| Title: | Optimization of a multiple headspace sorptive extraction method coupled to gas chromatography-mass spectrometry for the determination of volatile compounds in macroalgae |
| Author(s): | Maruti A; Duran-Guerrero E; Barroso CG; Castro R; |
| Address: | "Analytical Chemistry Department, Faculty of Sciences-IVAGRO, University of Cadiz, Agrifood Campus of International Excellence, Post Office Box 40, Pol. Rio San Pedro, Puerto Real 11510, Cadiz, Spain. Analytical Chemistry Department, Faculty of Sciences-IVAGRO, University of Cadiz, Agrifood Campus of International Excellence, Post Office Box 40, Pol. Rio San Pedro, Puerto Real 11510, Cadiz, Spain. Electronic address: enrique.duranguerrero@uca.es" |
| DOI: | 10.1016/j.chroma.2018.04.011 |
| ISSN/ISBN: | 1873-3778 (Electronic) 0021-9673 (Linking) |
| Abstract: | "A novel extraction technique is proposed in which the Multiple Headspace Extraction (MHE) approach is used in conjunction with Headspace Sorptive Extraction (HSSE) and Gas Chromatography-Mass Spectrometry (GC-MS) detection. The extraction method was developed to determine volatile compounds in macroalgae. Optimization of the extraction parameters was carried out using design of experiments to identify factors that affect the extraction: extraction time, temperature, twister length and amount of sample. The results of the optimization led to an extraction of 2?ª+g of sample using a 20?ª+mm Twister((R)) at 66?ª+ degrees C for 180?ª+min. The progression constants (beta) were calculated for 43 volatile compounds, 29 of which could be quantified using the method. Linearity was attained with a determination coefficient higher than 0.99 for all studied compounds. Inter-day and inter-twister precisions ranged from 0.22% to 19.01% and from 0.69% to 14.76% respectively, and values below 10% were obtained for the majority of compounds. LOD and LOQ values ranged from the values obtained for diethyl succinate (0.012?ª+mug/L and 0.088?ª+mug/L, respectively) and those obtained for dimethyl sulfide (5.544?ª+mug/L and 40.286?ª+mug/L, respectively). However, for the majority of compounds values obtained were below 1?ª+mug/L (LOD) and 5?ª+mug/L (LOQ). Compounds such as ethyl acetate, hexanal, heptadecane, 2-hexenal, 6-methyl-5-hepten-2-one, dimethyl sulfide, benzyl alcohol, beta ionone, or beta cyclocitral, among others were correctly determined in three species of macroalgae: Ulva sp., Gracillaria sp. and Enteromorpha sp" |
| Keywords: | Adsorption *Gas Chromatography-Mass Spectrometry Limit of Detection Seaweed/*chemistry/metabolism Solid Phase Extraction/methods Succinates/analysis/isolation & purification Sulfides/analysis/isolation & purification Volatile Organic Compounds/*analysis/i; |
| Notes: | "MedlineMaruti, Astrid Duran-Guerrero, Enrique Barroso, Carmelo G Castro, Remedios eng Netherlands 2018/04/14 J Chromatogr A. 2018 May 25; 1551:41-51. doi: 10.1016/j.chroma.2018.04.011. Epub 2018 Apr 5" |
