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    Process for Extraction of Pectin

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    Process For Extraction of Pectin

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    Ugur Tuc

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    © All Rights Reserved
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    «2 United States Patent Jensen et al. (10) Patent No.t (4s) Date of Patent: US 8,592,575 B2 Nov. 26, 2013 (54) PROC FOR EXTRACTION OF PECTIN (75) Inventors: Soren Vodstrup Jensen, Lille Skonsved (DX); Susanne Oxenball Sorensen, \allensbeek Strand (DK); Claws Rolin, Koege (DK) (73) Assignee: CP Keleo Aps (DK) () Notice: Subject to any disclaimer, dhe term ofthis patent is extended or adjusted under 35, U.S.C. 154(0) by 111 days (21) Appl. Nos 1984381 (22) Filed: Jun. 6, 2011 (65) Prior Publication Data US 2012003099461 Dac. 6,2012 (51) Inch. CTH 106 (2006.01) co7H 108 (2006.01) (2) US.c. usec 516/128 (58) Field of Classitication Search None ‘See application file for complete seach history. 66) References Cited US. PATENT DOCUMENTS. 40163si a + schinas 5162 4268533 A Wiliams eal 1850 A ‘Manabe eal SIME A Gia ‘672.030 BL Wat 6207194 BL Gin ‘677.000 BD Nieta 685536 BL ‘Buco t a 791986 B2 Niet. 20030064183 AL Gerth etal 200s 0176677 AL Dal Fara etal dooso0s9302 AL Chrisencen 26150 20060171996 AL Sala 21070202283 AL Kalo etal 20090110798 A Gisck FOREIGN PATENT DOCUMENTS: oN Ss105165 A 41987 roy N7100163 A 71988 oO 00106 A 31998 ow Isl0iss A 2001 roy 1o1sigs3s A 9.2000 ry 21d! AL—12009 GB SSeH08 A 1071983 RU 2101294 CL L998 RU 2119497 C1 RU 2123266 C1 RU 2140927 C1 RU disTIN0 C2 RU a RU o RU 2346s Cl wo ouissi7 wo 9749298 wo 039168 wo 2004020472 wo 2o10006621 ‘OTHER PUBLICATIONS. Joye etal. Caibohyate Polymers 43 (2000) 337-3 YVoldashevaetal ,“Petin Substancesof Sugar Beet Pulp" Chemisty cof Natal Compounds vo, 30, No, 4 1958, CBV02680785, Intemational Seach Rept for PCTIEP2O12 055425. niol Aug 8 2012 ‘Wren Opinion of he Iterations Searching Autor for PCT EP2012055425, mail Aug 8,201 Rolin, et al, “Pectin, Chaper 12 in S. Dmitri (ed), Polysae- aries Sirsa Diversity and Functional Versi, Mared-Dek- ker Ine NY, 1998, Devarcs, tal, Carboy Polym 4, 1984, 89 Koutala eal, Food Chemistry, 106, 2008, 1202 Kouta ltern Journal Fod Seience Technolgy, 4,200, 1809, Fishmanet al, Food Hydrol, 20,2006, 1170, * cit by examiner Primary Examiner —Layla Bland (78) Antornes, Agent, or Firm Brennan LLP Sutherland, sill & 7 ABSTRACT Embodiments of the processes provided herein allow for extraction of high quality pectns from pectin-containing plant materials using oxalic acid for extraction ofthe pectin containing material. Generally described, the process for extracting pectin having a high depree of polymerization includes preparing an aqueous suspension ofa pectn-con- ‘winiag plant material: adding oxalic acid andlor @ water- soluble oxalate to the aqueous suspension in an amount suf= ficient to provide a mixture having a pH of between 3.0 and 3 Ganda total molarity of oxalate greater than a total molarity of caleium(I); heating the mixture to a temperature from lout 5010 about 80° C fora time sufficient o extract pectin ‘om the poctin-containing plant material: