• Nenhum resultado encontrado

Braz. J. Chem. Eng. vol.33 número4

N/A
N/A
Protected

Academic year: 2018

Share "Braz. J. Chem. Eng. vol.33 número4"

Copied!
10
0
0

Texto

(1)

ISSN 0104-6632 Printed in Brazil

www.abeq.org.br/bjche

Vol. 33, No. 04, pp. 1011 - 1020, October - December, 2016 dx.doi.org/10.1590/0104-6632.20160334s20140010

*To whom correspondence should be addressed

Brazilian Journal

of Chemical

Engineering

OBTAINING FRUCTOOLIGOSACCHARIDES

FROM YACON (Smallanthus sonchifolius) BY AN

ULTRAFILTRATION PROCESS

M. L. Brites and C. P. Z. Noreña

*

Instituto de Ciência e Tecnologia de Alimentos, (ICTA), Universidade Federal do Rio Grande do Sul, (UFRGS), Av. Bento Gonçalves 9500, 91501-970 Porto Alegre - RS, Brazil.

Phone: + 55 51 3308 6673; Fax: + 55 51 3308 7048 E-mail: [email protected]

(Submitted: August 15, 2014 ; Revised: August 9, 2015 ; Accepted: August 15, 2015)

Abstract - The objective of this study was to evaluate the separation of fructooligosaccharides (FOS) from yacon extract by an ultrafiltration process using membranes of 10 and 30 kDa. The total resistance (Rt),

membrane resistance (Rm), fouling resistance (Rf), and concentration polarization (Rc) during the separation

process were also assessed. The operating pressures were 1.2 and 0.75 bar for UF-10 and UF-30, respectively. The permeate flux increased upon increasing the pressure from 0.5 to 2 bar and the resistance values showed a slight increase with increasing pressure. The fouling percentages were 61.24% and 57.33% for the membranes UF-10 and UF-30, being reversible after the cleaning procedure with acidic and basic solution, resulting in high percentages of flux recovery of 76.46% and 83.56% for U-10 and UF-30, respectively. The FOS retention values were 24.48% and 6.49% for both membranes UF-10 and UF-30, corresponding to 24% and 18.4% purity.

Keywords:Yacon; Fructooligosaccharides; Ultrafiltration.

INTRODUCTION

Nowadays, the demand for foods that promote health and well-being is increasingly evident. Thus, food that was considered for many years as a source of nutrients needed to sustain life has become the object of studies related to disease prevention and improved function of organs and tissues.

In this context, yacon roots, which originated from Andean regions, contain from 60 to 70% inulin (Vilhena et al., 2000). The native inulin is a mixture of oligomers and polymers containing long chain molecules of different degrees of polymerization (DP) from 2 to 60 units, with an average DP of about 12; the inulin present in yacon has low DP, between 3 and 10, therefore being considered fructooligosac-charides (FOS) (Goto et al., 1995; Villegas and Cos-tell, 2007).

According to Lewis (1993), FOS are defined as a combination of three sugar molecules: 1-kestose (GF2), nystose (GF3) and frutofuranosyl nystose (GF4) where the units fructosyltransferase (F) are combined with sucrose (GF) at the β position (2 → 1). Compounds such as FOS may be used as sugar substitutes, as they are more soluble and sweeter than native and long-chain inulin (Meyer et al., 2011).

(2)

incorporate them for human consumption. An alter-native is the membrane separation process (MSP) considered to be a clean technology. Ultrafiltration (UF) is a type of MSP considered to be a very attrac-tive alternaattrac-tive method since it does not use heat and involves no phase change, which makes the concen-tration process more economical, with the advantage of not using chemicals, since only a driving force is required to separate the compounds of interest (Kamada et al., 2002b).

UF membranes have pore diameters varying be-tween 0.01 µM and 0.001 µM, and are capable of retaining and fractionating macromolecules such as lipids, proteins and colloids present in solution whose molecular weight varies from 300 to 500,000 Daltons (Da) (Mulder, 1996). These membranes can retain solutes of different molecular weights, usually being specified by a nominal molecular weight cut-off or MWCO, which establishes the lowest molecu-lar weight that is retained with an efficiency of at least 95% (Modler, 2000).

The use of UF to separate inulin and FOS from yacon has been reported in several studies. Gibertoni

et al. (2006) evaluated the production of rich fruc-tans syrup from clarified yacon juice using a ceramic microfiltration membrane with nominal pore size of 0.14 µm, and UF membrane with molecular weight cut off of 50 kDa. Kamada et al. (2002a) evaluated the combination of ultrafiltration and nanofiltration on the purification and concentration of FOS from yacon roots, removing most of the mono-and disac-charides and obtaining a concentrated product with DP of three or more, and 98% purity.

The MSP have some limitations, highlighting the phenomena of concentration polarization and fouling at the membrane surface. The polarization occurs in the first minutes of the process when the solute is retained at the membrane surface, making difficult the solvent permeation and resulting in a permeation flux decline, which is a reversible phenomenon. In contrast, the fouling is characterized by a permeation flux decline resulting from clogging of the mem-brane pores, which can be an irreversible phenome-non depending on the situation (Wu et al., 1990).

The resistance-in-series model has been used to evaluate fouling in the membrane separation process (Brião and Tavares, 2012). These resistances include membrane resistance, an external or reversible foul-ing, which consists of cake layer deposition and con-centration polarization, and irreversible resistance (Bagci, 2014; Rezaei et al., 2014). The latter is due to particle and macromolecule deposition and ad-sorption of smaller-sized solutes onto the membrane pore walls (Ng et al., 2014; Rezaei et al., 2014).

