SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED FOR ORGANIC OIL RICH IN OMEGA-3 FATTY ACIDS A Dissertation Submitted to the Graduate Faculty of the North Dakota State University of Agriculture and Applied Science By Yun-ling Zheng In Partial Fulfillment of the Requirements for the Degree of DOCTOR OF PHILOSOPHY Major Program: Engineering Ph.D. November 2003 Fargo, North DakotaUMI Number: 3115004 INFORMATION TO USERS The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleed-through, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized ‘copyright material had to be removed, a note will indicate the deletion. UMI UMI Microform 3115004 Copyright 2004 by ProQuest Information and Learning Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. ProQuest Information and Learning Company 300 North Zeeb Road P.O. Box 1346, ‘Ann Arbor, MI 48106-1346North Dakota State University Graduate School Title SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED FOR ORGANIC OIL RICH IN OMEGA-3 FATTY ACIDS By Yun-Ling Zhen ‘The Supervisory Committee certifies that this disquisition complies with North Dakota State University’s regulations and meets the accepted standards for the degree of DOCTOR OF PHILOSOPHY SUPERVISORY COMMITTEE: or. dennis wiesenborn AGrons Mtsenrtorm/ Chair Prof. Leslie Backer Zt F bouche Dr. Dean Steele i, Dr. Clifford Hall IIT Dr. James Coykendall Approved by Department Chair: Mayer her 34, 2003 Lit Lhaf, /ABSTRACT Zheng, Yun-ling, Ph.D., Program of Engineering Ph.D., College of Engineering and Architecture, North Dakota state University, November 2003. Screw Pressing of Whole and Dehulled Flaxseed for Organic 0il Rich in Omega-3 Fatty Acids. Major Professor: Dr. Dennis. P. Wiesenborn. Flaxseed oil is a rich source of dietary omega-3 fatty acids and is commonly obtained by cold pressing whole seed. Furthermore, flaxseed hulls are emerging as a valuable lignan-rich product for functional food use; therefore, the pressing characteristics of dehulled seed should be understood. Screw press performance was measured for pressing whole and dehulled flaxseed with different fraction of hull removal (FHR). Steady-state energy analysis was carried out to calculate the specific mechanical energy (SME) from the calculation of net enthalpy change and heat loss. The influence of extraction and pretreatment methods on the quality of flaxseed oil was also measured. When whole Omega flaxseed was pressed through a 6 mm choke, an inverse relationship between seed moisture content (6.1 to 11.6% range) and oil recovery (70.1 to 85.7%) was observed. However, the oil recovery from pressing dehulled Omega flaxseed was low at both moisture content extremes. Although oil recovery from dehulled Omega flaxseed was lower than from whole Omega flaxseed, the weight of oil produced from dehulled Omega flaxseed per unit time was higher. iiiThe decrease of moisture content and FHR all resulted in significant increases of both oil and meal temperature and net enthalpy change. Conduction dissipated up to half of the mechanical energy input while convection was low. SME increased significantly from 81.1 to 104.7 kJ/kg when the moisture content of whole flaxseed decreased from 12.6 to 6.3% (dry basis). SME when pressing whole flaxseed was significantly higher than when pressing dehulled flaxseed. The oi1 recovery from pressing uncooked, dehulled flaxseed averaged 56.7% and was significantly higher than that from pressing corresponding samples cooked at 100°C or 120°C for 10 min. The oil sampled from pressing dehulled flaxseed that was cooked at 100°C for 10 minutes had the highest peroxide value at an average of 5.63 meq peroxide/kg oil. Oil from screw pressing whole uncooked flaxseed had the lowest peroxide value of 0.15 meq peroxide/kg oil compared with solvent extraction oil or pressed oil with dehulling or cooking pretreatment. Therefore, pressing dehulled flaxseed appears to offer advantages in organic flaxseed oil production. Thermal pretreatment is not recommended in pressing flaxseed oil. ivACKNOWLEDGMENTS The author would like to express her sincere appreciation to the following people: Dr. Dennis P. Wiesenborn, major adviser, for his advice, guidance, and encouragement throughout this project and in the preparation of this dissertation; and for financial support in pursuit of this degree. Dr. Earl C. Stegman, former department chair and committee member, for his encouragement, consideration, and suggestion for this study. Professor Leslie F. Backer, department chair and committee member, for his suggestions for conditioning flaxseed. Dr. Clifford Hall III, committee member, for his suggestion in oil quality consideration. Dr. Dean Steele, committee member, for his suggestion in statistical analysis and heat transfer calculation. Dr. James Coykendall, committee member, for his valuable contribution to this committee. Dr. Krishna K. Singh of the Central Institute of Agricultural Engineering (Bhopal, India) for his suggestion and support as a visiting scientist at North Dakota State University.Mr. Fuzhi Cheng, statistics help desk of NDSU, for assistance with the SAS program. Sincere thanks are extended to the kindness and hospitality from the faculty and staff of the Department of Agricultural and Biosystems Engineering. Special thanks are given to the following people: Ms. Kristi L. Tostenson for technical support throughout this project, helpful discussion, and her friendship. Ms. Nancy Kangas for oil quality analysis, helpful discussion, and her friendship. Ms. Jana Seaborn and Mr. James Moos for their assistance with research equipment. Appreciation is also given to those who have encouraged and helped me in the project. ‘This dissertation is dedicated with love to my husband, Chengli, and my daughter, zhengsheng (Betty). It would have been impossible for me to complete my project without their support and understanding. viTABLE OF CONTENTS ABSTRACT. : ACKNOWLEDGMENTS. . dopeacacd v CLARIFICATION OF CONTRIBUTIONS FOR MULTI-AUTHORED PAPERS...... we exddd LIST OF TABLES oe eeexiy, LIST OF FIGURES. . pevid NOMENCLATURE. eee) eee xix INTRODUCTION. ...... 1. Dissertation Organization... LITERATURE REVIEW. . 1. Flaxseed.. 1.1. O42., 1.2. Lignans..... 7 1.3. Mucilage. a ee a 1.4. Other components.............065 ee 2. Application of Flaxseeds..... 2.1, Application in the food industry.............. 