Stevia Sweetener Purification
Mitsubishi Chemical Corporation Separation Materials Department
What Is Stevia Sweeteners?
• Stevia sweeteners are natural sweeteners those are presented in the leaves Stevia rebaudiana Bertoni.
• Steviosides, rebaudioside A, B, C, D, E and dulcoside A are representative compounds.
• These compounds are 60 -300 times sweeter than sugar and contain significantly fewer calories.
2
Stevia leaves
H
H3C
H3CH
COOO
OH
HOH2C
HOHO
CH2
OO
O
HOH2CHO
O
O
OH
HOH2C
HOHO
O
OH
HOH2C
HOHO
Rebaudioside A C44H70O23, m.w.=967
H
H3C
H3CH
COOO
OH
HOH2C
HOHO
CH2
OO
O
HOH2CHOHO
O
OH
HOH2C
HOHO
Stevioside C38H60O18, m.w.=804
Flow Chart of Stevia Sweeteners purification
3
Dried stevia leaves
Extraction with hot water
Pretreatment
Filtration
(Solvent evaporation)
Cation exchange resins
Anion exchange resins
Finishing/decoloring
Concentration
Spray drying
Aqueous alcohol
solutions
Eluate
Product
Waste water
CaCl2, MgO, Ca(OH)2 etc.
DIAION Manual p.304
MeOH eluate
Adsorption of stevia sweeteners
Demineralization &
Decolorization
After treatment with IERs
Synthetic adsorbents
Our products – Synthetic Adsorbents -
We can provide synthetic adsorbents with various types of porosity.
4
SP825
DIAION HP21, MCI GEL CHP50
SP850
peptide・protein Mw 1000~tens of thouthands
β- lactam Mw~600 macrolide
Mw 500~1500
SP70
SP700
Pore
volum
e (
mL/g)
HP20,CHP20 HP2MGL,CMG20
SP207, CHP07
Molecular Weight
Stevioside Mw=804 RebaudiosideA Mw=967
Characteristic of SP700
5
HP20 SP700
Chemical Structure
Pore Volume(mL/g) 1.3 2.1
Specific Surface Area(m2/g)
590 1,200
Pore Radius(Å) 290 90
RebA Amount of adsorption (mg/mL-R)
92 149
ST Amount of adsorption (mg/mL-R)
98 146
CHCH2 CHCH2
CH CH2
CHCH2 CHCH2
CH CH2 CH2CH3
SP700 ・High specific surface area ・High stevia sweetener adsorption
Pore size distribution of synthetic adsorbents
6
SP700 has narrower pore size distribution and large surface area than HP20.
00.20.40.60.8
11.21.41.61.8
22.2
10 100 1000
PORE V
OLUM
E (mL/g)
PORE RADIUS (Å)
HP20 細孔容積
SP700 細孔容積
HP20 dPV
SP700 dPV
Pore volume
Pore volume
Pore radius
Pore radius
Loading profile
7
SP700 ・high capacity for stevia sweeteners adsorption ・long adsorption band →Multi column system is suitable for SP700.
Condition column:φ30mm x L1000mm Resins 400mL Room temperature Flow rate SV4
Short Adsorption
band
Long Adsorption
band
HP20
0102030405060708090
100
0 20 40 60 80 100 120 140 160 180 200
Leak
age C
/C0 (%
)
Stevia adsorpion amount(g/ L-R)
SP700
Multi column system operation
1 2 2 2 1 1
Loading
Eluent
Elution (MeOH or EtOH)
It is possible to effectively utilize the adsorption capacity of SP 700 with long adsorption zone.
8
Loading
Elution profile
9
0
20
40
60
80
100
120
140
0 1 2 3 4Ste
via
sw
eete
ner
conc
. (m
g/m
L)
Flow volume (mL/mL-resin)
HP20 (5% BTP) SP700 (70% BTP) Condition Column:φ30mm x L1000mm Resins 400mL Room temperature 85% MeOH SV2 2BV Sweet off water SV2 2BV
SP700 can concentrate higher stevia sweeteners than HP20. SP700 shows small tailing.
HP20 elution (5% BTP)
SP700 elution (70% BTP)
Brix 8.7 9.7
RA(mg/mL) 1.8 2.2
ST(mg/mL) 20.0 32.1
RA+ST recovery 100 % 100%
CER & Equipment
10
SK1B
Appearance
Type Strongly acidic cation (Gel)
Salt splitting capacity (meq/mL) 2.0 min.
Water content (%) 43–50 Shipping density* (g/L) 830
Effective size (mm) 0.40 min. Maximum operating temperature (°C) 120 (H
+, Na+)
Pump
Cat
ion
exch
ange r
esi
n
Sample solution
Thermostatic circulator
Jacketed column L 300 mm x 15 mm I.D.
Electric conductivity
meter
pH meter
AER and Equipment
11
HPA512L
Appearance
Type Strongly basic anion
Type I (trimethylammonium groups)
Salt splitting capacity (meq/mL) 0.7 min.
Water content (%) 63–73 Shipping density* (g/L) 670
Effective size (mm) 0.45 min. Maximum operating temperature (°C) 80 (Cl
–), 60 (OH–) Specific surface area* (m2/g) 9
Pore volume* (mL/g) 0.11 Pore radius* (Å) 191
Note: properties with a mark ‘*’ are reference data
Pump
Anion
exch
ange r
esi
n
Sample solution
Thermostatic circulator
Jacketed column L 300 mm x 15 mm I.D.
Electric conductivity
meter
pH meter
Decolorization and Recovery
12
MeOH eluate
After treatment with SK1B
After treatment with HPA512L
MeOH concentration 40% 40% 40% Absorbance (420 nm) 5.22 4.55 ≤ 0.3
Rebaudioside A recovery – 100% 83%
Stevioside recovery – 98% 77%
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0%
20%
40%
60%
80%
100%
Recovery
420nm
Abs.
BV
HPA512L
83%
16%
total recovery 99%
MeOH
HPA512L shows good performance for decolorization . Stevia sweeteners were Recovered in good yield.
MeOH eluate
After SK1B
After HPA512L
MeOH consumption is key factor for total cost, rather
than resin cost.
SP700 is High capacity → Less resins → Less MeOH Cost reduction
Running Cost Simulation
13
0
10
20
30
40
50
60
70
80
90
100
HP20
single column
SP700
single column
SP700
multi column
%
Cost Comparison
Resin MeOH Waste/water
Stevia adsorption
(g/L-R) resin (m3)
85% MeOH (m3)
waste (m3)
Process water (m3)
HP20 (single column)
65( 5%BTP) 15 30 375 180
SP700 (single column)
90( 5%BTP) 11 22 330 132
SP700 (multi column)
130(95%BTP) 7.5 15 285 90
For 1000kg stevia sweetener production
Stevia Sweetener PurificationWhat Is Stevia Sweeteners?Flow Chart of Stevia Sweeteners purificationOur products – Synthetic Adsorbents -Characteristic of SP700Pore size distribution of synthetic adsorbentsLoading profileMulti column system operationElution profileCER & EquipmentAER and EquipmentDecolorization and RecoveryRunning Cost Simulation
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