Charabot S.A., 10 Avenue Yves Emmanuel Baudoin, 06130 Grasse, France.
J Chromatogr A. 2012 Jun 8;1241:103-11. doi: 10.1016/j.chroma.2012.04.012. Epub 2012 Apr 11.
A simple, fast, and efficient High-Performance Thin-Layer Chromatography (HPTLC) method was developed for the simultaneous quantitative determination of alcohols and acetates in Haitian vetiver essential oils (Chryzopogon zizanioides) and its acetylated form. Analytes were separated by using a mixture of n-hexane-chloroform-ethyl acetate (8:6:0.5, v/v/v) as mobile phase under 47% humidity. Quantification was achieved by densitometric evaluation of the analytes in absorbance mode under visible light (λ=530 nm) after staining with a vanillin-sulfuric acid reagent. Reference mixtures of alcohols and acetates were obtained by fractionation of Haitian vetiver oil or vetiver acetates, followed by purification of the fractions of interest by means of Over-Pressured Layer Chromatography (OPLC). The chemical composition of each reference fraction was determined by using GC-MS and GC×GC-MS, and their overall purity was determined by GC/FID and HPTLC. The TLC method provided compact spots for alcohols (R(f2)=0.18±0.01 and R(f1)=0.28±0.01) and acetates (R(f3)=0.65±0.01). Calibration plots showed good linear correlation with r²=0.9995±0.0001 and r²=0.9995±0.0001 for alcohols and r²=0.9996±0.0001 for acetates in a 40-200 ng spot⁻¹ concentration range with respect to peak areas. The method was validated for precision and accuracy. Limit of detection (LOD) and quantification (LOQ) were determined. Method specificity was confirmed using retention factor (R(f)) and GC-MS control of the standards reference mixtures.
开发了一种简单、快速、高效的高效薄层色谱（HPTLC）方法，用于同时定量测定海地香根草精油（Chryzopogon zizanioides）及其乙酰化形式中的醇类和乙酸酯。在 47%湿度下，使用正己烷-氯仿-乙酸乙酯（8:6:0.5，v/v/v）混合物作为流动相分离分析物。通过在可见光（λ=530nm）下用香草醛-硫酸试剂对分析物进行染色，以吸光度模式对分析物进行密度计评估来实现定量。通过分馏海地香根草油或香根草乙酸酯获得醇类和乙酸酯的参考混合物，然后通过加压层色谱（OPLC）对感兴趣的馏分进行纯化。使用 GC-MS 和 GC×GC-MS 确定每个参考馏分的化学成分，并通过 GC/FID 和 HPTLC 确定其总纯度。TLC 方法为醇类（R(f2)=0.18±0.01 和 R(f1)=0.28±0.01）和乙酸酯（R(f3)=0.65±0.01）提供了紧凑的斑点。校准曲线显示出良好的线性相关性，r²=0.9995±0.0001 和 r²=0.9995±0.0001 用于醇类，r²=0.9996±0.0001 用于乙酸酯，在 40-200ng 斑点-¹浓度范围内，相对于峰面积。该方法经过精密度和准确性验证。确定了检测限（LOD）和定量限（LOQ）。通过保留因子（R(f)）和标准参考混合物的 GC-MS 控制来确认方法的特异性。