2.2. Disease prevention and health promotion effect.... 2.2.1. a-binolenic acid..... : eo 2.2.2. Lignans... pela 2.3. Application in cosmetics. soar) 3. Quality and Stability of Flaxseed and Its Products....... viiTABLE OF CONTENTS (continued) Pretreatment of Oilseeds............. pocecoBosadasn 16 Gri, Conditaonings se ee eee ee ie 4.2. Cracking.. 4.3. Dehulling 4.5. Cooking 4.6. Other methods of seed preparation oe 5. Mechanical Pressing.. 5.1. Pressing equipment... 5.2. Operation parameters. 5.3. Pressing of flaxseed. PAPER 1. SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED FOR ORGANIC OIL... 1. Abstract... 2. Introduction.. 3. Materials and Methods... 3.1. Materials eso 3.2. Pretreatment. Ea 50 oo 20 3.2.1. Conditioning....... +30 3.2.2, Dehulling...... gogoodbecqdodoadcdnonaasane 31 3.3. Pressing... 3.4. Analysis..... viiiTABLE OF CONTENTS (continued) 3.4.1. Moisture content...... 3.4.2. Sediment content.. 234 3.4.3. Room-temperature hexane extraction........34 3.4.4. O41 content and oil quality..........6....35 3.5. Calculations. 3.6. Data analysis... ae Recultg)and Discussion eer eet ee eee 37 4.1. Moisture content and choke size influence..... 37 4.2, Variety influence............ 9 42 4.3. Pressing of dehulled omega flaxseed. 45 4.4. Oil and meal temperature.. 49 bE Conclusions) y 3 53 6. Acknowledgements....... 54 7. References....... 5 54 PAPER 2. ENERGY ANALYSIS IN THE SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED... 57 1. Abstract... 2. Introduction. 3. Materials and Methods. . 3.1. Materials and pretreatment... 3.2. Pressing and temperature collection............. 61 3.3, Analysis... ixTABLE OF CONTENTS (continued) 3.4. Calculations fe o5) 3.5. Data analysis 4. Results and Discussion.. 4.1. Fraction of hull removal influence on press performance. 4.2, Net enthalpy change. . 4.3. Heat loss.. 4.4, Mechanical energy input. . 5. Conclusion... 6. Acknowledgements. . 7. References. . 88 PAPER 3. QUALITY OF FLAXSEED OIL FROM SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED....... 91 1. Abstract... gebocaospecod09 eee od 2. Introduction Gonnbansaneeonsoaacose 3. Materiais and Methods........... ecdocdogdadudsegnan 95 3.1. Materials and pretreatments..... vee DB 3.1.1. Dehulling and conditioning....... +95 iQeiea)Cookings: 4 =96 3.1.3. Pre-heating.. +97 3.2. Room-temperature hexane extraction.. 98 3.3. Pressing and temperature measurement... 98TABLE OF CONTENTS (continued) 3.4. Experiment organization... eee 99 3.5. Analysis......... oe 100 3.6. Calculations..... -101 3.7. Data analysis.. +102 4. Results and Discussion. . +103 4.1. Pre-heating influence on pressing dehulled flaxseed. . eee ses +103 4.2. Cooking influence on pressing dehulled flaxseed -105 4.3. O41 quality comparison with different extraction methods. 5. Conclusion. . 6. Acknowledgments. 7. References...... ee 16 ca COMPREHENSIVE REFERENCES...... APPENDIX I. CALCULATION OF FRACTION OF HULL REMOVAL... APPENDIX II. ANALYSIS OF VARIANCE FOR TWO-FACTOR FACTORIAL DESIGN BY SAS 132 APPENDIX III. SEDIMENT CONTENT OF THE SCREW-PRESSED OIL...135 APPENDIX IV. STATISTICAL ANALYSIS OF NEST DESIGN BY SAS. . -136 APPENDIX V. ANALYSIS OF VARIANCE WITH SINGLE FACTOR BY SAS. . APPENDIX VI. BOUNDARY LIMITATION OF FREE CONVECTION..... +142 xiTABLE OF CONTENTS (continued) APPENDIX VII. TEMPERATURE INFORMATION COLLECTING AND PROCESSING BY MATLAB IN PRESSING WHOLE OMEGA FLAXSEED 143 APPENDIX VIII. ANALYSIS OF COVARIANCE BY SAS....... 158 APPENDIX IX. TEMPERATURE INFORMATION FROM SCREW PRESSING. .161 APPENDIX X. CALCULATION OF RADIATION HEAT LOSS FROM SCREW PRESSING 163 xiiCLARIFICATION OF CONTRIBUTIONS FOR MULTI-AUTHORED PAPERS Dr. D.P, Wiesenborn served as major adviser. His contribution in that capacity is reflected in the authorship of papers included in this dissertation. The degree candidate was responsible for all experimental determinations as well as data interpretation and manuscript preparations. Oil quality analysis was carried out by Nancy Kangas Slightly altered versions of Papers 1 and 2 of this dissertation have been accepted and sent for publication, respectively, as Zheng Y¥.L., D. Wiesenborn, K. Tostenson, and N. Kangas. 2003. Screw Pressing of Whole and Dehulled Flaxseed for Organic Oil. Journal of American Oil Chemists’ Society 80(10): 1039- 1045 Zheng ¥.L., D. Wiesenborn, K. Tostenson, and N. Kangas, Energy analysis in the Screw Pressing of Whole and Dehulled Flaxseed. Journal of Food Engineering (Submitted) Both papers were subject to peer review and benefited from the editorial comments of anonymous reviewers. xidiLIST OF TABLES Table Page Literature Review 1. Pressing oil recovery influenced by moisture content.. +24 Paper 1 1, Analysis of Variance for the influence of moisture content, choke size, and the interaction of moisture content and choke size on oil recovery and capacity. 42 2. Analysis of Variance for the influence of variety and moisture content on oil recovery and capacity... 48 3. Analysis of Variance for the influence of dehulling condition and moisture content on oil recovery, capacity, and productivity... 48 4. Effects of processing and storage on flaxseed oil quality....... 52 5. Analysis of Variance for the influence of the dehulling condition and moisture content on oil and meal temperature... xivLIST OF TABLES (Continued) Paper 2 Composition of whole and dehulled flaxseed and press meal... 2. Influence of fraction of hull removal on oil recovery, oil and meal temperature, and net enthalpy change by Analysis of Covariance........... 74 3. Summary of the energy change from pressing whole and dehulled flaxseed............ 000 ecee cence ee ee BL 4. Influence of fraction of hull removal on specific mechanical energy by Analysis of Covariance. Paper 3 1. Effects of pre-heating whole flaxseed before screw pressing... ea +104 2. Analysis of Variance for the influence of moisture content and pre-heat temperature on press performance and oil quality... + +104 3. Effects of cooking dehulled flaxseed before screw pressing......... ‘i 106 xLIST OF TABLES (Continued) Analysis of Variance for the influence of moisture content, cooking condition, andthe interaction of moisture content and cooking condition on press performance and oil quality when screw pressing dehulled flaxseed... -107 Effects of pretreatment and extraction methods on flaxseed oil quality.............4. aaa Appendix IX Average temperature information of pressing whole and dehulled flaxseed. 