Production of High Quality Citrus Pectin Peel

Production of high quality citrus pectin peel

Susanne Oxenbøll Sørensen, CP Kelco ICBC , September 17th 2015

CP Kelco Confidential – Do not copy or share without permission Take Home Message

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!!!

CP Kelco Confidential – Do not copy or share without permission 2 Outline

• CP Kelco • Pectin • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 3 CP Kelco

• CP Kelco • Pectin • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 4 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 Confidential – Do not copy or share without permission 5 CP Kelco CP Kelco Manufacturing sites

Äänekoski, Finland Grossenbrode, Germany

Lille Skensved, Denmark Okmulgee, OK USA

Taixing, China Wulian/Shandong, China

San Diego, CA USA

Cebu, Philippines

Limeira, Brazil

CP Kelco Confidential – Do not copy or share without permission 6 CP Kelco

• Pectin extraction process

CP Kelco Confidential – Do not copy or share without permission 7 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, marinadesGelling & sauces • Water dessert gel

Applications – ConsumerStabilizing & Industrial • Agrochemicals & Animal Feed • Ceramics • Construction (viscosity modifying agent) & Paints • Household Products (paperEmulsifying towels, surface & toilet cleaners, detergents) • Oral Care • Personal Care (creams, gels, shampoo) • Pharmaceuticals • Textile Printing

CP Kelco Confidential – Do not copy or share without permission 8 Pectin

• CP Kelco • Pectin • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 9 Pectin

Schematic pectin structure

Rhamnogalacturonan I Xylogalacturonan Homogalacturonan Rhamnogalacturonan II

= D-Galacturonic acid = L-Arabinose = D-Apiose = O-Acetyl = L-Rhamnose = D-Galactose = L-Fucose = O-Methyl = D-Glucuronic acid = L-Aceric acid = D-Xylose B = Borate = Kdo == DD--DhaDha = L-Galactose

CP Kelco Confidential – Do not copy or share without permission 10 Pectin

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

CP Kelco Confidential – Do not copy or share without permission 11 Pectin

• Pectin quality parameters – Degree of esterification (DE) – Molecular size (Intrinsic viscosity – IV) – Galacturonic acid content (GA)

CP Kelco Confidential – Do not copy or share without permission 12 Pectin

OH OH • Degree of methyl esterificationO O OH   – DE > 50% (HM)4 1 4 OH 1 – DE < 50% (LM)O O O O COOH COOCH3 a. Galacturonic acid b. Methyl esterified galacturonan Methyl esterification of acid groups affects calcium reactivity O

CH3 OH O O  O 4 OH 1  4 OH 1 O O O CONH O 2 COOX c. Amidated galacturonan d. Acetylated galacturonan

CP Kelco Confidential – Do not copy or share without permission X = H, CH3 13

Pectin

• Molecular size (Intrinsic viscosity) – Average molecular size – Typical unit is dl/g – Correlates to grading strength of many applications – HPSEC • Viscotek

CP Kelco Confidential – Do not copy or share without permission 14 Pectin

• Galacturonic acid content – The amount of GA residues relative to the total amount of pectin – Homogalacturonan – Considered the “active” part of pectin

CP Kelco Confidential – Do not copy or share without permission 15 Pectin

• 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

CP Kelco Confidential – Do not copy or share without permission 16 Citrus pectin peel

• CP Kelco • Pectin structure and localization • Pectin quality • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 17 Citrus pectin peel

What happens to the processed peel? Total citrus harvest (2014/15) Source: USDA /FAS Total crop 88,473 kMT 90 % Cattle feed + other

74% Fresh fruit 26% processed

10% Dry peel Estimated annual dry peel production 115,000 MT 1% Other 13% >80% of Lemon/Lime wet peel 30% Orange dry pectin peel Lime

1-2% of Orange wet peel dry pectin peel 56% Lemon CP Kelco Confidential – Do not copy or share without permission 18 Parameters affecting peel quality

• CP Kelco • Pectin • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 19 Parameters affecting peel quality Dry pectin peel process

Fruit Milling

Compactor Juice/oil extraction Wet Dry peel with 10% moisture in 50 kg bales peel Dry peel Cooling

Three pass dryer

Pre-Screw press Tank 3 Tank 2 Tank 1

Pre-dryer single pass Final Screw press

3-step counter current washing 2 step pressing 2 step drying CP Kelco Confidential – Do not copy or share without permission 20 Parameters affecting peel quality

• 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)

CP Kelco Confidential – Do not copy or share without permission 21 Parameters affecting peel quality Dry pectin peel process

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

Important Important Important • Fruit ripeness • pH • Drying temperatures • Fruit quality • Brix • Cooling of peel to • Residence time of • Temperature ambient temperature fruit and peel • Residence time • De-oiling of wet peel • Size distribution after milling CP Kelco Confidential – Do not copy or share without permission 22 Parameters affecting peel quality Fruit ripeness/quality and residence time

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

Important • Fruit ripeness • Fruit quality • Residence time of fruit and peel • De-oiling • Size distribution after milling CP Kelco Confidential – Do not copy or share without permission 23 Parameters affecting peel quality

Best quality at time of juicing… … starts immediately

Enzymatic degradation

Enzymes Endogenous (in the peel) or exogenous (microbial or ”process aid”)

Enzymatic activity depends on temperature and pH

CP Kelco Confidential – Do not copy or share without permission 24 Parameters affecting peel quality Impact of fruit ripeness and wet peel residence time on peel quality

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%

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

CP Kelco Confidential – Do not copy or share without permission 25 Parameters affecting peel quality De-oiling

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

• 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

Rasping Puncturing preferred

CP Kelco Confidential – Do not copy or share without permission 27 Parameters affecting peel quality Peel particle size

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

• 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

CP Kelco Confidential – Do not copy or share without permission 29 Parameters affecting peel quality Washing conditions

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

Important • pH • Brix • Temperature • Residence time of wet peel

CP Kelco Confidential – Do not copy or share without permission 30 Parameters affecting peel quality

• 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

CP Kelco Confidential – Do not copy or share without permission 31 Parameters affecting peel quality Drying temperatures

• Rotary dryer • Counter • Juice/Oil to reach 10% current extraction Wet Dry moisture Fruit washing • Milling of with water • Compacting peel peel peel into 50 kg • Screw press bales

Important • Drying temperatures • Cooling of peel to ambient temperature

CP Kelco Confidential – Do not copy or share without permission 32 Parameters affecting peel quality

• Drying temperature – Pectin chain (IV) degradation accelerates when peel temperature exceeds 90 °C Peel drying temperature and pectin quality 7

6 /g

dL 5

Viscosity 3

Intrinsic 1

0 50 60 70 80 90 100 110 120 130 140 150 Peel temperature (after drying) °C • Recommended drying conditions – Air inlet of dryer <500 °C and outlet 110-120 °C – Peel outlet of dryer 70-80 °C

CP Kelco Confidential – Do not copy or share without permission 33 Summary

• CP Kelco • Pectin • Citrus pectin peel • Parameters affecting peel quality • Summary

CP Kelco Confidential – Do not copy or share without permission 34 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!!!

CP Kelco Confidential – Do not copy or share without permission 35 Acknowledgements

Thanks to my colleagues :

Thomas Alsted

Olney Greilberger

Paul van Wagenen

CP Kelco Confidential – Do not copy or share without permission 36