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PHYTOCHEMICAL  PROCESSING SAIFUL IRWAN ZUBAIRI   PMIFT, Grad B.E.M.   B. Eng. (Chemical-Bioprocess) (Hons.), UTM M. Eng. (Bioprocess), UTM ROOM NO.: 2166, CHEMISTRY BUILDING, TEL. (OFF.): 03-89215828, FOOD SCIENCE PROGRAMME, CENTRE OF CHEMICAL SCIENCES AND FOOD TECHNOLOGY,  UKM BANGI, SELANGOR
PROCESSING OBJECTIVES ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Chart of Classification and Separation of Plant Material Based on Solvent Polarity and Process  (Phytochemicals Approach) Plant  Material H2O-Glycerol Extraction Non-Polar compound extraction SFE (Phytonics: Phytosol) Terpenoids Essential Oil (e.g. mono & Esquiterpenes: geraniol, limonese Diterpenoids (Phytol, abietic acid) Triterpenoids (Cucurbitacin) Carotenoids ( β-Carotene, lutien, Zeaxanthin, etc) Multi Solvent Extraction  Process Terpenoids (e.g. Menthol, carrone, squalene, α-Carotene, lycopene) Lipids Polar Compound Extraction Flavanoid (e.g. anthocyanin-cyanidin, flavanols- Kaemferol, isoflavanoid-rotenone) Polar alkaloid (e.g. Ephedrine) Sugar & Derivatives (e.g. monosacharide, Oligosacharide, sugar alcol) Fiber Acid  Hydrolysis filtrate Cellulose filtrate Hemicellulose filtrate Lignin
Chart of Classification and Separation of Plant Material Based on Solvent Polarity and Process  (Herbal Approach) Plant Material Solvent Extract filtrate Freeze dried Whole concrete extract Membrane  Filtration or  Low T vacuum evaporation Whole concentrate extract Water Extract Spray dried Whole powder extract Freeze dried Whole freeze dried extract Spray dried Concentrate extract
EXAMPLES OF RAW MATERIALS TEA TREE PANDAN CITRONELLA EUCALYPTUS CINNAMON KESUM CURRY TONGKAT ALI
OVERALL PROCESSING TECHNIQUES
PRETREATMENT OF HERBS
PREPARATION OF RAW MATERIAL AND THE  PROCESSING OF ESSENTIAL OILS RAW MATERIAL PRETREATMENT PROCESS EXTRACTION PURIFICATION
Percolation Process
Reflux Extraction
Soxhlet Extraction
Steam Distillation
Phytosol Extractor (industrial scale)
PURIFICATION PROCESSES
FREEZE DRYING ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
SPRAY DRYER ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
PHYTOCHEMICAL PROCESSING :  CASE STUDIES
CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves   Process Flow Chart for Crude Cinnamon Oil Production Cinnamon Leaves Drying Size Reduction Extraction ( Apply heat & agitation) Condensation Product (Crude Essential Oil) Deionized Water Steam is formed carrying along essential oil
Process Flow Chart for Crude Cinnamon Oil Purification Crude Essential Oil Neutralization (pH Control) Separation (centrifuge) Other method: clarifying, purifying and decanting Product (Essential Oil) Distillation  (using laboratory set) Solvent Solubility (add solvent) Evaporation CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves
C Cinnamon Leaf (1000 kg) 1000 kg COARSE GRINDER Deionized water   (5000 kg)  Condensation Rate  : 700 kg/hr Water Oil (15%) Oil (85%) Leaf + 30% water Water + Oil 1 L  0.5 M NaOH 26 L Cinnamon Oil C Soap Purified Cinnamon Oil (25 L) CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves
CASE STUDY II: Production of Phyto-Extract from Tongkat Ali Process Flow Chart for Herb Processing – Tongkat Ali Tongkat Ali Sizing (Grinding)/Drying Extraction Filtration Product (Concentrate Extract) Packaging Solvent (Deionized Water) Spray Dryer  (other product intensification method can also be used - freeze drying) Concentrate Product (Powdered Form) EXTRACTION