161 Comparison of meal temperature collected by CR10 data log and infrared thermometer... +++ 162 xviLIST OF FIGURES Figure Page Literature Review 1. Screw press..........055 ee eee) Paper 1 1. Oil recovery and capacity of pressing whole Omega flaxseed influenced by dry basis moisture content and choke size 2. Oil recovery and capacity of pressing whole flaxseed influenced by dry basis moisture content and variety. 3. Dehulling and dry basis moisture content influence on the oil recovery and productivity of pressing Omega flaxseed eee 46 4. The oil and meal temperature influenced by dry basis moisture content and dehulling condition.......... eee 50 Paper 2 1. Steady state mass and energy flows for the screw press. ed -62 2. Dry basis moisture content influence on oil recovery and productivity...... pe +73 xviiLIST OF FIGURES (Continued) 3. Dry basis moisture content influence on oil and meal temperature 4. Dry basis moisture content influence on net enthalpy change. . -78 5. Dry basis moisture content influence on specific mechanical energy.............. Paper 3 1. The relationship between oil recovery and seed moisture content influenced by cooking before screw pressing dehulled flaxseed... 110 Appendix III Sediment content of the screw-pressed oil and dehulling influence................00005 Peso) xviiiFER bebo D x EQORS NOMENCLATURE Fraction of hull removed (%) heat transfer area (m’) specific heat (J/(g-K)) diameter (m) convection heat transfer coefficient (W/(m*-°c)) thermal conductivity (W/(m-°C) axial position with respect to feed end of press barrel (m) mass fraction mass flow rate (g/s) heat loss (W) temperature (°C) energy input of the screw (W) oil content (%) subscripts ae a ESPON VO SHEE HOA oe ash press barrel carbohydrate conductive pure embryo fat pure hull press head hot surface dehulled flaxseed embryo meal oil protein reference radiation raw material screw water convective whole flaxseed xixINTRODUCTION Flaxseed is unique among oilseeds because of its exceptionally high content of alpha-linolenic acid (ALA, 18:3n-3) and lignans. Flaxseed contains 35 to 45% oil, of which 45 to 52% is ALA (Bhatty, 1995). Its ALA content is outstanding among established oilseeds in North America. ALA is classified as an omega-3 fatty acid, a group that also includes long-chain metabolites of ALA. Omega-3 fatty acids have anti-inflammatory, anti-thrombotic, and anti-arrhythmic properties (Simopoulos, 1999). Fish oil is the traditional source of dietary omega-3 fatty acids while flaxseed oil can be used as a vegetarian source of dietary omega-3 fatty acids. The flaxseed hull is a concentrated source of lignan, ive., 30.9 mg/g hull vs. 12.9 mg/g whole seed (Madhusudhan et al., 2000). Axelson et al. (1982) and Kurzer et al. (1995) concluded that lignans might possess impressive cancer- preventive properties, especially against breast and colon cancer. Solvent extraction and mechanical pressing are the traditional methods for oil and fat extraction. Mechanical pressing is required by the organic food industry because no good alternative to solvent extraction exists. Screw pressing is a simple, flexible, safe, and continuous mechanical pressing procedure (Singh and Bargale, 2000). However, screw 1pressing provides relatively low oil recovery. The low oil recovery of mechanical pressing can be partially overcome by suitable pretreatments of the flaxseed, i.e., cracking, dehulling, conditioning, flaking, pre-heating, and cooking. Conditioning, dehulling, pre-heating, and cooking were the four major pretreatment methods used in this project. Adjusting pressing parameters can improve oil recovery, and ternal pressure and temperature of the screw press will be discussed in this dissertation. The friction inside the screw press increases the temperature of the materials. ALA is sensitive to heat, oxygen, and light. To stabilize this nutritional polyunsaturated fatty acids, the process temperature should be as low as possible. All forms of excess heating should be avoided (Shukla, 2003). “Cold pressing oil’ was defined as vegetable oil obtained by mechanical procedures, e.g., expelling or pressing, without the application of heat (FAO/WHO, 1999). Energy input into the materials during screw pressing is an important parameter in the design of the screw press (Singh and Bargale, 2000) and the modeling of the screw press operation (Omobuwajo et al., 1997). If measured directly by torque and rotating speed, the accurate screw torque meter for bench scale equipment is expensive. If measured 2indirectly through the electrical energy input, the efficiency of the motor should be taken into account (Singh and Bargale, 2000), but motor efficiency data are often not available. Calculating mechanical energy input from a thermal energy balance appeared to be a simple, inexpensive alternative. Analysis of mechanical energy input and its dissipation will also help us understand the principle behind the increase in oil temperature during screw pressing. The overall objective of this research is to obtain high-quality flaxseed oil with high oil recovery by suitable pretreatments and screw pressing. The specific objectives of this research are 1) to characterize the relationship between pretreatment methods (conditioning, dehulling, pre-heating, and cooking) and the oil recovery of screw pressing; 2) to elate the press parameters (pressure and temperature) to the yield and quality of oil; 3) to reveal the oil temperature increase mechanism by analyzing mechanical energy input dissipation of screw press; and 4) to relate process conditions (pretreatment methods, especially thermal treatment, and extraction methods) to the quality of flaxseed oil.1. Dissertation Organization The body of this dissertation is organized into three papers prefaced by the introduction and literature review, and followed by the general conclusion and appendices containing experiment data, equation deduction, and SAS and Matlab programs and results. The first paper describes the screw pressing of the flaxseed, which includes the influence of pretreatment and screw press parameters on oil recovery and oil quality. The second paper addresses the steady state mass and heat analysis in the screw press procedure and then calculated mechanical energy input by the calculation of net enthalpy change and heat loss. The third paper evaluates the