The aim of this study was to evaluate the separa-tion of FOS from yacon extract using ultrafiltrasepara-tion as a membrane separation process. The parameters of total resistance, membrane resistance, fouling re-sistance, and concentration polarization during the separation process were also investigated.

MATERIAL AND METHODS Raw Material

The yacon roots were cleaned and selected con-sidering the absence of visual damage and infections, and peeled and sliced with a mean diameter of 4.55 ± 0.25 mm and a thickness of 1.75 ± 0.35 mm (Scher

et al., 2009) and subjected to a blanching treatment for 4 minutes at 100 ºC, followed by cooling in an ice bath for 3 minutes (Fante and Noreña, 2012). The juice was extracted using a food processor. The re-maining sugars were extracted from the pulp ob-tained after separation of the juice by addition of water at 80 ºC in a 2:1 ratio (weight water/weight pulp), maintaining the mixture at 80 ºC ± 2 ºC for one hour, according to the methodology proposed by Toneli et al. (2007). The yacon juice and the liquid solution obtained from the pulp were separately fil-tered under vacuum. The filtrates were mixed, which constituted the yacon extract, to which 1% (w/v) citric acid was added and filtered on Whatman filter paper Nº. 01 to remove suspended solids.

Membrane Separation Process

Polyethersulfone UF membranes (Synder Filtra-tion Headquarters, Vacaville, USA) with nominal molecular weight cut off (NMWCO) of 10.000 and 30.000 Daltons were used. UF experiments were performed under the conditions of the configuration shown in Figure 1, which comprises: (1) a feed jack-eted glass vessel with a total volume of 2.0 Liters connected to an ultrasonic thermostatic bath (model CE-110/10, CienlaB, Brazil); (2) pneumatic diaphragm pump (model Ingersoll-Rand PD05P-ARS-PAA-B); (3) pre-filter; (4) AISI 316 stainless steel flat mem-brane module with area of 0.008118 m2; (5) and (6) AISI 316 stainless steel pressure gauges, scale 0-12 bar; (7) pressure valves; (8) bypass valve. Prior to the UF process, the extract passed through a pre-filter with a nominal pore size of 5 µm.

(3)

b fl F ce (4 m b b sl m th ti m b m th K u 3 la fo u ac ca ti cl R th Ji re th R w w

ar higher tha lux (Jp) was c

Figure 1: Sc ess. Legend: 4) membran manometer o ypass valve.

The hydra rane (Lpi) (L

lope of the membrane pre he water pe ime, with vo minutes, with

oth membran The separa mode with co he feed tank Kamada et al

red every 15 0 minutes in asted 6 hours or UF-30. Fin

sing NaOH cid solution, The same alculate the h ion process o leaning proc Resistance A The declin he resistance iraratananon esistance (m he other resis

t m c

R =R +R +

where Rm is with water (m

Obtaining Fru

Brazilian J an the workin

calculated.

chematic rep : (1) feed tan ne module, output, (7) p

aulic permea L.m-2.h-1.bar

-permeate fl essure. The p ermeation fl olume measu h a total proc

nes.

ation process omplete recir and permeat

l. (2002a). Th 5 minutes dur n the follow s for UF-10, nally, a clean

solution, 0.3 5 g.L-1, pH 2 procedure us hydraulic pe of the yacon edures (Lpc).

Analysis

ne of the perm e-in-series m

and Chanac

-1), which ca

stances accor

f R +

s the resistan m-1); Rc is th

uctooligosacchari

Journal of Chemic ng pressure.

presentation nk, (2) pump

(5) input m pressure con

ability for t

1) was calcu

lux as a fun process was lux became urements at cess time of 1

ses were perf rculation of te removal, a he permeate ring the first wing hours. T and 5 hours ning procedu 35 g.L-1, pH

2.0.

sed to find (L

ermeability a n extract (Lpf

.

meate flux w odel (de Bru chai, 1996). an be expres

rding to Equ

nce of the n he resistance

ides from Yacon

cal Engineering V Then the wa

of the UF p p, (3) pre-fil manometer, ntrol valve,

the new me ulated from nction of tra conducted un

constant w intervals of 150 minutes

formed in ba the retentate as described

flux was me hour and ev The UF proc and 30 minu ure was realiz H 10-10.5; cit

Lpi) was used after the sepa

pf) and after

was analyzed uijn et al. 20 is the to sed in terms uation (1):

new membra e of the conc

(Smallanthus son

Vol. 33, No. 04, ater pro-lter, (6) (8) em-the ans-until with f 15 for atch e to d by eas-very cess utes zed itric d to ara-the d by 002; otal s of (1) ane cen-tra an sis dra tio m R t R m R wh en (1) irr et M an cal et Fo Fl wh cle per Bo acc (20 o R

nchifolius) by an

pp. 1011 - 1020, ation polariza

d Rf is th stances were

aulic permea ons described

1

m

wLpi μ =

1

t

w pfL μ = 1 m f w R L μ + =

here μw is th The resistan ce between ). Rc and Rf

eversible fou

al., 2014).

embrane Fo nd Membran

Both memb lculated by E

al. (2007) an

ouling =⎛⎜⎜Lpi

lux recovery

here Jpc is eaning proce

rmeation flu oth flows wer The obser cording to E 011):

1 p

obs r C C ⎡ ⎤ = − ⎣ ⎦ Ultrafiltration Pro

October - Decem ation on the he fouling re

calculated b ability, in ac d by Cassano

1

pc

L

he water visc nce Rc was the other re

f are also de uling resistan

ouling, Clea ne Retention

brane fouling Equations (5)

nd Liikanen e

1 00 i pf pi L x L ⎞ − ⎟⎟ ⎠

1 0 pc pi J x J ⎛ ⎞ =⎜ ⎝ ⎠

the water p

edure (L.m-2. ux of the ne

re measured ved retentio quation (7) a

1x 00 ⎤

rocess

ember, 2016 e membrane

esistance (m

by using the ccordance w o et al. (2007

cosity (Pa.s). calculated fr esistances, u denominated

ances, respec

aning Efficie n

g and flux r ) and (6) acc

et al. (2002)

