European Food Research and Technology

, Volume 238, Issue 1, pp 85–91 | Cite as

Subcritical water extraction of phenolic compounds from flaxseed meal sticks using accelerated solvent extractor (ASE)

  • Evrim Özkaynak KanmazEmail author
Original Paper


Subcritical water extraction (SWE) is a technique based on the use of water as an extractant, at temperatures between 100 and 374 °C and at a pressure high enough to maintain the liquid state. SWE provides higher selectivities, low cost, and shorter extraction times. In this study, phenolic compounds in flaxseed (Linum usitatissimum L.) meal sticks were extracted with subcritical water using accelerated solvent extractor. For this aim, the interactions between temperature (160, 170, and 180 °C) and extraction time (5, 15, 30, and 60 min) for subcritical water extraction of SDG lignan, total phenolics, and total flavonoids from flaxseed meal sticks were investigated. The highest extraction yield of SDG lignan (77.01 %) in subcritical water extracts was determined at 160 °C for 60 min. However, high extraction yields were obtained as 70.67 and 72.57 % at 170 and 180 °C for 15 min, respectively. Also, the highest extraction yield of total phenolics (70.82 %) and total flavonoids (267.14 %) were determined at 180 °C for 15 min. Besides, high correlations between SDG lignan–total phenolics, SDG lignan–total flavonoids, and total phenolics–total flavonoids were obtained from 0.86 to 1 in water extracts.


Subcritical water extraction Accelerated solvent extractor (ASE) Flaxseed meal SDG lignan Total phenolics Total flavonoids 



This research was financed by TÜBİTAK as “The Support Programme for Scientific and Technological Research Projects (1001)” (project number 108O498). The authors gratefully acknowledge Aegean Agricultural Research Institute for providing flaxseed sample and Ege University Center of Drug Research & Development and Pharmacokinetic president and researchers for their technical helpings. Also, the authors would like to thank N. Bükey A.Ş. for the cold screw press of flaxseed.

Conflict of interest


Compliance with Ethics Requirements

This article does not contain any studies with human or animal subjects.