oil quality from different pretreatment and extraction methods, and special efforts are paid to thermal treatmentsLITERATURE REVIEW 1. Flaxseed Flaxseed or linseed is an ancient crop; its botanical name is Linum usitatissimum. Flaxseed has been cultivated for at least 5000 years. Initially, flaxseed was used mostly for fiber processing, and only a limited amount of evidence dealt with its usage as human food (Judd, 1995). Although flaxseed has been cultivated since ancient times, it is not a major oilseed crop. The world production of flaxseed has remained relatively static, between 2.45 and 2.90 million metric tons and this amount accounted for only 1% of the world’s oilseed production (Daun et al., 2003). Flaxseed is planted in the following countries (in decreasing order): Canada, China, the United States, and India (Daun et al., 2003) Flaxseed was formerly much more important in North America for its “linseed oil” used in paints and coatings The high double bond content accounts for the desirable properties of linseed oil as a coating (Wicks et al., 1992) Recently, the food industry in Europe and North America has shown an increased interest in flaxseed consumption primarily because flaxseed is high in alpha-linolenic acid (ALA), lignan, and soluble fiber; and may have anti-cancer and cardiovascular benefits (Bhatty, 1995; Setchell, 1995)Mature flaxseeds are flat, oval, and beaked or pointed at one end. The surface of the seeds is smooth and highly polished. Their colors vary from dark brown ‘to yellow. Flaxseed contains a seed coat or true hull (also called testa), a thin endosperm, two embryos, and an embryo axis. Embryos form 55% of the total weight of hand-dissected flaxseed; the seed coat and the endosperm account for 36% of the total weight; and the embryo axis is 4% (Bhatty, 1995). 1.1. 042 Flaxseed contains 35 to 45% oil. Bmbryos are the major oil storage tissues, containing 75% of the seed oil (Bhatty, 1995). The oil content of the embryo axis is 44.9% and that of embryos is 51.0%. The combined testa and endosperm contain 22.9% oil (Dorrell, 1970). Flaxseed oil is present as triacylglycerols in discrete oil bodies with an average diameter of 1.3 pm. Neutral lipids are the major constituent of these oil bodies, accounting for 98% of the total lipids (Tzen et al., 1993). Flaxseed contains 5 to 6% palmitic acid (16 ), 3 to 6% stearic acid (1 }, 19 to 29% oleic acid (18:1n-9), 14 to 18% linoleic acid (18:2n-6), and 45 to 52% ALA (18:3n-3) (Bhatty, 1995). The ALA content is outstanding in plant sources. The tissue’s fatty acid composition is not 6homogeneous. The linolenic contents in embryos, testa, and endosperm are all higher than that in the embryo axis (Dorrell, 1970). Although flaxseed oil is naturally high in anti-oxidant nutrients, for example, beta-carotene, traditional flaxseed oil is easily oxidized after being extracted and purified (Holstun and Zetocha, 1994). 1.2. Lignans Lignans are a class of diphenolic compounds containing a dibenzylbutane skeleton structure (Rickard, 1997). Analyses of some foods have shown that flaxseed is the richest source of two types of lignans: secoisolariciresinol (SECO) and matairesinol. SECO occurs in the form of secoisolariciresinol diglucoside (SDG) in flaxseed. The SDG content was 11.7 to 24.1 mg/g in defatted flaxseed flour and 6.1 to 13.3 mg/g in whole flaxseeds (Johnsson et al., 2000). Madhusudhan et al. (2000) developed a dry mechanical method to produce a hull- vich fraction from flaxseed, and the lignan content of that fraction was 30.9 mg/g vs. 12.9 mg/g whole seed. 1.3. Mucilage The mucilage accounts for about 8% of the flaxseed weight. It is composed primarily of polysaccharides. The acid .hydrolysis products of these polysaccharides are L-galactose; D-xylose; L-arabinose; L-rhamnose; D-galacturonic acid; and, perhaps, traces of D-glucose. The mucilage can be extracted by water and has good foam stability properties (Mazza and Biliaderis, 1989). 1.4. Other components Flaxseed is comprised of approximately 30% dietary fiber, 20% protein, 4% ash, and 6% moisture. The proximate composition varies with sample source and analytical methodology, and the variation due to sample source is uncontrollable (Daun et al., 2003). 2. Application of Flaxseeds 2.1. Application in the food industry Traditionally, flaxseed was used as an ingredient in breakfast cereals, breads, and baked goods in some European countries and in North America (Kolodziejcayk and Fedec, 1995). Flaxseed oil has the highest content of ALA of the well- established crops--about 50 percent. Unrefined flaxseed oil can be added directly to dressing to make it more healthful. Flaxseed oil has a distinctive nutty flavor. Both the health- conscious and flavor-centered consumers will enjoy it. In 8addition, unrefined flaxseed oil contains a high amount of natural anti-oxidants, e.g., beta-carotene, which enhance the shelf life of the final product (Brandt, 2000). One of the biggest challenges in developing flaxseed oil dressings is protecting the ALA from degradation. Polyunsaturated fatty acids are more fragile than monounsaturated or saturated fatty acids, so the ALA in flaxseed oil must be protected from light, oxygen, and heat. Packaging the dressings in glass bottles that have a full overwrap sleeve is a protection method used by Spectrum Naturals, Inc. of Petaluma, California (Brandt, 2000). Both liquid and encapsulated cold pressed flaxseed oils are available in the health food market (www.barleans.com and www.wholehealthmd.com). Flaxseed oil may replace up to 25% of the milk fat in a frozen dessert resembling ice cream and result in a product containing more ALA than does standard ice cream (Hall and Schwarz, 2002). 2.2. Disease prevention and health promotion effect Flaxseed has a long tradition of use in folk medicine. Flaxseed was used as a cure for gastric disorders; its laxative properties have recently been confirmed in well- controlled human trials. The mucilage, which is abundant in the seed, is thought to be the active ingredient in such 9applications. Flaxseed oil was used for burn treatment (Kolodziejezyk and Fedec, 1995). 