CASE STUDY II: Production of Phyto-Extract from Tongkat Ali Deionized Water  (120kg) T = 120 O C t  = 2 Hr Extract + fibre (40kg) Slurry Water Extract   T  feed  = 70 O C 1.5 brix FILTER efficiency = 56% EXTRACTOR SPRAY DRYER efficiency = 80% Hot Air   306 kg/hr T = 170 O C T 1  = 170 O C T 2  = 103 O C Evaporation Rate = 12.6 kg/hr Recovery = 3% Moisture content = 2% t  = 7 hrs HOLDING TANK Temperature = 70 0 C Tongkat Ali  (40kg)
CASE STUDY III: Production of Soybean Powder Soy bean Soak (24 hrs) Dehulling Wet Grinding  (Soy: Water  1:4) Soy Extract Product Solvent (Deionized Water) Filtration Spray Dry T = 90 0 C, t = 1 hr 5% Maltodextrin,  1% Sodium Casienate
Dehulling 1000 kg Soy 4000 kg Deionized water Soy Fiber 4000 kg extract 200 kg Maltodextrin 40 kg Sodium Casienate T = 90 0 C t  = 1 hr 2420 kg Soy Solution 2 brix T 1  = 185 0 C T 2  = 105 0 C Hot Air Feed (2300 kg/ hr) t  =  24 hrs Evaporation Rate = 100 kg/ hr Product Flow Rate = 20.16 kg / hr Recovery = 20 % Moisture content = 2 % CASE STUDY III: Production of Soybean Powder Wet Grinding Filter Press
CASE STUDY IV: Extraction of Oleoresin (Curcuminoid) from Turmeric Process Flow Chart for Production of Cucurminoid Turmeric Sizing & Drying Steam Distillation Wet Turmeric Fine Grinding Crystallization Solvent (Deionized Water) Drying Vacuum Distillation Volatile Oil Product (Curcuminoid) Packaging Ethanol
CASE STUDY IV:Extraction of Oleoresin (Curcuminoid) from Turmeric Coarse Grinder Fine Grinder 1000 Kg Turmeric 5000 kg Dioinized water Evaporation Rate:  833 kg/hr 4200 kg water + volatile Oil Water 20 kg volatile oil 70% Water 600 kg fine turmeric 800 kg water + 1000 kg turmeric DRYER VACUUM DISTILLATION UNIT STEAM DISTILLATION UNIT OIL SEPARATOR OIL STORAGE Volatile Oil Packaging CRYSTALLIZER 24 Kg Curcuminoid FILTER UNIT EXTRACTION VESSEL
Raw Material Sizing (Grinding)/Drying Extraction Filtration Ultrafiltration Spray Dryer Solvent (Deionized Water) Microfiltration Reverse Osmosis PURIFICATION CASE STUDY V: Production of Plant-Based Sugar from Stevia Product (Stevioside: 66%) T = 100 0 C, t = 2 hrs Maltodextrin
CASE STUDY V: Production of Plant-Based Sugar from Stevia Sweet Tea (100kg) Deionized Water  (2500kg) T = 100 O C t  = 2 hrs Water Extract Water Extract   (400 kg solution + 2 kg maltodextrin) T feed = 70 O C 1.5 brix EXTRACTOR SPRAY DRYER efficiency = 80% Hot Air   550kg/hr T = 170 O C T 1  = 170 O C T 2  = 103 O C Evaporation Rate = 100 kg/hr Product Flow Rate = 1.75 kg/hr Recovery = 5% Moisture content = 2% Purity = 66% t  = 4 hrs PURIFICATION (microfiltration, Ultrafiltration Reverse osmosis) Impurities
CASE STUDY VI: Production of Pegaga Powder  M EXTRACTOR M M Pegaga (cleaned and ground) Deionized Water  BLENDING TANK EVAPORATOR SPRAY DRYER PLATE & FRAME FILTER T = 120 0 C t = 2 hrs T = 70 0 C Water Extract   T  feed   = 70 O C 5 brix Hot Air   306 kg/hr T = 170 O C T 1  = 170 O C T 2  = 103 O C Recovery = 2% from raw material Moisture content = 2% max Water Process Plant Layout for the Production of Pegaga Powder
Pegaga Cleaning Sizing Extraction Evaporation Blending Spray Drying Packaging Dehydrated Product Figure 1: Process Flow for the Production of Pegaga Powder

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Phytochemical Processing

  • 1. PHYTOCHEMICAL PROCESSING SAIFUL IRWAN ZUBAIRI PMIFT, Grad B.E.M. B. Eng. (Chemical-Bioprocess) (Hons.), UTM M. Eng. (Bioprocess), UTM ROOM NO.: 2166, CHEMISTRY BUILDING, TEL. (OFF.): 03-89215828, FOOD SCIENCE PROGRAMME, CENTRE OF CHEMICAL SCIENCES AND FOOD TECHNOLOGY, UKM BANGI, SELANGOR
  • 2.
