A novel method for the determination of total 1,3-octanediols in apple juice via 1,3-dioxanes by solid-phase microextraction and high-speed gas chromatography

• Published in: Journal of Chromatography A 2010-04, Vol.1217 (18), p.2993-2999
• Main Authors: Llorente, Daniel Díaz, Abrodo, Pilar Arias, de la Fuente, Enrique Dapena, Alonso, Juan José Mangas, Álvarez, Maria Dolores Gutiérrez, Gomis, Domingo Blanco
• Format: Article
• Language: English
• Subjects: 1,3-Dioxanes; 1,3-Octanediols; acetaldehyde; alcohols; Apple juice; Biological and medical sciences; chemical reactions; derivatization; Experimental design; food analysis; Food industries; Fruit and vegetable industries; Fundamental and applied biological sciences. Psychology; gas chromatography; Gas chromatography–mass spectrometry; High-speed gas chromatography; Malus; microextraction; Non alcoholic beverage industries and mineral waters; solid phase extraction; Solid-phase microextraction
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2010.02.074

In this work, a novel, simple and fast method based on solid-phase microextraction (SPME) followed by high-speed gas chromatography (HSGC) was developed for the analysis of total 1,3-octanediols in apple juices by means of derivatization reaction to volatile 1,3-dioxanes. The derivatization reaction, SPME conditions, glycosidically bound fraction and 1,3-nonanediol as a surrogate standard were studied. The formation of 1,3-dioxanes from 1,3-diols was confirmed by GC–MS. The method was validated obtaining a regression coefficient ( r 2) of 0.9996, precisions between 0.3 and 9.8%, extraction recoveries in the range 94.7–112.2% and LOD of 2.9 μg l −1. Experimental design has been employed in the optimization of extraction factors and robustness assessment. The method was applied to the analysis of 21 Asturian apple varieties finding a double reciprocal relationship between the concentrations of saturated and unsaturated 1,3-octanediol.