Evaluation of a Microwave-Assisted Extraction Method for Lignan Quantification in Flaxseed Cultivars and Selected Oil Se
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Evaluation of a Microwave-Assisted Extraction Method for Lignan Quantification in Flaxseed Cultivars and Selected Oil Seeds Simona Mihaela Nemes & Valérie Orsat
Received: 1 June 2011 / Accepted: 2 August 2011 / Published online: 17 August 2011 # Springer Science+Business Media, LLC 2011
Abstract An optimized microwave-assisted extraction (MAE) method was evaluated through repeatability, recovery and efficiency testing. The repeatability tests, performed by three users over time, were not significantly different. The recovery of lignan throughout the extraction, preparation and analysis steps is 97.5% with a coefficient of variation 99%)—were purchased from Chromadex (Santa Ana, CA, USA); SECO (molecular weight, 362.4; purity, ≥95%) was purchased from SigmaAldrich (Oakville, ON, Canada). The solvents acetonitrile, methanol and hexane of HPLC grade were obtained from Fisher Scientific (Ottawa, ON, Canada). The reagents sodium hydroxide ≥98%, sulphuric acid 95–98% ACS, phosphoric acid ≥85% and dipotassium hydrogen phosphate 98% were purchased from Sigma-Aldrich. Samples The flaxseed (Linum usitatissiumum L.) used for the MAE method efficiency assessment and validation was purchased in 2009 from a local grocery store (Montreal, QC, Canada); the country of provenance was Guatemala, as specified on the package. The flaxseed cultivars (CDC Bethune, McBeth, Prairie Blue, Flanders, 09LS01, CRGL 8.1 and CRGL 8.2) analysed for SDG content were provided by Mr. Yves Dion from Centre de Recherche sur les Grains Inc. (CEROM). All the cultivars or advanced breeding lines were grown in Saint-Mathieu-de-Beloeil, (QC, Canada) in 2009. The Omega-3 Flax Hull, produced in May 2010, was provided by Dr. Nam Fong Han from Natunola Health Inc. (Winchester, ON, Canada). Other samples used for lignan analysis were purchased from local grocery stores in 2008 and 2010 as follows: white and black sesame (Sesamum indicum L.) seeds and black chia (Salvia hispanica L.) seeds were purchased in 2008; white and black chia seeds, brown sesame seeds, sunflower seeds and almonds were purchased in 2010. All the samples were divided into batches of 100–300 g, packed in plastic bags (the flaxhull was vacuum-packed) and stored at −18 °C until use. Microwave Extraction Apparatus The MAE experiments were carried out in a mono-mode (focused) microwave apparatus (Star System 2, CEM, Mathews, USA) with a nominal power of 800 W and microwave frequency of 2.45 GHz. The temperature was monitored by a built-in IR temperature sensor placed at the
All extracts were analysed in triplicate (coefficient of variation, 0.999. The following equations were used for quantification: SDG = peak height/ 0.4494, SECO = peak height/1.054, ANSECO = peak height/0.8065. Sample Preparation Microwave-Assisted Extraction Experiments were carried out in order to assess the repeatability and the efficiency of the optimized MAE method and for the quantification of lignans in various flaxseed cultivars, flaxseed hulls, sesame seeds, chia seeds, almonds and sunflower seeds. Some experiments
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