2.2.1. a-Linolenic acid (ALA) Flaxseed can raise ALA and long-chain omega-3 fatty acids in both plasma and erythrocyte lipids in humans, as well as decrease postprandial glucose responses and raise urinary thiocyanate excretion. Up to 50 g flaxseed/day, that is, about 10 g ALA/day, is palatable, safe, and may be nutritionally beneficial in humans (Cunnane et al., 1993). Consumption of flaxseed has also been shown to reduce total and low-density-lipoprotein cholesterol as well as platelet aggregation (Hasler, 1998). The omega-3 fatty acids include ALA (18:3n-3), an essential fatty acid, and its long-chain metabolites. In omega-3 fatty acids, the first double bond is located at the third carbon from the methyl end of the hydrocarbon chain For omega-6 fatty acids, it is located at the sixth carbon. Fish oil is the tra ional source of omega-3 fatty acids that contains both EPA (eicosapentaenoic acid, 20:5n-3) and DHA (docosahexaenoic acid, 22:6n-3). Consumption of flaxseed ALA leads to significant increases in tissue EPA but not DHA in humans (Mantzioris et al., 2000) 10Human beings should consume a diet that contains a certain ratio of omega-3 and omega-6 essential fatty acids Over the past 100 to 150 years, the consumption of vegetable oils from corn, sunflower seeds, safflower seeds cottonseeds, and soybeans increased, so the consumption of omega-6 fatty acids increased greatly. The ratio of omega-6 to omega-3 fatty acids is 20:1 to 30:1 in Western diets today (Simopoulos, 1999). The recommended ratio of omega-6 to omega-3 fatty acids is in the range of 4:1 to 10:1 for adults, and omega-6 and omega-3 fatty acid intakes should account for at least 3 and 0.5% of energy intake respectively (Carter, 1993). Omega-3 fatty acids have anti-inflammatory, anti- thrombotic, anti-arrhythmic, hypolipidemic, and vasodilatory properties. These beneficial effects of omega-3 fatty acids have been shown in the secondary prevention of coronary heart disease; hypertension; type 2 diabetes; and, in some patients with renal disease, rheumatoid arthritis, ulcerative colitis, Crohn's disease, and chronic obstructive pulmonary disease as reviewed by Simopoulos (1999). Omega-3 fatty acids are important constituents of heart cell membranes, and adequate levels of them are needed to optimize heart function. Omega-3 fatty acids can protect the heart against lethal ventricular arrhythmia, or irregular aLheartbeats. Omega-3 fatty acids may reduce platelet activity and fibrinogen concentrations, and thus could be viewed as anti-thrombotic. They lessen the production of proinflammatory mediators, and they also reduce the cell growth factors responsible for the proliferation of cells in artery walls that cause narrowing of arteries. Omega-3 fatty acid consump’ n led to reduced thromboxane production and increased prostacyclin production, resulting in decreased platelet aggregation and increased blood vessel dilation (Haumann, 1997b) Vegetarians have lower platelet and plasma concentrations of omega-3 fatty acids than do omnivores. ALA from flaxseed has a beneficial effect on omega-3 fatty acid concentrations of platelet phospholipids and plasma lipids in vegetarian males (Li et al., 1999). 2.2.2, Lignans The flaxseed hull is a concentrated source of lignan. Compelling studies funded by the National Cancer Institute have shown that lignans may possess cancer-preventative properties (Axelson et al., 1982). Lignans offer protection against breast and colon cancer due to their anti-estrogenic and/or anti-oxidative effects (Kurzer et al., 1995). In addition, epidemiological data show that lignans have anti- 12mitotic, anti-tumor, and anti-oxidant activities (Carter, 1993). The two primary mammalian lignans are enterodiol and its oxidation product, enterolactone. They can be formed in the mammalian intestinal tract by bacterial action on plant lignan precursors. Flaxseed is the richest source of mammalian lignan precursors. Because enterodiol and enterolactone have been shown to possess weakly estrogenic and anti-estrogenic activities, they may prevent estroge: dependent cancers. The ingestion of 10 g of flaxseed per day can reduce breast cancer risk (Hasler, 1998). Thompson et al. (2000) found that dietary modification with flaxseed and its components, such as lignans, could reduce tumor growth in patients with breast cancer in a placebo-controlled clinical trial. Demark-Wahnefried et al. (2001) found that a flaxseed-supplemented, fat-restricted diet might affect prostate cancer biology due to high lignan and omega-3 fatty acid intake. Flaxseed lignan spe and its mammalian lignan metabolites, enterodiol and enterolactone. also had anti-oxidant activity (Kitts et al., 1999) 2.3. Application in cosmetics The application of flaxseed oil in cosmetics has received interest recently. Flaxseed oil can be used in the 13treatment of skin conditions, such as eczema, acne, and skin dryness, and it is also used in skin cleaners and liquid soaps (Kolodziejczyk and Fedec, 1995). 3. Quality and stability of Flaxseed and Its Products ‘The unsaturated bonds present in the ALA and linolenic acid of flaxseed oil represent active sites that can react with oxygen, even at low temperatures. The reaction is autoxidation, and it forms primary, secondary, and tertiary oxide on products that impart a rancid odor and flavor. Therefore, the process is also called rancidification. Lipid oxidation also occurs in living cells. In this case, it is called lipid peroxidation (Liu, 1997). Flaxseed products are stable despite their high ALA content. Storing milled flaxseed at ambient temperatures for more than 4 months did not cause noticeable changes in quality. The endogenous antioxidants in the milled flaxseed may account for this stability (Malcolmson et al., 2000). Flaxseed products can tolerate heat to a certain extent. Heating at 178°C for 1.5 hours did not change the ALA content in the whole flaxseed. ALA decreased from 55.1 to 51.3% in ground flaxseed under the same conditions, and ALA content dropped to §1.7% in lipid extracts under the same conditions (Chen et al., 1994). 