0

00

permeation

.h-1) and Jp

ew membran at the same on (%) w as described

10

surface (m -m-1). These r values of h with the equ 7):

(2

(3

(4

rom the diffe using Equatio reversible an

ctively (Reza

ency Protoc

recovery we ording to Sah , respectively

(5

(6

flux after th

pi is the wat ne (L.m-2.h

-pressure. was calculate

by Cissé et a

(4)

w su re th 1 an S co th fo p S o C se te o n m w S fo 9 S E g g L o (d an g N v g 1 in y

where Cp is ugar accumu etentate conc he end of th

00% (compl nd solvent pa

Sugar Assays

For determ ontents, the hrough 0.22 or 3 minutes

erformed by ambucetti (2 f direct dete Chromatograp

eries 200 ch ector, Milli-Q

f 0.6 mL / m omenex Rez mm, and total was performe

Statistical An

Data were or multiple c .3 (SAS Inst

RE

Sugar Conce Extract

The sugar /100 g (dm) lucose, and Lago et al. (2

f 1.07 ± 0.1 dm) for inuli nd 3.15 ± 0.

(dm) for in Nieto (1991) alues of 2.4 lucose and su

The soluti .41 ± 0.00, nulin, glucos

acon extract

the permeat

ulated in the centration of he process. T lete retentio ass freely thr

s

mination of i e samples

µm membran prior to HPL y the metho 2001) with a ermination by

phy (HPLC-hromatograph

Q water as m min, tempera

zex RHM M l run time of ed in duplicat

nalyses

e assessed by comparisons titute Inc.).

ESULTS AND

entration in

content of y for inulin, 4 11.00 ± 0.03 2012) found 8, 3.30 ± 0.2 in, glucose a 16, 10.98 ± nulin, glucos studied 10 y 7, 1.63, and ucrose. ion extracted

2.57 ± 0.09, se and fructo t containing

te concentra

tank (g.L-1) f the same s The Robs val

n of solute) rough the me

inulin, gluco were defr ne and place LC analysis. d described daptations, w y High Perfo -RI), using a h with refrac mobile phase ature of 80 ºC Monosacchar

f 14 minutes. te for each sa

y ANOVA an between me

D DISCUSS

the Juice, P

yacon juice w 4.74 ± 0.01 g

3 g/100 g (dm sugar conce 28 and 2.99 and fructose 0.32 and 4.3 se and fructo yacon specie d 2.51 g/100

d from the , 3.17 ± 0.02 ose, respecti

yacon juice

ation of a giv

) and Cr is sugar (g.L-1) lue varies fr ) to 0% (sol embrane).

ose and fruct rosted, filte ed in a sonica . Analyses w by Zuleta a which consis ormance Liq a Perkin Elm

ctive index e at a flow r C, column P ride, 300 x . The proced ample.

nd Tukey’s t eans, using S

SION

Pulp and Yac

was 5.42 ± 0 /100 g (dm) m) for fructo entration valu

± 0.18 g/10 in yacon jui 30 ± 0.57 g/1 ose in the pu es and obtain g for fructo

pulp presen 2 g/100 g (d ively. The fi and pulp lea

ven the ) at rom lute tose ered ator were and sted quid mer de-rate Phe-7.8 dure test SAS con 0.01 for ose. lues 0 g ice, 100 ulp. ned ose, nted dm) inal ach sol 11 glu Ul pa per sur lin as me 22 UF inc par exp bra flu cu all tha me 38 me ob fro Fig tra (● Ef Ex tim sur (20 fir

lution had a .36 ± 0.08, ucose and fru

ltrafiltration

Initially, the ction tests a rmeation flux re were real nearly with in shown in F eability with .45 L.m-2.h. F-30. This di creased wate

red to mem plained by t ane, since th ux under the lation flow w l pressure c at the hydra embrane usin

L.m-2.h.bar -embrane UF bserved by C

om 5 to 150 k

gure 2: Perm ansmembrane

).

ffect of Pre xtract

Figure 3 sh me for the m

res from 0. 007), each cu

st correspond

a final com 16.44 ± 0.0 uctose, respe

n Process

e experiment nd, after tha x as a functio lized. The p ncreasing pre Figure 2. The

h water wer bar-1 for the ifference in

r flux of the mbrane UF-1 the larger po he larger the e same proc was 26.5 L·h onditions. S aulic permea ng a pressur

-1 to 134 L.m

F-30 for UF-Cissé et al.

kDa and a pr

meate flow e pressure at

essure on P

hows the grap membranes U 5 to 2 bar. urve can be d

ding to a rap

mposition of 07 g/100 g (

ectively.

ts were perfo at, measurem on of transm permeation f essure for bot e values of re 12.05 L.m he membrane

permeability membrane U 10, whose p

ore size of t e pore size t cessing cond h-1 and it wa Saha et al. ability valu re of 1 bar in m-2.h.bar-1 by

-50. The sam (2011) usin ressure of 5 b

of water as t 25 °C.

