector with liquid-liquid extraction for the rapid separation and determination of tyrosol and hydroxytyrosol in olive oil.The mobile phase was mixture with 0.2% （v/v） formic acid acetonitrile and 0.2% （v/v） formic acid water at a flow rate of 0.15 mL/min after extracted by ethanol. Using the BEH（ 1.0 mm i.d. × 50 mm 1.7 μm）column.The fluorescence detector was detected at the excitation wavelength of 300 nm and the emission wavelength of 350 nm.The whole analysis process is only 10 rain.The limit of detection（LOD） and limit of quantification （LOQ） of tyrosol and hydroxytyrosol were 0.11,0.13 μg/g and 0.31,0.39 μg/g, respectively.The recovery rate of the 2 components at the high,middle and low levels of 3 concentration levels was higher than 89.52%.The determination of tyrosol and hydroxytyrosol in 20 batches of olive oil from different areas were carried out under the optimal conditions.The contents of tyrosol and hydroxytyrosol were range from 1.28-20.34 μg/g and 1.03-21.22μg/g, respectively.This method is simple,fast and reproducible, and could applicable for determination of tyrosol and hydroxytyrosol in olive oil.