14Crushing oilseeds to produce vegetable oils creates a contact interface between the triacylglycerols and the native enzyme system of the seed. The active enzymes can catalyze oxidation and hydrolysis reactions that will deteriorate the quality of the oil during this contact. The three major modes of oi] degradation are hydrolysis, oxidation, and thermal decomposition (Gupta, 2000). Oil hydrolysis can by measured by free fatty acid content or acid value (Gupta, 2000). Oil oxidation can be measured by peroxide value, which measures hydroperoxides formed by the reaction of unsaturated oil with triplet or singlet oxygen (White, 2000). The hydroperoxides formed from linolenates oxidation all have a conjugated diene system, so conjugated diene content can be used as an indicator of ALA quality (Nawar, 1985). However hydroperoxides begin to decompose as soon as they are formed and they break down in several steps, yiel: ig a wide variety of decomposition products (Nawar, 1985). Thermal decomposition is a combination of oxidative and thermolytic degradation of the oil (Gupta, 2000). The FAO/WHO (1999) standard for virgin oils and cold pressed fats and oils required that the peroxide value be lower than 15 meq peroxide/kg oil, and the acid value should be lower than 4.0 mg KOH/g fat or oil, or 2.0% free fatty acids as oleic. 15Heating the oilseed before extraction can inactivate the enzymes that catalyze the hydrolytic reaction in oil. However, the activity of enzymes can increase when seed temperature increases until the temperature becomes sufficiently high to inactivate those enzymes. Therefore, the inactivation threshold temperature should be attained as fast as possible to avoid undesired enzymatic actions (Veldsink et al., 1999). 4. Pretreatment of Oilseeds 4.1. Conditioning The moisture content of the oilseed will affect the efficiency of cracking and dehulling (Tandy, 1991). Changing the m ‘ture content of oilseeds will change their plasticity and, hence, change their pressing properties (Liu, 1997). Heated air is used on oilseeds to achieve some loss of water, and then, cooler air removes the residual moisture- laden air. After drying, the oilseeds must be stored for 5 to 20 days to allow the moisture coi tent to reach equilibrium in every part of the seed (Liu, 1997). The typical time for flaxseeds to reach their equilibrium moisture content is 1 to 5 weeks depending on the temperature and humidity (Jayas et al., 1989). 164.2. Cracking The objective of cracking is to break the oilseeds into small pieces for dehulling and flaking. The oilseed is cracked by passing it between two corrugated rolls turning at high speeds in opposite directions. The speed of the two rolls is slightly different. This speed difference, together with the sharp edges of the rolls, cracks the seed (Liu 1997). 4.3. Dehulling The common reasons for removing the hull of most oilseeds are to improve the flavor, to increase the protein content of the meal, and/or to increase oil productivity (Fils, 2000). However, flaxseed can also be dehulled to recover the hull for use as a lignan concentrate. Dehulling significantly concentrated both major components (i.e., oil and protein) and minor components (i.e., phenolic acids and cyanogenic compounds) (Oomah and Mazza, 1997). Therefore, the hull and the embryo can be used separately to obtain two high-value products: ALA-rich flaxseed oil and lignan The fibrous hull of the flaxseed is smooth and firmly attached to the embryo, and the flaxseed is flat rather than round like a soybean; therefore, the flaxseed is very difficult to dehull (Freeman, 1995). 17Furthermore, the presence of the hull in pressing can help generate more frictional forces to make pressing more effective. The hull also serves as a good porous matrix for pressing the oil (Singh and Bargale, 1991). 4.4, Flaking Oilseeds are flaked by passing them between horizontal, smooth rolls to produce flakes of typically 0.3-0.4 mm thickness, and the pressure of the rolls is maintained by springs under hydraulic pressure (Fils, 2000). Flaking increases the surface area of the oilseed, so more oil cells will be found at or near the surface. Flaking also contributes to the rupturing of the cell walls. Because the cell walls are almost impervious, the cell walls must be broken by flaking operations to allow the oil to come out easily (Ajibola, 1990). 4.5, Cooking Cooking generally improves oil yield and process capacity. Cooking may also improve pressed oil and/or meal quality by preventing undesirable enzymatic reactions. In contrast, excessive cooking can seriously reduce the yield of oil (Reuber, 1992) and oil quality (Unger, 1991) during the pressing processes. Thus, there is an optimal degree of 18cooking, and this degree will vary with seed type and screw press design. Many changes take place within the seeds during cooking. 0i1 is present in uncooked seed as an emulsion, and protein serves as a surface-active agent to stabilize this emulsion (Norris, 1982). Cooking denatures the protein, and then, oil droplets can coalesce into larger droplets, In addition, cooking can lower oil viscosity, so the fluidity of the oil may increase. These changes all help ease oil extraction from the oilseed. If the seed has been dehulled, the denatured protein replaces the hull fiber as the cohesive agent that maintains a matrix of meal while oil is removed. Another advantage of protein denaturation is the inactivation of enzymes, some of which (lipase, lipoxygenase, and myrosinase) may degrade oil or meal quality. Cooking can also increase the plasticity of the oilseeds, so the oilseeds may be more suitable for the pressing operation (Liu, 1997). Singh et al. (2002b) observed that cooking of crambe seed provided higher oil recovery in screw pressing from 67.9 to 82.5% compared with from 63.5 to 78.5% for uncooked seed when moisture content decreased from 7 to 3.5% (dry basis). 194.6. Other methods of seed preparation Pre-heating raw seed increased oil output and efficiency in pressing sunflower seed (Jacobsen and Backer, 1986). Soaking the flaxseed in water will reduce the gum content of the flaxseed, thereby increasing the oil recovery (Singh and Bargale, 1990). + Mechanical Pressing Mechanical pressing of oilseeds provides a no-solvent method for oil recovery and is particularly important when studying novel oilseeds. The screw press construction is simple and sturdy; therefore, the initial investment is low The screw press is easily maintained and operated in the laboratory without much supervision. The feedstock needed is small, so it can be adapted quickly to process different varieties of vegetable seeds. The pressing is a continuous operation, and the products are made within a few minutes of processing. The simplicity and safety of pressing are advantages over the more complete oil recovery obtained by solvent-extraction equipment. The 1990 Clear Air Act, which set strict requirements on solvent extraction