and separating the cxtacted pectin from the mixture. The extracted pect desie- ably ischaracterized as having a degree of esterification (DE) ofat least 72nd high depree of polymerization, the degree of polymerization being characterized by an intinsicviseos ity of greater than about 6.5 dL. 20 Claims, 7 Drawing Sheets US. Patent Nov. 26, 2013 Sheet 1 of 7 US 8,592,575 B2 Drying and Mili L@ US. Patent Nov. 26, 2013 Sheet 2 of 7 US 8,592,575 B2 US. Patent Nov. 26, 2013 Sheet 3 of 7 US 8,592,575 B2 Residual calcium eS 10 3 9 a 8 : a 7 7 « 70C 2S :— B4 he = 80C i: bi 21 6 9 _—_—___— ype stoich. 0 20 40 satn. oxalic acid g/kg peel FIG.3 US. Patent Nov. 26,2013 Sheet 4 of 7 US 8,592,575 B2 Effect of pH on yield —+— 0x15T70 —+— 0x15T80. —#— 0x20770 ~~~ Ox20T80 *— Ox25T70 —s— 0x25T80 —+— 0x30T70 *—~ Ox30T8O Yield of gross peel % wiw 25 27 29 34 33 3.5 pH of concentrated extraction FIG.4 US. Patent Nov. 26,2013 Sheet Sof 7 US 8,592,575 B2 Effect of pHon IV —— 0x20T70 | —#— 0x20T80 | —s— 0x25T70 *— Ox25T80 ~*~ 0x30T70 —*— 0x30T80| 1 —e— 0x15770 —— = + 0x15780) Intrinsic viscosity dL/g oan woruaraeod 25 27 29 34 3.3 35 pH of concentrated extraction FIG. 5 US. Patent Nov. 26, 2013 Sheet 6 of 7 US 8,592,575 B2 Yield pectin/peel g 40 x —____, 3g 30 7 « 70C g 2 » 20 % 8 = 80C £410 3 | @ 07 i, _ |--------- stoich.| > 0 20 40 |__satn._| oxalic acid g/kg peel FIG.6 US. Patent Nov. 26, 2013 Sheet 7 of 7 US 8,592,575 B2 Product of yield times IV 200 aan 150 8 g { *70C 2 100 g = 80C 50 - 0 0 20 40 oxalic acid g/kg peel FIG.7 US 8,592,575 B2 1 PROCESS FOR EXTRACTION OF PECTIN ‘TECHNICAL FIBLD Embodtiments ofthe present description relate to methods forextrationofhigh quality ectns. In particular, the present description relates to low-emperature processes for exe tion of pectin from citrus pecs that avoids significant degra- dation of pectin durin the extraction process BACKGROUND Pectin is a complex polysaccharide associated with plant ‘ell walls. consists of an alpha 1-$ linked polygalscturonic acid backbone intervened by shamnose residues and modified ‘with neutal sugar side chains and non-sugar compoeris such as acetyl methyl, ae feruic acid groups. The neutral sugar side chains, which include arabinan and arabinogalac- tans, ae attached tothe ehamnose residues in the backbone. A significant amount of research on pectin has been ca riedout due to itsimportance asa food product, a dietary fiber ‘and a component of cell walls in higher plans, and to the rowing awareness of » mimber of pharmacological actvi- lies. Curent methods of extracting pectin, however, do not produce pectns of sufficient quality for all such uses, Conventional methods of pectin extaction require ‘extended heating ofthe pectn-containing plant materials at sub-boiling temperatures (approximately 65-85° C.) in an acidic media (pH below 2.2) for 110 10 hours. These pro- ‘esses, however, ave high residence times and energy Fequiremenis and may provide only a moderate yield 20- 30%%)of pectin using a countercurrent process (ea process using a number, n, of extraction stages with which the orgi- nating raw material goes to extraction stage #1, the originat- ing pure water goes the stage #, and forany tage, assum ing I

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