production of high quality citrus pectin peel - uf/ifas...

CP Kelco Confidential – Do not copy or share without permission

Production of high quality citrus pectin peel

Susanne Oxenbøll Sørensen, CP KelcoICBC , September 17th 2015

CP Kelco Confidential – Do not copy or share without permission2

In case you are already fantasizing about drinks in the bar….

• High quality citrus pectin peel

– Efficient washing and drying process

• Peel particle size

– Control of enzymatic acitivity

• Time

• pH

– Don’t burn the pectin peel!!!

Take Home Message


• CP Kelco

• Pectin

• Citrus pectin peel

• Parameters affecting peel quality

• Summary

Outline


• CP Kelco

• Pectin



• Summary

CP Kelco


• CP Kelco is a hydrocolloids producer 100% owned by the JM Huber Corporation

• JM Huber is a 120 year old family owned corporation comprising CP Kelco, Huber Engineered Woods and Huber Engineered Materials

• CP Kelco’s Hydrocolloid portfolio – Pectin

• Extracted from citrus peel (DEN, GER, BRA)

– Carrageenan

• Extracted from seaweed (DEN, PHI)

– Carboxymethyl Cellulose (CMC)

• Manufactured from wood pulp or cotton linters (FIN, CHN)

– Biogums (Gellan, Xanthan and Diutan)

• Produced by fermentation (USA, CHN)

CP Kelco


CP Kelco

Lille Skensved,Denmark

Limeira, Brazil

Grossenbrode, Germany

Cebu, Philippines

San Diego, CAUSA

Okmulgee, OK

USA

Äänekoski, Finland

Wulian/Shandong, China

Taixing, China

CP Kelco Manufacturing sites


• Pectin extraction process

CP Kelco


CP Kelco

Applications – Food & Beverage• Bakery• Beverage systems• Confectionery• Dairy (cheeses, ice cream, yogurts and desserts)• Fruit based products including jams/jellies• Meat, poultry, analogue and fish processing • Salad dressings, marinades & sauces • Water dessert gel

Applications – Consumer & Industrial

• Agrochemicals & Animal Feed• Ceramics• Construction (viscosity modifying agent) & Paints• Household Products (paper towels, surface &

toilet cleaners, detergents)• Oral Care• Personal Care (creams, gels, shampoo) • Pharmaceuticals• Textile Printing

GellingStabilizingEmulsifying


• CP Kelco

• Pectin



• Summary

Pectin


Pectin

Rhamnogalacturonan I Homogalacturonan Rhamnogalacturonan IIXylogalacturonan

B

Schematic pectin structure

= L-Rhamnose

= D-Galacturonic acid = L-Arabinose

= D-Galactose

= O-Acetyl

= O-Methyl

= D-Glucuronic acid = Borate

= D-Apiose

= L-Fucose

= L-Aceric acid = D-Xylose

= Kdo = D-Dha

B

= L-Galactose= D-Dha


Pectin

• Model of plant cell wall structure - pectin is the glue


• Pectin quality parameters

– Degree of esterification (DE)

– Molecular size (Intrinsic viscosity – IV)

– Galacturonic acid content (GA)

Pectin


• Degree of methyl esterification

– DE > 50% (HM)

– DE < 50% (LM)

Pectin

O

O

COOH

OH

OH

O

4 1

O

O

CONH2

OH

OH

O

4 1

O

O

COOCH3

OH

OH

O

4 1

O

O

COOX

O

OH

O

CH3

O

4 1

X = H, CH3

a. Galacturonic acid b. Methyl esterified galacturonan

c. Amidated galacturonan d. Acetylated galacturonan

Methyl esterification of acid groups affects calcium reactivity


• Molecular size (Intrinsic viscosity)

– Average molecular size

– Typical unit is dl/g

– Correlates to grading strength of many applications

– HPSEC • Viscotek

Pectin


• Galacturonic acid content

– The amount of GA residues relative to the total amount of pectin

– Homogalacturonan

– Considered the “active” part of pectin

Pectin

B


• The best preserved pectin precursor is always the preferred choice

• Citrus peel is by nature an excellent precursor

– High yield and quality

– Available in sufficient amount

– Stable and consistent supply…

However…

attention/effort is required to ensure high peel quality

Pectin


• CP Kelco

• Pectin structure and localization

• Pectin quality



• Summary

Citrus pectin peel


Citrus pectin peel

Total citrus harvest (2014/15)Source: USDA /FAS

Total crop 88,473 kMT

26% processed74% Fresh fruit

Estimated annual dry peel production 115,000 MT

What happens to the processed peel?