plants, limits emissions of volatile organic compounds and hazardous air pollutants. If the facility exceeds emission limits, the act 20requires record maintenance and purchase of a “permit” (Haumann, 1997a) . Compared to solvent-extracted crude oil, mechanical pressed oil is remarkably stable to oxidation. Pressed oil contains lower amounts of peroxides, free fatty acids, trace metals, sterols, phosphatides, unsaponifiable matters, moisture, and volatile matter while it contains the same amounts of pigment, fatty acids, and triglycerides as crude solvent-extracted oil. The stability of pressed oil is due to the presence of natural anti-oxidants (carotenoids and tocopherols), and the low levels of phospholipids and peroxides (Said, 1998). The pressed oil is termed “virgin oil” because no solvent is used, and it can be sold refined or unrefined (Haumann, 1997a). The disadvantage of mechanical pressing is the ely low oil recovery. However, a small expeller can achieve over 90% oil recovery from oilseeds (Sivakumaran and Goodrum, 1988) 5.1. Pressing equipment an oilseed screw press, as illustrated in Figure 1, has a horizontal main shaft carrying the screw assembly that is formed integrally with the shaft. The screw rotates within a barrel. The screw is designed so that the volume displacement 21at the feed end of the press is considerably greater than at the discharge end. As a result, when the material is conveyed from the feed end to the discharge end, the pressure increases, and oil is expelled through the small openings on the barrel. At the discharge end, the inside diameter of the choke controls the operating pressure. The heat generated because of friction can be dissipated by cooling the cage and shaft with water (Khan and Hanna, 1983) Raw Seed CATR Figure 1. Screw press 225.2. Operation parameters The yield and quality of oil during pressing is influenced by the particle size, seed moisture content, period of pre-heating, temperature, the pressure inside the screw press barrel, and the design of the press itself The oil yield will increase with an increase in pressure (Adeeko and Ajibola, 1990). The oil in the seed is contained in sacs or in fibrous capillaries. when pressure is applied, the volume of the capillaries is reduced, and the oil is expelled. However, the increasing pressure narrows, shears, and eventually seals the capillaries. Therefore, the screw press has a practical limit for its oil recovery (ward, 1976). The moisture content of oilseeds significantly influences the screw press performance. Its influence is summarized in Table 1. The rate of oil flow during expression will increase by increasing the temperature, heating time, and particle size. Increasing temperature and heating time will also increase free fatty acid content, peroxide value, and color intensity of the oil (Adeeko and Ajibola, 1990). 23Table 1. Pressing oil recovery influenced by moisture content MC. Range oil Oit Material (8) (w.b.) Recovery Recovery Reference (highest) (lowest) Crambe 3.5 to 8d 78.98 67.7% Singh et al (Uncooked) (at 3.5) (at 8.4%) 2002 Crambe 3.5 to 8.4 80.9% 69.08 Singh et al. (cooked) (at 3.5) fat 8.4%) — 2002b Rapeseed 5.1 to 11.1 90.2% 77.3% Singh and (at 7.5) (at 11.18) Bargale, 2000 Soybean 8.2 to 19.3 66.8% 54.678 Singh and (at 17.28) (at 8.2%) Bargale, 1991 Linseed 5.3 to 11.1 81.35% 70.26% Singh and (at 9.18) (at 11.248) Bargale, 1990 Soybean 10.6 to 12.0 67.948 63.71% Nelson et (at 11.05%) (at 10.59%) al., 1987 Sunflower 11 and 6 Bee 78% Jacobsen and seed (at 6%) (at 118) Backer, 1986 cottenseed 3.1 to 11.0 23.8% 14.98 Khan and (at 5.35%) (at 3.108) Hanna, 1983 5.3. Pressing of flaxseed Although flaxseed has high oil content (35 to 45%) pressing it by a single pressing at moderate temperatures is not satisfactory. It is common to break up the oil cake derived from the first pressing and subject it to a second pressing to recover additional oil. The average yield of oil from commercial processing of flaxseed with normal moisture content is approximately 34 kg oil per 100 kg flaxseed. This yield usually means that the residual oil content of the cake is more than 10%. A second pressing allows recovery of an additional few percent; however, it adds labor and equipment costs, and the oil will be of lower quality. Expellers 24designed to develop increased pressures are also used to maximize the recovery of the oil (Kolodziejczyk and Fedec, 1995). The delicate flaxseed oil deteriorates very easily without special processing and handling. Under normal conditions, frictional heat may raise oil temperature flaxseed should be extracted at cold considerably. Therefore processing temperatures--under 48.9°C (120°F)--while eliminating the destructive effects of light, heat, and oxygen (Kolodziejczyk and Fedec, 1995) Cold pressed oil is a term without legal definition in the United States, and the processes involved in the oil production vary greatly. In the United Kingdom, this type of product is regulated by a law that forbids high-temperature processing and recommends a maximum oi1 temperature of 50°C when exiting the screw press. In addition, cold pressed seed oils should not undergo physical or chemical processes besides the mechanical press (Panfilis et al., 1998). The flaxseed oil industry feels cold pressed oil should be produced under a temperature lower than 35°C and under low- oxygen conditions in the screw press. These conditions can be readily achieved by using expellers fitted with water-cooled shafts (Kolodziejczyk and Fedec, 1995) 25PAPER 1 SCREW PRESSING OF WHOLE AND DEHULLED FLAXSEED FOR ORGANIC OIL 1. Abstract Flaxseed oil is a rich source of dietary omega-3 fatty acids and is commonly obtained by cold pressing whole seed. Furthermore, flaxseed hulls are emerging as a valuable lignan-rich product for functional food use; therefore, the pressing characteristics of dehulled seed should be understood. Screw press performance was measured for the pressing of whole and dehulled flaxseed. When whole Omega flaxseed was pressed through a 6 mm choke, an inverse relationship between seed moisture content (6.1 to 11.6% range) and oil recovery (70.1 to 85.7%) was observed. However, a peak in oil recovery from pressing dehulled Omega flaxseed of 72.0% was found at 10.5% moisture content in the moisture content range of 7.7 to 11.2%. Although oil recovery from dehulled Omega flaxseed was lower than from whole Omega flaxseed, the weight of oil produced from dehulled omega flaxseed per unit time was higher. The dependence of capacity on moisture content was less evident with the 6 mm choke than with the 8 mm choke. An inverse relationship between the moisture content of whole flaxseed and the oil and meal 26temperature was observed. The oil and meal temperatures from pressing dehulled flaxseed were significantly lower than those from whole flaxseed. Therefore, pressing dehulled flaxseed appears to offer advantages in organic flaxseed oil production. 