UF-Permeate Fl

aphs of Jp ve

UF-10 and U According divided into t pid decline o

8.21 ± 0.0 dm) of inuli

ormed by com ments of wat membrane pre flux increase th membrane hydraulic pe m-2.h.bar-1 an

es UF-10 an y is due to th UF-30 as com performance

the first mem the higher th ditions. Reci

s the same f (2007) foun ues for a ne

ncreased fro y changing th

me effect w ng membran

bar.

a function 10 (■); UF-3

lux of Yaco

ersus operatio UF-30 at pre

to Rai et a

two stages, th f the permea

(5)

fl ce th Z cr m fl d v p U iz re an st su tr so m d T b su so to et d tr fl m fo ta th B th g ca b su ar b st 3 lo p (J T en li te F 1 p

lux, which ca entration pol he effective d Zydnei, 1999

reases with mass transfer, lux (Benhab ecrease was aried from 2 ared to the in UF-30, respe

zed by a less eaching a ste nce with Art tate permeat ure values. M ration polari

olute during macromolecu ecisive influ The particles

y the memb urface there olutes having o Jiraratanan

t al. (2011), uced concen ransfer coef lux. This w means a decli

ormation in angential ve he deposited Bruijn and Bó

he transmem ential veloc ase, de Bru oth blocking uperposition re almost co locking dom

Figure 4 s tate permeat 0. The perm ower TMP p

ermeate flux

Jlim), regardle The point at w

nt is conside imiting flux endency to co For membran

.5 bar, the pe endent of pr

Obtaining Fru

Brazilian J an be attribu larization tha driving force 9). The thick time, thus i , as shown b iles et al., 2 s higher wit 26.6 to 39.6%

nitial flux of ctively. The s pronounced eady-state. In thanareeswar te flux incre Mulder (1996

ization influ g the separat ular solutes, uence on the with higher brane eventu

of, which r g smaller mo non and Cha

, an increas ntration polar fficient and way, an incre ine of the re membrane f locity remov d cake due

órquez, 2006 mbrane press

city is maint uijn and Bór g of the por

of solute an onstant duri minating over shows the ef te flux for m meate flux sh pressures, wh

x values wer ess of further

which the pr ered to be the

that can min oncentration ne UF-10 un

ermeate flux ressure, indic

uctooligosacchari

Journal of Chemic uted to the ef

at results in t e (Cheryan, kness of the increasing th by the decrea 2013). In ad th increasing % and 10.2 t f the membra

second stag d decrease o n this condit ran et al. (20 eased with in

6) reported t uences the re

tion of mixtu where the p e selectivity r molecular w

ually form retains a lar olecular weig anachai (199

e in recircu rization, enh increased t ease in tang elative partic fouling, beca

ves a consid to the incre 6). On the ot sure increase

tained const rquez (2006 re entrance w nd blocking b ing UF, with r cake format ffect of TMP membranes U

howed a lin hile at highe e close to a increases in ressure is cle e optimum ∆ nimize both n polarization

nder pressure x of yacon ex cating that th

ides from Yacon

cal Engineering V ffect of the c

the reduction 1998; Reis a e layer also he resistance ase in perme dition, the f g pressure, a to 61% as co anes UF-10 a ge is charact of the flux un

tion, in acco 10), the stea ncreasing pr that the conc etention of ures contain polarization h

of the proce weight retain a layer on rger number

ghts. Accord 6) and Mon ulation flow hanced the m the permeat gential veloc cipation of ca ause the hig derable part eased shear

her hand, wh es and the t

tant, as in 6) mention t with or with by a cake la h internal p tion. P on the stea

UF-10 and U near increase

r pressures, threshold va pressure valu early indepen ∆P, which is

fouling and n (Baker, 200

e values abo xtract was in

he limiting f

(Smallanthus son

Vol. 33, No. 04, on-n of and in-e to eate flux and om-and ter-until ord- ady- res- cen-the ning has ess. ned the r of ding ndal re-mass tion city ake gher t of (de hen tan-our that hout ayer pore ady- UF-e at the alue ues. nd-the the 04). ove nde-flux wa lim Sim (20 Fig of 10 bar Fig ya UF

nchifolius) by an

pp. 1011 - 1020, as reached, w miting flux w

milar observ 004) and Cas

gure 3: Perm time at 25 ° membrane r, (▲) 1 bar,

gure 4: Eff con extract i F-30 (■).

Ultrafiltration Pro

October - Decem whereas for

was reached vations were

ssano et al. (

(A

(B meate flow o °C at differen

(A), UF-30 (■) 1.5 bar, (

fect of press in the steady

rocess

ember, 2016 the membra d at a press realized by (2008).

A)

B)

of yacon extr nt pressures 0 membrane

(●) 2 bar.

sure on perm y-state at 25 °

10

ane UF-30, th sure of 1 ba y Rektor et a

ract a functio using the UF (B), (▼) 0

meate flow °C. UF-10 (●

(6)

ca op m ef (C m 1 U p th w 4 to cr su ov m co E E p cr cl (L za d m m 2 fo an br d F 4 te th m 1 p b th b ob se o According al point of v perated at p may lead to a ffects of fo Cassano et a

membrane pr .2 bar and 0 UF-30, respe rovided the hese conditio with time, fro .1 L.m-2.h-1 f o the bound reased conce urface (conce ver, the acc membrane po

ontributed to

Effect of Fo Extract

A major l rocess is fou rease energy leaning proc Liao et al., 2

The memb ation are lim ecrease in pe mulation of co membrane po

001). Figure ore (Jpi) an nd after the c

ranes UF-10 raulic perm For the mem

.67 and 9.12 er permeation he experime membrane UF

8.76 L.m-2.h Habert et

ermeability o e monitored here was ad

rane integrit bserved, ind evere change The memb f hydraulic

g to Habert e

view, any m pressures low a limiting flu ouling and

al., 2008). Fo ressure chose 0.75 bar for

ectively, sin most accep ons, the per om 5.9 to 3. for UF-10 an dary-layer p entration of entration pol cumulation ores (membra o decreasing

