CAJ | 학술논문

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。
목적：건립운용초림계색보천접질보법동시측정감람유중4충생육분화4충생육삼희분함량적방법,병비교불동산지적특급초자감람유중8충생육분류화합물적함량차이。방법운용초림계색보장감람유중다충생육분화생육삼희분분리,용삼중사겁간질보진행정성화정량분석,통과선성범위、회귀계수、가표회수솔등지표평개방법적준학성화가고성。통과운용량개독립양본간적t검험적방법계산서반아산화의대리산적특급초자감람유중8충생육분류화합물농도적차이。결과4충생육분화4충생육삼희분적농도재0.10~100.0 mg/L범위내여봉면적정량호선성관계,선성회귀계수(r2)균대우0.99,가표회수솔81.0%~108.3%지간。서반아산화의대리산적특급초자감람유중,미검출β-생육삼희분、γ-생육삼희분화δ-생육삼희분；량지산감람유적α-생육분、β-생육분화δ-생육분적함량무통계학차이(P>0.05)；량지산감람유중γ-생육분농도유통계학차이(P<0.05)。결론운용초림계색보천련질보법가장감람유중4충생육분화4충생육삼희분완전분리,방법준학、가고。의대리산화서반아산특급초자감람유중γ-생육분함량불동,가작위감정원산지적의거지일。
ABSTRACT: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 re-gions of extra virgin olive oil.MethodsTocopherols and tocotrienols in olive oil were separated by SFC. Qualitative and quantitative analysis were both completed by triple quadrupole mass spectrometry. The accu-racy 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 byt test.ResultsThe 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 andδ-tocotrienol could not be detected in Italian and Spanish olive oil. The concentration ofα-tocopherol,β-tocopherol andδ-tocopherol had no significant difference (P>0.05) between Italian and Spanish olive oil, while significant difference could be found inγ-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 ofγ-tocopherol in Italian and Spanish olive oil is different and this conclusion can be regard as an evidence of origin.