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Multidimensional gas chromatographic‒Mass spectrometric method for separation and identification of triacylglycerols in olive oil.
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-08-18 , DOI: 10.1016/j.chroma.2020.461474
Habtewold D Waktola 1 , Yada Nolvachai 1 , Philip J Marriott 1
Affiliation  

A ‘heart-cut’ multidimensional gas chromatography‒mass spectrometry (H/C MDGC‒MS) method for separation and identification of triacylglycerols (TAGs) in extra virgin olive oil was developed. A GC configuration, comprising a non-polar first dimension (1D) column (15 m length) and a mid-polarity second dimension (2D) column (9 m length), was employed. Standard TAGs were used to test and demonstrate the H/C MDGC method, for identification of TAG components and to validate the method. Various chromatographic conditions such as column flow and temperature program were evaluated. The 1D separation resulted in overlap of some standard TAG peaks. These overlapped 1D regions of the standard TAGs were H/C to 2D for further separation and resulted in clearly distinguished individual TAG component peaks. The 1D separation of olive oil TAGs displayed three major peaks and four minor peaks. The application of the H/C MDGC method to olive oil TAGs resulted in the separation of each sampled 1D region into two or more TAG peaks. TAG components in olive oil resolved on the 2D column were identified based on characteristic mass fragment ions such as [M–RCO2]+, [RCO+128]+, [RCO+74]+ and RCO+ and comparison of their mass spectra with that of the standard TAGs. Sixteen olive oil TAGs were identified by MS after 2D separation. The repeatability of the H/C method was evaluated in terms of retention time shift and area response in the 2D and found to be <0.02% and <8% RSD respectively.



中文翻译:

多维气相色谱‒质谱法分离和鉴定橄榄油中的三酰基甘油。

开发了一种“心切”多维气相色谱-质谱法(H / C MDGC‒MS),用于分离和鉴定特级初榨橄榄油中的三酰基甘油(TAGs)。采用了一种GC配置,包括一个非极性的第一维(1 D)色谱柱(15 m长)和一个中等极性的第二维(2 D)色谱柱(9 m长)。标准TAG用于测试和演示H / C MDGC方法,用于识别TAG组件并验证该方法。评估了各种色谱条件,例如柱流量和温度程序。的1 d分离导致的一些标准TAG峰重叠。这些重叠的1个标准TAG的d区分别为H / C至2D进行进一步分离,并得到清晰区分的单个TAG组分峰。的1橄榄油TAG的分离d显示三个主要峰和四个次要峰。H / C MDGC方法对橄榄油TAG的应用导致将每个采样的1 D区分离为两个或多个TAG峰。在解决在橄榄油TAG部件2 d柱中鉴定基于特征质量碎片离子,如[M-RCO 2 ] +,[RCO + 128] +,[RCO + 74] +和RCO +和它们的质量的比较具有标准TAG的光谱。2次后MS鉴定出16个橄榄油TAGD分离。的H / C方法的重复性在保留时间漂移和面积响应来评价2 d,发现为<分别为0.02%和<8%RSD。

更新日期:2020-08-19
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