ouling on P

limitation of uling. It may y consumpt cedures or r

008). brane fouling miting factor

ermeate flux omponents f ores and on e 5 shows th nd after (Jpf

cleaning proc

0 and UF-30 eabilities wi mbrane UF-1 2 L.m-2.h.bar n flow of th ents and cle F-30, these v h.bar-1, respec

al. (2006) r of the memb

before and a dequate clean ty. A sharp d dicating tha es during the brane fouling

permeabilit

et al. (2006) membrane sys

wer than tho ux, in order t

concentratio ollowing this

en for the U the membra nce these p ptable perm rmeate flux

4 L.m-2.h-1 a nd UF-30, re henomenon, solute near larization) too of macromo ane fouling) flow.

Permeate F

f the membr decrease per ion, and le replacement

g and conce rs for MSP, s x with time c from the feed the surface he water per

) the ultrafil

cedures (Jpc

0. From this ith water w 10, the value

r-1, respective e new memb eaning proce

values were 2 ctively.

reported tha branes with p

after the pro ning and en decline in pe at the mem e process.

g estimated f ty of the p

, from a pra stem should ose values t to minimize on polarizat s line, the tra UF process w anes UF-10 a pressure valu eate fluxes. also decrea and from 6.9 espectively, d

where an the membra ok place. Mo olecules in could also ha

Flux of Yac

rane separat rmeate flux, ad to frequ of membran

entration pola since there i caused by ac d solution in (Czekaj et

rmeate flux ltration proce

)

c for the me figure the h were calculat

es were 12. ely, for the w brane, and af edures. For

22.45, 9.58 a

at the hydrau pure water m

cess to check nsure the me

ermeability w mbrane suffe

from the valu ermeate flux acti-d be that the tion ans-was and ues In ased 9 to due in-ane ore-the ave con tion in-uent anes ari-is a ccu-the al., be-ess, em- hy-ted. .05, wa-fter the and ulic must k if em-was ered lues uxes we ma blo fac act me res bra ind ass tio res are de sel of rec Fig tra UF flo (J pro ult ere 61.24% ain phenome ocking, parti ce (cake) and tion between embrane ma sulting in hig ane surface ( dicated that sumed to oc on and its e sistance. The e an increase creased effic lectivity. Th

the target sp covery (Li et

gure 5: Perm ansmembrane

F-10, 1.2 bar ow of water i

) pi

J , (■) Perm ocedure (Jp

trafiltration o

(UF-10) an na contributi icle adsorpti d / or inside n the solute in aterial, and f gh concentrat (Liao et al., 2

the phenom cur during th ffects are in erefore, the ed resistance ciency and /

is affects th pecies, with

t al., 2010).

(A

(B meate flow e pressure a r (A); UF-30, in the new m meate flow o

)

c , (▲) Perm of the extract

nd 57.33% ting to foulin ion on the m

its pores du n the feed so formation o tions of solu 2004). Hasa menon of por

he first mom ncluded in t

consequenc e to membra / or changes he separation

a consequen

A)

B)

of water as at 25 °C fo , 0.75 bar (B membrane aft of water afte

rmeate flow

of yacon (Jp

(UF-30). Th ng include po membrane su ue to the inte olution and th of a gel laye ute at the mem

n et al. (201 re blocking ments of filtr the membran ces of foulin ane separatio

in membran n performan nt low produ

a function or membran B) (●) Permea ter compactio er the cleanin

of water aft

(7)

sy 3 b co cl ca w an p m R cl re N fo ob U ef ti in o E re an an in th o v fo se m fo sh fr 1 m th m m p fl p n cr re

Saha et al. ystem, and o 0 kDa memb rane. The a ontained var logging of p ant flow redu

After the c were 76.46%

nd UF-30, r ossible to re membranes in Rodrigues e

larification u eported that NaOH solutio

or 2 hours, bserved for UF-30. Souza fficiency of ime due to c nstability, low

ccurrence of

Effect of Ope

Figure 6 s esistance, m nd polarizati nd UF-30.

The memb ncreasing pre he lowest pre f 2 bar usin alue increase or the memb erved by Gö membrane wi

or ultrafiltrat howed little rom 1 to 4 b 013 m-1, they molecular we hat Rm decrea

membrane to membrane.

The increa ressure can b low of solut ressure. The ounced conc rease in Rc (L

eported that,

Obtaining Fru

Brazilian J . (2007) stud obtained foul brane, and 4 authors conc

rious macrom ores and incr uction.

cleaning pro and 83.56% respectively. estore the pe n a new proc

et al. (200 using membr t, after the on (pH 10)

a flux rec the membra a and Quadri

polymeric m chemical de w fluxes and f swelling ph

erating Con

shows the e membrane res ion resistanc

brane resistan essure, with v essure and 3. ng the memb

ed from 1.69 brane UF-30

ökmen and ith molecula tion of apple change wh ar, changing y decreased eight cut off ased from 8. o 2.47 × 1

ase in resista be attributed te into the e increase in

centration p Li and Chen at higher pr

uctooligosacchari

Journal of Chemic died sugarcan ling values o 42.60% for a luded that s molecules th

reased foulin

ocedure, the % for the mem

From these ermeate flux

cess with the 3) studied ranes of 10 a

cleaning p and 0.8% N covery of ab ane UF-10 an i (2013) men membranes gradation, fo d compaction henomena.

ditions on R

effect of TM sistance, fou

e for the mem

nces increase values of 3.2 .41 × 1013 m brane UF-10 9 × 1013 to 0. This effec Cetinkaya ( ar weight cut e juice. Altho hen the pres g from 0.83 × with increas f. Wan et al