  1. 1.
    Adlercreutz H (2002) Phyto-oestrogens and cancer. Lancet Oncol 3:364–373CrossRefGoogle Scholar
  2. 2.
    AOAC (1998) Official methods of analysis of the association of analytical chemists. Washington D. C, USAGoogle Scholar
  3. 3.
    Ayala RS, Luque de Castro MD (2001) Analytical, nutritional and clinical methods section. continuous subcritical water extraction as a useful tool for isolation of edible essential oils. Food Chem 75:109–113CrossRefGoogle Scholar
  4. 4.
    Beejmohun V, Fliniaux O, Grand E, Lamblin F, Bensaddek L, Christen P, Kovensky J, Fliniaux M, Mesnard F (2007) Microwave-assisted extraction of the main phenolic compounds in flaxseed. Phytochemical Analysis 18:275–282CrossRefGoogle Scholar
  5. 5.
    Bozan B, Temelli F (2008) Chemical composition and oxidative stability of flax, safflower and poppy seed and seed oils. Bioresource Technol 99:6354–6359CrossRefGoogle Scholar
  6. 6.
    Cacace JE, Mazza G (2006) Pressurized low polarity water extraction of lignans from whole flaxseed. J Food Eng 77:1087–1095CrossRefGoogle Scholar
  7. 7.
    Choo WS, Birch J, Dufour JP (2007) Physicochemical and quality characteristics of cold-pressed flaxseed oils. J Food Compos Anal 20:202–211CrossRefGoogle Scholar
  8. 8.
    Collins TFX, Sprando RL, Black TN, Olejnik N, Wiesenfeld PW, Babu US, Bryant M, Flynn TJ, Ruggles DI (2003) Effects of flaxseed and defatted flaxseed meal on reproduction and development in rats. Food Chem Toxicol 41:819–834CrossRefGoogle Scholar
  9. 9.
    Çam M (2009) Extraction of antioxidant compounds of pomegranate peels and seeds with water using pressurized liquid extractor. Doctorate thesis, Ege Üniversity 245pGoogle Scholar
  10. 10.
    Çam M, Hışıl Y, Durmaz G (2009) Classification of eight pomegranate juices based on antioxidant capacity measured by four methods. Food Chem 112:721–726CrossRefGoogle Scholar
  11. 11.
    Eikani MH, Golmohammad F, Rowshanzamir S (2007) Subcritical water extraction of essential oils from coriander seeds (Coriandrum sativum L.). J Food Eng 80:735–740CrossRefGoogle Scholar
  12. 12.
    Eliasson C, Kamal-Eldin A, Andersson R, A man P (2003) High-performance liquid chromatographic analysis of secoisolariciresinol diglucoside and hydroxycinnamic acid glucosides in flaxseed by alkaline extraction. J Chromatogr A 1012:151–159CrossRefGoogle Scholar
  13. 13.
    Güçlü Üstündağ Ö, Balsevich J, Mazza G (2007) Pressurized low polarity water extraction of saponins from cow cockle seed. J Food Eng 80:619–630CrossRefGoogle Scholar
  14. 14.
    Hata S, Wiboonsirikul J, Maedab A, Kimura Y, Adachi S (2007) Extraction of defatted rice bran by subcritical water treatment. Biochem Eng J 40(1):44–53CrossRefGoogle Scholar
  15. 15.
    Herrero M, Martı′n-A′ lvarez PJ, Sen˜ora′ns FJ, Cifuentes A, Iba′n˜ez a E (2005) Optimization of accelerated solvent extraction of antioxidants from Spirulina platensis microalga. Food Chem 93:417–423CrossRefGoogle Scholar
  16. 16.
    Herrero M, Cifuentes A, Ibañez E (2006) Sub- and supercritical fluid extraction of functional ingredients from different natural sources: plants, food-by-products, algae and microalgae. Food Chem 98:136–148CrossRefGoogle Scholar
  17. 17.
    Ho CHL, Cacacea JE, Mazza G (2007) Extraction of lignans, proteins and carbohydrates from flaxseed meal with pressurized low polarity water. LWT-Food Science and Technol 40:1637–1647CrossRefGoogle Scholar
  18. 18.
    Hosseinian FS, Muir AD, Westcott ND, Krol ES (2006) Antioxidant capacity of flaxseed lignans in two model systems. J Am Oil Chem Soc 83(10):835–840CrossRefGoogle Scholar
  19. 19.
    Jime′nez-Carmonaa MM, Uberab JL, Luque de Castroa MD (1999) Comparison of continuous subcritical water extraction and hydrodistillation of marjoram essential oil. J Chromatogr 855:625–632CrossRefGoogle Scholar
  20. 20.
    Johnsson P, Peerlkampa N, Kamal-Eldin A, Andersson RE, Anderssona R, Lundgren LN, Åman P (2002) Polymeric fractions containing phenol glucosides in flaxseed. Food Chem 76:207–212CrossRefGoogle Scholar
  21. 21.
    Ju ZY, Howard LR (2005) Effects of solvent and temperature on pressurized liquid extraction of anthocyanins and total phenolics from dried red grape skin. J Agric Food Chem 51:5207–5213CrossRefGoogle Scholar
  22. 22.
