超临界色谱串联质谱法测定橄榄油中 维生素E含量的研究

Determination of vitamin E in olive oil by supercritical fluid chromatography tandem mass spectrometry

中文关键词:  生育酚  生育三烯酚  超临界色谱  质谱法

英文关键词:tocopherol  tocotrienol  supercritical fluid chromatography  mass spectrography

中文摘要:

      目的 建立运用超临界色谱串接质谱法同时测定橄榄油中4种生育酚和4种生育三烯酚含量的方法, 并比较不同产地的特级初榨橄榄油中8种生育酚类化合物的含量差异。方法 运用超临界色谱将橄榄油中多种生育酚和生育三烯酚分离, 用三重四极杆质谱进行定性和定量分析, 通过线性范围、回归系数、加标回收率等指标评价方法的准确性和可靠性。通过运用两个独立样本间的t检验的方法计算西班牙产和意大利产的特级初榨橄榄油中8种生育酚类化合物浓度的差异。结果 4种生育酚和4种生育三烯酚的浓度在0.10~100.0 mg/L范围内与峰面积呈良好线性关系, 线性回归系数(r2)均大于0.99, 加标回收率81.0%~108.3%之间。西班牙产和意大利产的特级初榨橄榄油中, 未检出β-生育三烯酚、γ-生育三烯酚和δ-生育三烯酚; 两地产橄榄油的α-生育酚、β-生育酚和δ-生育酚的含量无统计学差异(P>0.05); 两地产橄榄油中γ-生育酚浓度有统计学差异(P<0.05)。结论 运用超临界色谱串联质谱法可将橄榄油中4种生育酚和4种生育三烯酚完全分离, 方法准确、可靠。意大利产和西班牙产特级初榨橄榄油中γ-生育酚含量不同, 可作为鉴定原产地的依据之一。

英文摘要:

      Objective To establish a method for simultaneous determination of 4 kinds of tocopherols and 4 kinds of tocotrienols in Italian and Spanish olive oil by supercritical fluid chromatography tandem mass spectrometry (SFC-MS), and compare the content difference of 8 kinds of phenolic compounds of different regions of extra virgin olive oil. Methods Tocopherols and tocotrienols in olive oil were separated by SFC. Qualitative and quantitative analysis were both completed by triple quadrupole mass spectrometry. The accuracy and reliability of the method was calculated by range of linearity, coefficient of regression and sample added recovery. The concentration of all kinds of tocopherols and tocotrienols in Italian and Spanish olive oil were tested by t test. Results The concentration of tocopherol and tocotrienol at the range of 0.10 to 100.0 mg/L had a good linearity with the peak area, coefficient of regression was higher than 0.99, and recoveries was 81.0%~108.3%. β-tocotrienol, γ-tocotrienol and δ-tocotrienol could not be detected in Italian and Spanish olive oil. The concentration of α-tocopherol, β-tocopherol and δ-tocopherol had no significant difference (P>0.05) between Italian and Spanish olive oil, while significant difference could be found in γ-tocopherol (P<0.05). Conclusion Four kinds of tocopherols and 4 kinds of tocotrienols in olive oil can be separated completely by SFC-MS. The concentration of γ-tocopherol in Italian and Spanish olive oil is different and this conclusion can be regard as an evidence of origin.