Méjean Marie, Brunelle Alain, Touboul David
Institut de Chimie des Substances Naturelles, UPR2301, CNRS, Avenue de la Terrasse, 91198, Gif-sur-Yvette, France.
Anal Bioanal Chem. 2015 Jul;407(17):5133-42. doi: 10.1007/s00216-015-8604-7. Epub 2015 Mar 31.
For the most effective analytical strategies, development and validation include optimization of such analytical variables as resolution, detectability, sensitivity, simplicity, cost effectiveness, flexibility, and speed. However, other aspects concerning operator safety and environmental impact are not considered at the same level. The result has been many unintended negative effects of analytical methods developed to investigate different kinds of sample, especially hydrophobic compounds that generate a large amount of chemical waste and have a strong negative environmental impact. In this context, quantification of tocopherols and tocotrienols, i.e. the vitamin E family, is usually achieved by normal-phase liquid chromatography using large volumes of toxic organic solvents, or reversed-phase liquid chromatography using a high percentage of methanol for elution. We propose here a "greener" analytical strategy, including the hyphenation of supercritical-fluid chromatography, using CO2 and ethanol as mobile phase, NH2 as stationary phase, and mass spectrometry for the detection and quantification of vitamin E congeners in soybean oil. An atmospheric-pressure photoionization (APPI) source seemed significantly more sensitive and robust than electrospray or atmospheric-pressure chemical ionization (APCI). This method led to shortened analysis time (less than 5 min) and was revealed to be as sensitive as more traditional approaches, with limits of detection and quantification in the tens of μg L(-1).
对于最有效的分析策略而言，方法的开发与验证包括对诸如分离度、可检测性、灵敏度、简易性、成本效益、灵活性和速度等分析变量的优化。然而，与操作人员安全和环境影响相关的其他方面并未得到同等程度的考量。其结果是，为研究各类样品（尤其是疏水性化合物，这类化合物会产生大量化学废物并对环境造成严重负面影响）而开发的分析方法产生了许多意想不到的负面效应。在此背景下，生育酚和生育三烯酚（即维生素E家族）的定量分析通常通过正相液相色谱法实现，该方法需使用大量有毒有机溶剂，或者通过反相液相色谱法实现，此方法使用高比例甲醇进行洗脱。我们在此提出一种“更环保”的分析策略，包括超临界流体色谱联用，以二氧化碳和乙醇作为流动相，氨基作为固定相，并采用质谱法对大豆油中的维生素E同系物进行检测和定量分析。大气压光电离（APPI）源似乎比电喷雾或大气压化学电离（APCI）源显著更灵敏且更稳定。该方法使分析时间缩短（不到5分钟），并且经证实与更传统的方法一样灵敏，检测限和定量限在数十μg L(-1)。