40 × 1013 m -1013 m-1 usi ance values w

to the increa membrane w n Rt leads t

olarization, n, 2010). Lab ressures, mo

ides from Yacon

cal Engineering V ne juice in a of 52.63% fo a 50 kDa me sugarcane ju hat caused ra ng, with sign

flux recover mbranes UF

results, it w and reuse b e yacon extra

banana ju and 30 kDa, a

procedure w NaClO solut

bout 95% w nd 75% for ntioned that decreases w fouling, therm

n, as well as

Resistances

MP on the to uling resistan

mbranes UF

ed slightly w 25 × 1013 m-1

-1 for a press

0, whereas t 1.89 × 1013 ct was also (2007) using t off of 10 k ough Rm valu

ssure increa × 1013 to 1.24

sing membra

l. (2012) fou

-1 using a 1 k

ing a 10 k

with increas ased convect with increas to a more p causing an bbe et al. (19 ore solutes su

(Smallanthus son

Vol. 33, No. 04, UF or a em-uice apid nifi-ries -10 was both act. uice and with tion was the the with mal the otal nce, -10 with for sure this m-1 ob-g a kDa ues ased 4 × ane und kDa kDa sing tive sing pro- in-90) uch as po rev all the are oth sis bra dep bra Fig bra UF (▼ Sa to hig UF 30 dif

nchifolius) by an

pp. 1011 - 1020, sugars and ores, increasi

versible resis l filtration. R e concentrat e much more her effects. stance is caus ane surface

pends on the ane (Brião an

gure 6: Effe ane pressure F-10, 1.2 bar

▼) Rm (▲) Rf.

accharides R

The UF me retain the F ghest Robs for F-10 (24.48%

(6.49%). T fferences in

Ultrafiltration Pro

October - Decem acids passe ing fouling stance was t Rezaei et al.

ion polariza e important f On the oth sed by strong and the inte e interactions nd Tavares, 2

(A

(B ect of the pr e resistance (A); UF-30, . Retention an embranes use FOS accordin r FOS was re %) as compa This differen the molecul

rocess

ember, 2016 ed through t

resistance the main res

(2014) dem ation and ca

for the total r her hand, ir g adsorption ensity of this

s between so 2012).

A)

B)

pressure on t at 25 °C fo , 0.75 bar (B

nd Purity

ed in this stu ng to their p eached with ared to the m nce was exp lar weight cu

10

the membran Rf. Thus, th

istance durin monstrated th

ake resistanc resistance tha rreversible r

onto the mem s phenomeno lute and mem

the transmem or membran B), (●) Rt (■) R

udy were ab pore size. Th

the membran membrane UF pected due ut off. Simil

(8)

behavior was observed for glucose (12.95 and 9.11%) and fructose (22.18 and 11.31%). Kuhn et al. (2010) emphasized that the simple sugars and FOS have a molar mass in Daltons smaller than the pore size of the membranes UF-10 and UF-30 (glucose and fruc-tose: 180; sucrose: 342; 1-kestose (GF2) 504, nys-tose (GF3): 666 and frutofuranosilnisnys-tose (GF4): 828, FG5: 1080; GF6: 1260; GF7 1440; GF8: 1620; GF9: 1800), which allowed them to pass through the pores and be collected in the permeate.

The degree of the purity of the FOS in the perme-ate was 24.08% and 18.43% for UF-10 and UF-30, respectively. This degree was obtained from the rela-tionship between FOS and sugar total concentration into the permeate. The degree of purity in the juice and yacon extract was 25.61% and 22.79%, respec-tively. It can be noticed that the enrichment in FOS versus simple sugars was not as high as desirable. A principal reason is that the membranes have a pore size distribution which does not allow effective sepa-ration of FOS from glucose and fructose molecules. Zhu et al. (2012) reported that the major FOS in yacon are kestose (GF2), nystose (GF3) and 1-fructofuranosyl nystose (GF4) whose content in oli-gosaccharides were 12.29%, 12.17%, 6.20%, respec-tively. The molecular weights of these FOS are less than 1 kDa (Kuhn et al., 2010). For this reason it is necessary to include in this process the separation by nanofiltration. Kamada et al. (2002a) used the com-bination of NF-UF to purify FOS present in a mix-ture of sugars derived from yacon and observed re-tention of 54.8% and the rere-tention values of 14.0% for monosaccharides, 46.2% for disaccharides, 80.9% for trisaccharides and from 91.5 to 99.9% for sugars with DP ≥ 4, using a 1 kDa membrane and pressure of 5 bar.

CONCLUSIONS

The effects of pressure on the total resistance, membrane resistance, fouling resistance and polari-zation resistance were evaluated using polyethersul-fone membrane with nominal molecular weight cut offs of 10 and 30 kDa. It was observed that the in-crease in pressure resulted in a slight inin-crease in all resistance values.

It was found that, for both membranes, the re-versible resistance was the dominant resistance which reduced the permeate flux, while irreversible fouling resistance gave less of a contribution.

A good restoration of the hydraulic permeability was obtained after the cleaning procedure with acidic and basic solution.

ACKNOWLEDGMENTS

This work was supported by the Brazilian agen-cies CNPq, CAPES and FAPERGS.

REFERENCES

Arthanareeswaran, G., Mohan, D. and Raajenthiren, M., Preparation, characterization and performance studies of ultrafiltration membranes with poly-meric additive. Journal of Membrane Science, 350, 130-138 (2010).

Bagci, P. O., Effective clarification of pomegranate juice: A comparative study of pretreatment methods and their influence on ultrafiltration flux. Journal of Food Engineering, 141, 58-64 (2014).

Baker, R. W., Membrane Technology and Applica-tions. 2nd Ed., John Wiley and Sons, England (2004).