90 % Cattle feed + other

10% Dry peel

>80% of Lemon/Lime wet peel dry pectin peel

1-2% of Orange wet peel dry pectin peel

30% Lime

56% Lemon

13% Orange

1% Other


• CP Kelco

• Pectin



• Summary

Parameters affecting peel quality



Juice/oil extraction

Pre-Screw press

3-step counter current washing

Final Screw press

Tank 3 Tank 2 Tank 1

2 step pressing

Pre-dryer single pass

Three pass dryer

Compactor

Cooling

FruitMilling

Wet peel

Dry peel

Dry peel with 10% moisture in 50 kg bales

Dry pectin peel process

2 step drying

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• Why is washing and drying required?

– Increase net pectin content = pectin extraction yield

– Prevent further degradation = stabilize pectin• Long distance transport of peel (South America – Europe)



• Juice/Oil extraction

• Milling of peel

Fruit

• Counter current washing with water

• Screw press

Wet peel

• Rotary dryer to reach 10% moisture

• Compacting into 50 kg bales

Dry peel


Important• pH• Brix• Temperature• Residence time

of wet peel

Important• Fruit ripeness• Fruit quality• Residence time of

fruit and peel• De-oiling• Size distribution after

milling

Important• Drying temperatures• Cooling of peel to

ambient temperature

Dry pectin peel process




• Milling of peel

Fruit


• Screw press

Wet peel



Dry peel



milling

Fruit ripeness/quality and residence time



Best quality at time of juicing… … starts immediately

EnzymesEndogenous (in the peel) or exogenous (microbial or ”process aid”)

Enzymatic activity depends on temperature and pH

Enzymaticdegradation



Quality Hours’ residence time from juice extraction to washing/drying

Production

month 0h 1h 2h 3h 4h 5h 6h 7h

Season start 100% 97% 94% 91% 88% 85% 82% 79%

1 Month 99% 96% 93% 90% 87% 84% 81% 78%

2 Month 98% 95% 92% 89% 86% 83% 80% 77%

3 Month 96% 94% 91% 88% 85% 82% 79% 76%

4 Month 95% 92% 89% 87% 84% 81% 78% 75%

5 Month 94% 91% 88% 86% 83% 80% 77% 74%

6 Month 93% 90% 87% 84% 82% 79% 76% 73%

7 Month 92% 89% 86% 83% 81% 78% 75% 72%

Impact of fruit ripeness and wet peel residence time on peel quality

1.2% loss of functionality per month and 3% per hour




• Milling of peel

Fruit


• Screw press

Wet peel



Dry peel



milling

De-oiling


• De-oiling prior to juicing

– De-oiling by gently puncturing oil cells (Flavedo layer) is an advantage versus rasping technology• The hard and water repellant peel surface is opened and permeable to

water both during peel washing and during pectin extraction process


Puncturing preferredRasping




• Milling of peel

Fruit


• Screw press

Wet peel



Dry peel



milling

Peel particle size


• Peel Particle size

– Uniform particle size is recommended• Preferably ~5mm

• Important to adjust mill according to peel hardness and keep knives sharp

– Uniform particle size distribution means• Easier removal of soluble solids during washing (increasing pectin yield)

• Gentle but effective drying without burning small particles

– Larger particles contain more moisture – more difficult to dry





• Milling of peel

Fruit


• Screw press

Wet peel



Dry peel

Important• pH• Brix• Temperature• Residence time

of wet peel

Washing conditions


• Washing conditions

– pH - the ”regulator” of enzymes• General conditions – we recommend pH 4 (last wash/final press)

– At pH >4 DE reducing enzymes are active

– At pH <4 IV reducing enzymes are active

– Brix – indicator of washing efficiency (removed soluble solids)• As low as possible is preferred

• Depend on local conditions

– Temperature – ambient is preferred• Increased solubility and thus higher washing efficency at higher temp.

• But enzymatic activity is then also increased

– Time – no residence time of washed peel• Increased risk of enzymatic degradation





• Milling of peel

Fruit


• Screw press

Wet peel



Dry peel

Important• Drying temperatures• Cooling of peel to

ambient temperature

Drying temperatures



• Drying temperature

– Pectin chain (IV) degradation accelerates when peel temperature exceeds 90 °C

• Recommended drying conditions

– Air inlet of dryer <500 °C and outlet 110-120 °C

– Peel outlet of dryer 70-80 °C

0

1

2

3

4

5

6

7

50 60 70 80 90 100 110 120 130 140 150

Intr

insi

c V

isco

sity

dL/

g

Peel temperature (after drying) °C

Peel drying temperature and pectin quality


• CP Kelco

• Pectin



• Summary

Summary


• High quality citrus pectin peel

– Efficient washing and drying process

• Peel particle size

– Control of enzymatic acitivity

• Time

• pH

– Don’t ”burn” the pectin peel!!!

Summary


Acknowledgements

Thanks to my colleagues :

Thomas Alsted

Olney Greilberger

Paul van Wagenen

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