    Ibanez E, Kubátová A, Seňoráns FJ, Cavero S, Reglero G, Hawthorne SB (2003) Subcritical water extraction of antioxidant compounds from rosemary plants. J Agric Food Chem 51:375–382CrossRefGoogle Scholar
  23. 23.
    Kubátová A, Lagadec AJM, Miller DJ, Hawthorne SB (2001) Selective extraction of oxygenates from savory and peppermint using subcritical water. Flavour Fragr J 16:64–73CrossRefGoogle Scholar
  24. 24.
    Lucas EA, Lightfoot SA, Hammond JL, Devareddy L, Khalil DA, Daggy BP, Smith BJ, Westcott N, Mocanu V, Soung do Y, Arjmandi BH (2004) Flaxseed reduces plasma cholesterol and atherosclerotic lesion formation in ovariectomized Golden Syrian hamsters. Atherosclerosis 173:223–229CrossRefGoogle Scholar
  25. 25.
    Monrad JK, Howard LR, King GJW, Srinivas K, Mauromoustakos A (2010) Subcritical solvent extraction of procyanidins from dried red grape pomace. J Agric Food Chem 58(7):4014–4021CrossRefGoogle Scholar
  26. 26.
    Muir AD, Westcott ND (2000) Quantitation of the lignan secoisolariciresinol diglucoside in baked goods containing flax seed or flax meal. J Agric Food Chem 48:4048–4052CrossRefGoogle Scholar
  27. 27.
    Oomah BD, Mazza G, Kenaschuk EO (1996) Flavonoid content of flax seed. Influ cultivar environ Euphytica 90:163–167CrossRefGoogle Scholar
  28. 28.
    Ozel MZ, Gogus F, Lewis AC (2003) Subcritical water extraction of essential oils from Thymbra spicata. Food Chem 82:381–386CrossRefGoogle Scholar
  29. 29.
    Özkaynak Kanmaz E, Ova G (2013) The effective parameters for subcritical water extraction of SDG lignan from flaxseed (Linum usitatissimum L.) using accelerated solvent extractor. Eur Food Res Technol 237(2):159–166Google Scholar
  30. 30.
    Palma M, Pineiro Z, Barroso CG (2002) In-line pressurized-fluid extraction–solid-phase extraction for determining phenolic compounds in grapes. J Chromatogr A 968:1–6CrossRefGoogle Scholar
  31. 31.
    Rangsriwong P, Rangkadilok N, Satayavivad J, Goto M, Shotipruk A (2009) Subcritical water extraction of polyphenolic compounds from Terminalia chebula Retz. Fruits Sep Purif Technol 66:51–56CrossRefGoogle Scholar
  32. 32.
    Richter BE, Jones BA, Ezzell JL, Porter NL, Avdalovic N, Pohl C (1996) Accelerated solvent extraction: a technique for sample preparation. Anal Chem 68:1033–1039CrossRefGoogle Scholar
  33. 33.
    Rodríguez-Meizoso I, Marin FR, Herrero M, Se˜norans FJ, Reglero G, Cifuentes A, Ibáňez E (2006) Subcritical water extraction of nutraceuticals with antioxidant activity from oregano, chemical and functional characterization. J Pharm Biomed Anal 41:1560–1565CrossRefGoogle Scholar
  34. 34.
    Shotipruk A, Kiatsongserm J, Pavasant P, Goto M, Sasaki M (2004) Pressurized hot water extraction of anthraquinones from the roots of Morinda citrifolia. Biotechnol Prog 20:1872–1875CrossRefGoogle Scholar
  35. 35.
    Struijs K, Vincken JP, Verhoef R, van Oostveen-van Casteren VHM, Voragen AGJ, Gruppen H (2007) The flavonoid herbacetin diglucoside as a constituent of the lignan macromolecule from flaxseed hulls. Phytochemistry 68:1227–1235CrossRefGoogle Scholar
  36. 36.
    Teo CC, Tan SN, Yong JWH, Hew CS, Ong ES (2008) Evaluation of the extraction efficiency of thermally labile bioactive compounds in Gastrodia elata Blume by pressurized hot water extraction and microwave-assisted extraction. J Chromatogr A 1182(1):34–40CrossRefGoogle Scholar
  37. 37.
    Vanharanta M, Voutilainen S, Rissanen TH, Adlercreutz H, Salonen JT (2003) Risk of cardiovascular disease-related and all-cause death according to serum concentrations of enterolactone: Kuopio Ischaemic Heart Disease Risk Factor Study. Intern Arch Med 163:1099–1104CrossRefGoogle Scholar
  38. 38.
    Wiboonsirikul J, Kimura Y, Kadota M, Morita M, Tsuno T, Adachi S (2007) Properties of extracts from defatted rice bran by its subcritical water treatment. J Agric Food Chem 55:8759–8765CrossRefGoogle Scholar
  39. 39.
    Yang Y, Kayan B, Bozer N, Pate B, Baker C, Gizir AM (2007) Terpene degradation and extraction from basil and oregano leaves using subcritical water. J Chromatogr A 1152:262–267CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  1. 1.Nutrition and Dietetics Department, Health CollegeArtvin Çoruh UniversityArtvinTurkey

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