Benhabiles, M. S., Abdi, N., Drouiche, N., Lounici, H., Pauss, A., Goosen, M. F. A. and Mameri, N., Protein recovery by ultrafiltration during isolation of chitin from shrimp shells Parapenaeus longi-rostris. Food Hydrocolloids, 32, 28-34 (2013). Brião, V. B. and Tavares, C. R. G., Pore blocking

mechanism for the recovery of milk solids from dairy wastewater by ultrafiltration. Brazilian Jour-nal of Chemical Engineering, 29, 393-407 (2012). Cassano, A., Conidi, C. and Drioli, E., Clarification

and concentration of pomegranate juice (Punica granatum L.) using membrane processes. Journal of Food Engineering, 107, 366-373 (2011).

Cassano, A., Mecchia, A. and Drioli, E., Analyses of hydrodynamic resistances and operating parame-ters in the ultrafiltration of grape must. Journal of Food Engineering, 89, 171-177 (2008).

Cassano, A., Donato, L. and Drioli, E., Ultrafiltration of kiwifruit juice: Operating parameters, juice quality and membrane fouling. Journal of Food En-gineering, 79, 613-621 (2007).

Cheryan, M., Ultrafiltration and Microfiltration Hand-book. Lancaster, Technomic Publishing Company (1998).

Cissé, M., Vaillant, F., Pallet, D. and Dornier, M., Selecting ultrafiltration and nanofiltration mem-branes to concentrate anthocyanins from roselle extract (Hibiscus sabdariffa L.). Food Research International, 44, 2607-2614 (2011).

(9)

Obtaining Fructooligosaccharides from Yacon (Smallanthus sonchifolius) by an Ultrafiltration Process 1019

Brazilian Journal of Chemical Engineering Vol. 33, No. 04, pp. 1011 - 1020, October - December, 2016 de Bruijn, J. and Bórquez, R., Analysis of the fouling

mechanisms during cross-flow ultrafiltration of apple juice. LWT - Food Science and Technology, 39, 861-871 (2006).

de Bruijn, J., Venegas, A. and Borquez, R., Influence of crossflow ultrafiltration on membrane fouling and apple juice quality. Desalination, 148, 131-136 (2002).

Fante, L. and Noreña, C. P. Z., Enzyme inactivation kinetics and colour changes in Garlic (Allium sa-tivum L.) blanched under different conditions. Jour-nal of Food Engineering, 108, 436-443 (2012). Gibertoni, C. F., Nogueira, A. M. P. and Venturini,

W. G., Ultra e micro filtração de suco de yacon (Polymnia sonchifolia) na obtenção de xarope rico em frutanos. Revista Raízes e Amidos Tropi-cais, 2, 68-81 (2006). (In Portuguese).

Gibson, R. and Roberfroid, M., Dietary modulation of the human colonic microbiota: Updating the concept of prebiotics. Journal of Nutrition, 125, 1401-1412 (1995).

Gökmen, V. and Cetinkaya, O., Effect of pretreat-ment with gelatin and bentonite on permeate flux and fouling layer resistance during apple juice ul-trafiltration. Journal of Food Engineering, 80, 300-305 (2007).

Goto, K., Fukai, K., Hikida, J., Nanjo, F. and Hara, Y., Isolation and structural analysis of oligosac-charides from yacon (Polymnia sonchifolia). Bio-science Biotechnology Biochemistry, 59, 2346-2347 (1995).

Habert, A. C., Borges, C. P. and Nobrega, R., Pro-cesso de Separação por Membranas. Editora E-pa-pers, Rio de Janeiro (2006). (In Portuguese). Hasan, A., Peluso, C. R., Hull, T. S., Fieschko, J. and

Chatterjee, S. G., A surface-renewal model of cross-flow microfiltration. Brazilian Journal of Chemical Engineering, 30, 167-186 (2013).

Jiraratananon, R. and Chanachai, A., A study of foul-ing in the ultrafiltration of passion fruit juice. Journal of Membrane Science, 111, 39-48 (1996). Kamada, T., Nakajima, M., Nabetani, H. and Iwa-moto, S., Pilot-scale study of the purification and concentration of non-digestible saccharides from yacon rootstock using membrane technology. Food Science and Technology Research, 8, 172-177 (2002a).

Kamada, T., Nakajima, M., Nabetani, H., Saglam, N. and Iwamoto, S., Availability of membrane tech-nology for purifying and concentrating oligosac-charides. European Food Research and Technol-ogy, 214, 435-440 (2002b).

Kuhn, R. C., Filho, F. M., Silva, V., Palacio, L., Her-nandez, A. and Pradanos, P., Mass transfer and

transport during purificationof fructooligosaccha-rides by nanofiltration. Journal of Membrane Sci-ence, 365, 356-365 (2010).

Labbe, J. P., Quemeiras, A., Michel, F. and Daufin, G., Fouling of inorganic membranes during whey ultrafiltration: Analytical methodology. Journal of Membrane Science, 51, 293-307 (1990).

Lago, C. C., Bernstein, A., Brandelli, A. and Noreña, C. Z., Characterization of powdered yacon ( Smal-lanthus sonchifolius) juice and pulp. Food and Bioprocess Technology, 5, 2183-2191 (2012). Lewis, D. H., Nomenclature and diagrammatic

repre-sentation of oligomericfructans. A paper for dis-cussion. New Phytologist, 124, 583-594 (1993). Li, H. and Chen, V., Membrane Fouling and

Clean-ing in Food and BioprocessClean-ing. In: Cui, Z. F. and Muralidhara, H. S. Membrane Technology. A Practical Guide to Membrane Technology and Ap-plications in Food and Bioprocessing, Chapter 10, Elsevier (2010).

Liao, B. Q., Bagley, D. M., Kraemer, H. E., Leppard, G. G. and Liss, S. N., A review of biofouling and its control in membrane separation bioreactors. Water Environmental Research, 76, 425-436 (2004).

