Ledesma-Escobar Carlos A, Priego-Capote Feliciano, Luque de Castro María Dolores
Department of Analytical Chemistry, Annex C-3, Campus of Rabanales, University of Córdoba, Córdoba, Spain; University of Córdoba Agroalimentary Excellence Campus, ceiA3, and Institute of Biomedical Research Maimónides (IMIBIC), Reina Sofía Hospital, University of Córdoba, E-14071 Córdoba, Spain.
Department of Analytical Chemistry, Annex C-3, Campus of Rabanales, University of Córdoba, Córdoba, Spain; University of Córdoba Agroalimentary Excellence Campus, ceiA3, and Institute of Biomedical Research Maimónides (IMIBIC), Reina Sofía Hospital, University of Córdoba, E-14071 Córdoba, Spain.
Talanta. 2015 Nov 1;144:522-8. doi: 10.1016/j.talanta.2015.07.011. Epub 2015 Jul 6.
A comparative study of methods for ultrasound-assisted extraction (USAE), microwave-assisted extraction (MAE) and superheated liquid extraction (SHLE) of compounds from citrus has been performed. The suited conditions for each method were evaluated to maximize the concentration of 10 representative compounds (sugars, carboxylic acids, phenolic acids and flavonoids) by a desirability function approach based on the chromatographic peaks obtained by LC-DAD. Extracts obtained under the suited conditions were analyzed by LC-QTOF MS/MS. The ANOVA on the molecular entities showed 232 significant entities (p<0.01), and pairwise comparison revealed that USAE and MAE methods are the most similar (50 different entities), and USAE and SHLE the most dissimilar (224 different entities). A discrimination test by PCA showed a clear discrimination among the extraction methods, explaining 78.51% of the total variability. Similarities in the abundance of the monitored compounds was tested by ANOVA showing that the extraction of carboxylic acids (malic and citric acids) was equal by all methods; while for each of the other eight compounds, at least one extraction method is different from the others. Under the evaluated conditions the SHLE method is the less favorable to extract metabolites from citrus, being the best the USAE method.
对柑橘类化合物的超声辅助萃取（USAE）、微波辅助萃取（MAE）和过热液体萃取（SHLE）方法进行了比较研究。基于LC-DAD获得的色谱峰，通过期望函数法评估了每种方法的适宜条件，以最大化10种代表性化合物（糖类、羧酸类、酚酸类和黄酮类）的浓度。在适宜条件下获得的提取物通过LC-QTOF MS/MS进行分析。对分子实体的方差分析显示有232个显著实体（p<0.01），成对比较表明USAE和MAE方法最相似（50个不同实体），而USAE和SHLE最不相似（224个不同实体）。主成分分析（PCA）的判别测试表明萃取方法之间有明显区分，解释了总变异性的78.51%。通过方差分析测试了所监测化合物丰度的相似性，结果表明所有方法对羧酸类（苹果酸和柠檬酸）的萃取效果相同；而对于其他八种化合物中的每一种，至少有一种萃取方法与其他方法不同。在所评估的条件下，SHLE方法最不利于从柑橘中萃取出代谢物，USAE方法最佳。
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