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Determination of n-alkanes in C-annuum (bell pepper) fruit and seed using GC-MS: comparison of extraction methods and application to samples of different geographical origin

机译:用气相色谱-质谱法测定桔梗(柿子椒)果实和种子中的正构烷烃:比较提取方法并应用于不同地理来源的样品

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摘要

An efficient extraction and analysis method was developed for the isolation and quantification of n-alkanes from bell peppers of different geographical locations. Five extraction techniques, i.e., accelerated solvent extraction (ASE), ball mill extraction, ultrasonication, rinsing, and shaking, were quantitatively compared using gas chromatography coupled to mass spectrometry (GC-MS). Rinsing of the surface wax layer of freeze-dried bell peppers with chloroform proved to be a relatively quick and easy method to efficiently extract the main n-alkanes C-27, C-29, C-31, and C-33. A combined cleanup and fractionation approach on Teflon-coated silica SPE columns resulted in clean chromatograms and gave reproducible results (recoveries 90-95 %). The GC-MS method was reproducible (R (2) = 0.994-0.997, peak area standard deviation = 2-5 %) and sensitive (LODs, S/N = 3, 0.05-0.15 ng/mu L). The total main n-alkane concentrations were in the range of 5-50 mu g/g dry weight. Seed extractions resulted in much lower total amounts of extracted n-alkanes compared to flesh and surface extractions, demonstrating the need for further improvement of pre-concentration and cleanup. The method was applied to 131 pepper samples from four different countries, and by using the relative n-alkane concentration ratios, Dutch peppers could be discriminated from those of the other countries, with the exception of peppers from the same cultivar.
机译:开发了一种有效的提取和分析方法,用于从不同地理位置的甜椒中分离和定量正构烷烃。使用气相色谱-质谱联用技术(GC-MS)定量比较了五种提取技术,即加速溶剂提取(ASE),球磨机提取,超声处理,漂洗和振荡。事实证明,用氯仿冲洗冻干甜椒的表面蜡层是一种相对快速简便的方法,可以有效地提取主要的正构烷烃C-27,C-29,C-31和C-33。在特富龙涂层硅胶SPE色谱柱上采用组合的净化和分馏方法可得到干净的色谱图,并得到可重现的结果(回收率90-95%)。 GC-MS方法具有可重现性(R(2)= 0.994-0.997,峰面积标准偏差= 2-5%)和灵敏(LOD,S / N = 3,0.05-0.15 ng /μL)。正主链烷烃的总浓度在5至50微克/克干重之间。与果肉和表面提取相比,种子提取导致提取的正构烷烃总量低得多,这表明需要进一步改善预浓缩和净化效果。该方法应用于来自四个不同国家的131个胡椒样品,并且通过使用相对正构烷烃浓度比,可以将荷兰胡椒与其他国家的胡椒区别开来,但同一品种的胡椒除外。

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