Liikanen, R., Yli-Kuivila, J. and Laukkanen, R., Efficiency of various chemical cleanings for nanofiltration membrane fouled by convention-ally-treated surface water. Journal of Membrane Science, 195, 265-276 (2002).

Meyer, D., Bayarri, S., Tárrega, A. and Costell, E., Inulin as texture modifier in dairy products. Food Hydrocolloids, 25, 1881-1890 (2011).

Modler, W. H., Milk Processing. In: Shuryo, N. and Modler, W. H. Food Protein Processing Applica-tions. 1st Ed., Wiley, New York (2000).

Mondal, S., Cassano, A., Tasselli, F. and De, S., A generalized model for clarification of fruit juice during ultrafiltration under total recycle and batch mode. Journal of Membrane Science, 366, 295-303 (2011).

Mulder, M., Basic Principles of Membrane Technol-ogy. 2nd Ed., Kluwer Academics Publishers Group, Netherlands (1996).

Ng, C. Y., Mohammad, A. W., Ng, L. Y. and Jahim, J. M., Membrane fouling mechanisms during ultra-filtration of skimmed coconut milk. Journal of Food Engineering, 142, 190-200 (2014).

Nieto, C. C., Agronomical and bromatological studies in jicama (Polymnia sonchifolia Poep et Endl.). Archivos Latinoamericanos de Nutrición, 41, 213-221 (1991).

(10)

flux and quality during ultrafiltration of mosambi juice. Journal of Food Engineering, 78, 561-568 (2007).

Reis, R. and Zydnei, A., Protein Ultrafiltration. In: Flickinger, M. C. and Drew, S. W. (Eds.). Ency-clopedia of Bioprocess Technology: Fermenta-tion, Biocatalysis, and BioseparaFermenta-tion, New York, John Wiley and Sons (1999).

Rektor, A., Pap, N., Kókai, Z., Szabó, R., Vatai, G. and Békássy-Molnár, E., Application of mem-brane filtration methods for must processing and preservation. Desalination, 162, 271-277 (2004). Rezaei, H., Ashtiani, F. Z. and Fouladitajar, A.,

Foul-ing behavior and performance of microfiltration membranes for whey treatment in steady and un-steady-state conditions. Brazilian Journal of Che-mical Engineering, 31, 503-518 (2014).

Rodrigues, S. L. C., Moreira, R. L. S., Cardoso, M. H. and Merçon, F., Avaliação de parâmetros de ultrafiltração de suco de banana. Ciência e Tecnologia de Alimentos, 2, 98-101(2003). (In Portuguese).

Saha, N. K., Balakrishnan, M. and Ulbricht, M., Sugarcane juice ultrafiltration: FTIR and SEM analysis of polysaccharide fouling. Journal of Membrane Science, 306, 287-297 (2007).

Scher, C. F., Rios, A. O. and Noreña, C. P. Z., Hot air drying of yacon (Smallanthus sonchifolius) and its effect on sugar concentrations. International Food Science and Technology, 44, 2169-2175 (2009). Souza, V. C. and Quadri, M. G. N., Organic-inorganic

hybrid membranes in separation processes: A 10-year review. Brazilian Journal of Chemical Engi-neering, 30, 683-700 (2013).

Toneli, J. T. C. L., Mürr, F. E. X., Martinelli, P., DalFabbro, I. M. and Park, K. J., Optimization of a physical concentration process for inulin. Jour-nal of Food Engineering, 80, 832-838(2007). Vilhena, S. M. C., Câmara, F. L. A. and Kakihara, S.

T., O cultivo de yacon no Brasil. Horticultura Bra-sileira, 18, 5-8 (2000). (In Portuguese).

Villegas, B. and Costell, E., Flow behaviour of inu-lin–milk beverages. Influence of inulin average chain length and of milk fat content. International Dairy Journal, 17, 776-781 (2007).

Wan, Y., Prudente, A. and Sathivel, S., Purification of soluble rice bran fiber using ultrafiltration tech-nology. LWT - Food Science and Technology, 46, 574-579 (2012).

Wu, M. L., Zall, R. R. and Tzeng, W. C., Microfiltra-tion and ultrafiltraMicrofiltra-tion comparison of apple juices clarification. Journal of Food Science, 55, 1162-1163 (1990).

Zhu, Z. Y., Lian, H. Y., Si, C. L., Liu. Y., Liu, N., Chen, J., Ding, L. N., Yao, Q. and Zhang, Y., The chromatographic analysis of oligosaccharides and preparation of 1-kestose and nystose in yacon. In-ternational Journal of Food Science and Nutrition, 63, 338-42 (2012).

Referências

Documentos relacionados

Sugarcane juice with passion fruit pulp was clarified using microfiltration under different T (temperature), P (pressure), and V (tangential velocity).. The effects of these

The various modes of pore blocking are a function of the solid/solute size and shape in relation to the membrane pore size distribution: complete pore blocking (the pore

This ozonation process resulted in a 29.1, 93.7 and 99.2% reduction in the COD, color and turbidity of the effluent, respectively, indicating that this procedure was appropriate

In the present case, the thermal hydrolysis extract was produced at the same temperature, but from spent coffee (roasted coffee that had already been submitted to

The mathematical model fitted to the microalgal growth experimental data was appropriate for predicting the efficiency of the reactor in producing Scenedesmus obliquus

On the other hand, with a lower range of operating pressure and higher and lower ranges of feed flow rates, the CA membrane shows a better performance, as compared to the

The microbial production of water in SSC can be controlled with high air flow rates on an inert sup- port that enable fungal growth in the biofilm and aerial phases.. Oxygen

One of the objectives behind the implementation and validation of the ADM1 was to develop an appli- cation that could be used for process monitoring of a two-stage