2. Introduction Flaxseed (Linum usitatissimum) is unique among oilseeds because of its exceptionally high content of a-linolenic acid (ALA, 18 n-3) and lignans. ALA is classified as an omega-3 fatty acid, a group that also includes long-chain metabolites of ALA. Omega-3 fatty acids have anti-inflammatory, anti- thrombotic, and anti-arrhythmic properties. These beneficial effects of omega-3 fatty acids have been shown in the secondary prevention of heart disease, hypertension, type 2 diabetes, and other medical conditions (Simopoulos, 1999). Flaxseed contains 35 to 45% oil, of which 45 to 52% is ALA (Bhatty, 1995). The seed embryo is the major oil storage tissue, containing 75% of the seed oil. The ALA content of flaxseed oil is outstanding among established oilseeds in North America. Solvent extraction and mechanical pressing are the leading methods for commercial oil extraction. Mechanical pressing is allowed by the organic food industry; however, 27solvent extraction with petroleum distillates, such as hexane, is not allowed (USDA, 2000). Omega-3 fatty acids are sensitive to heat, oxygen, and light; thus, flaxseed is usually cold pressed. “Cold pressing” is not a well-defined term, and the legal definition is different or non-existent in some countries. For example, in order to be labeled “cold pressed" in the United Kingdom, oil temperature when exiting the screw press should be less than 50°C (Panfilis et al., 1998). Pressing temperatures are rarely reported in scientific literature, with one report of exiting oil temperatures less than or equal to 70°C (Singh and Bargale, 2000) . Mechanical screw presses typically recover 86 to 92% of the oil from oilseeds (Singh and Bargale, 2000). Adjusting pressing parameters can improve oil recovery; for example. increasing the internal pressure results in a decrease of the residual oil in the meal (Jacobsen and Backer, 1986). Oil recovery can also be enhanced by suitable pretreatment of the oilseed, i.e., cracking, dehulling, conditioning, flaking and cooking (Fils, 2000). The importance of raw material moisture content in the screw press has been studied for a wide range of raw materials (Singh and Bargale, 1990, 2000; Fils, 2000 Wiesenborn et al., 2001; Singh et al., 2002). Little has been published on screw pressing flaxseed for edible use. Singh 28and Bargale (1990) found that adjusting moisture content and a soaking treatment can influence the oil recovery significantly when screw pressing flaxseed The common reasons for removing the hull of most oilseeds are to improve the flavor, to increase the protein content of the meal, and/or to increase oil productivity (Pils, 2000). However, flaxseed can also be dehulled to recover the hull for use as a lignan concentrate. Lignans offer protection against breast and colon cancer due to their anti-estrogenic and/or anti-oxidative effects (kurzer et al 1995). The meal from pressing dehulled flaxseed may be a good feed for non-ruminant animals because of its low fiber content and high protein content, and because the residual oil may be a good source of ALA for fish and poultry (National Research Council, 1993; VanElswyk, 1997). However, dehulled flaxseed (embryo) cannot be readily pressed using a process configured for pressing whole flaxseed because of the high oil content and low fiber content, which results in a particularly soft material. The objective of this research was to obtain high flaxseed oil recovery by suitable pretreatment and press parameters from whole and dehulled flaxseed (embryo). Two kinds of pretreatments (moisture content adjustment and dehulling) and two kinds of press parameters (pressure and 29temperature) were studied regarding their effect on oil recovery, oil quality, capacity, and sediment content. Two commonly used edible varieties of flaxseed (Omega and Neche) were compared as well 3. Materials and Methods 3.1. Materials Two varieties of flaxseed were used: a dark-brown variety (Neche) from Werth Certified Seeds (Lehr, ND) and a golden-yellow variety (Omega) from Reimer’s Seed Farm (Carrington, ND). Seeds were stored at 5°C and equilibrated over night in sealed polyethylene bags to room temperature before use. 3.2. Pretreatment 3.2.1. Conditioning To increase moisture content, a calculated quantity of distilled water was sprinkled on the flaxseed and was thoroughly mixed by hand. The seed clumps formed by direct water addition were removed using a 9.5 mm (3/8-in.) sieve. To decrease moisture content, flaxseed was spread on a plate to a depth of less than 1.5 cm and then kept in a gravity convection oven (Model 18EG, 1420 W, and 120 v) at less than 50°C until the desired moisture content was attained. The 30conditioned flaxseed was stored in a closed polyethylene bag at 5°C for more than 5 days for equilibration. 3.2.2. Dehulling Flaxseed (6.8% dry basis moisture content) was manually and continuously fed into a model VSH-8088 Huller (Codema, Inc., Maple Grove, Minnesota) at 400 to 500 kg/hr using a rotor tangential speed of 48 m/s. Fines were removed using a sifter (Rotex, Style No. 12, The Orville Simpson Co., Cincinnati, OH) with a 1.0 m long x 0.4 m wide 18 mesh screen. The embryo fraction was obtained from this sifted product using a gravity table (Forsberg, Model 10-M2, Thief River Falls, MN). 3.3. Pressing A Komet screw press (Model § 87G, IBG Monforts Gmbh & Co., Monchengladbach, Germany) was used to press the flaxseed in one pass. Samples were fed from the hopper to the press on demand by gravity. The length of the press barrel was 95.8 mm, and the constant inside diameter of the press barrel was 75.1 mm. The length of the shaft was 198.3 mm, and the constant outside diameter of the shaft was 53.7 mm. The choke (or die) at the meal discharge end of the screw press had an adjustable inside diameter of 6 or 8 mm. An R8 shaft (16 mm 31