  • 3. Chart of Classification and Separation of Plant Material Based on Solvent Polarity and Process (Phytochemicals Approach) Plant Material H2O-Glycerol Extraction Non-Polar compound extraction SFE (Phytonics: Phytosol) Terpenoids Essential Oil (e.g. mono & Esquiterpenes: geraniol, limonese Diterpenoids (Phytol, abietic acid) Triterpenoids (Cucurbitacin) Carotenoids ( β-Carotene, lutien, Zeaxanthin, etc) Multi Solvent Extraction Process Terpenoids (e.g. Menthol, carrone, squalene, α-Carotene, lycopene) Lipids Polar Compound Extraction Flavanoid (e.g. anthocyanin-cyanidin, flavanols- Kaemferol, isoflavanoid-rotenone) Polar alkaloid (e.g. Ephedrine) Sugar & Derivatives (e.g. monosacharide, Oligosacharide, sugar alcol) Fiber Acid Hydrolysis filtrate Cellulose filtrate Hemicellulose filtrate Lignin
  • 4. Chart of Classification and Separation of Plant Material Based on Solvent Polarity and Process (Herbal Approach) Plant Material Solvent Extract filtrate Freeze dried Whole concrete extract Membrane Filtration or Low T vacuum evaporation Whole concentrate extract Water Extract Spray dried Whole powder extract Freeze dried Whole freeze dried extract Spray dried Concentrate extract
  • 5. EXAMPLES OF RAW MATERIALS TEA TREE PANDAN CITRONELLA EUCALYPTUS CINNAMON KESUM CURRY TONGKAT ALI
  • 8. PREPARATION OF RAW MATERIAL AND THE PROCESSING OF ESSENTIAL OILS RAW MATERIAL PRETREATMENT PROCESS EXTRACTION PURIFICATION
  • 15.
  • 16.
  • 18. CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves Process Flow Chart for Crude Cinnamon Oil Production Cinnamon Leaves Drying Size Reduction Extraction ( Apply heat & agitation) Condensation Product (Crude Essential Oil) Deionized Water Steam is formed carrying along essential oil
  • 19. Process Flow Chart for Crude Cinnamon Oil Purification Crude Essential Oil Neutralization (pH Control) Separation (centrifuge) Other method: clarifying, purifying and decanting Product (Essential Oil) Distillation (using laboratory set) Solvent Solubility (add solvent) Evaporation CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves
  • 20. C Cinnamon Leaf (1000 kg) 1000 kg COARSE GRINDER Deionized water (5000 kg) Condensation Rate : 700 kg/hr Water Oil (15%) Oil (85%) Leaf + 30% water Water + Oil 1 L 0.5 M NaOH 26 L Cinnamon Oil C Soap Purified Cinnamon Oil (25 L) CASE STUDY I: Production of Cinnamon Oil from Cinnamon Leaves
  • 21. CASE STUDY II: Production of Phyto-Extract from Tongkat Ali Process Flow Chart for Herb Processing – Tongkat Ali Tongkat Ali Sizing (Grinding)/Drying Extraction Filtration Product (Concentrate Extract) Packaging Solvent (Deionized Water) Spray Dryer (other product intensification method can also be used - freeze drying) Concentrate Product (Powdered Form) EXTRACTION
  • 22. CASE STUDY II: Production of Phyto-Extract from Tongkat Ali Deionized Water (120kg) T = 120 O C t = 2 Hr Extract + fibre (40kg) Slurry Water Extract T feed = 70 O C 1.5 brix FILTER efficiency = 56% EXTRACTOR SPRAY DRYER efficiency = 80% Hot Air 306 kg/hr T = 170 O C T 1 = 170 O C T 2 = 103 O C Evaporation Rate = 12.6 kg/hr Recovery = 3% Moisture content = 2% t = 7 hrs HOLDING TANK Temperature = 70 0 C Tongkat Ali (40kg)
  • 23. CASE STUDY III: Production of Soybean Powder Soy bean Soak (24 hrs) Dehulling Wet Grinding (Soy: Water 1:4) Soy Extract Product Solvent (Deionized Water) Filtration Spray Dry T = 90 0 C, t = 1 hr 5% Maltodextrin, 1% Sodium Casienate
  • 24. Dehulling 1000 kg Soy 4000 kg Deionized water Soy Fiber 4000 kg extract 200 kg Maltodextrin 40 kg Sodium Casienate T = 90 0 C t = 1 hr 2420 kg Soy Solution 2 brix T 1 = 185 0 C T 2 = 105 0 C Hot Air Feed (2300 kg/ hr) t = 24 hrs Evaporation Rate = 100 kg/ hr Product Flow Rate = 20.16 kg / hr Recovery = 20 % Moisture content = 2 % CASE STUDY III: Production of Soybean Powder Wet Grinding Filter Press
  • 25. CASE STUDY IV: Extraction of Oleoresin (Curcuminoid) from Turmeric Process Flow Chart for Production of Cucurminoid Turmeric Sizing & Drying Steam Distillation Wet Turmeric Fine Grinding Crystallization Solvent (Deionized Water) Drying Vacuum Distillation Volatile Oil Product (Curcuminoid) Packaging Ethanol
  • 26. CASE STUDY IV:Extraction of Oleoresin (Curcuminoid) from Turmeric Coarse Grinder Fine Grinder 1000 Kg Turmeric 5000 kg Dioinized water Evaporation Rate: 833 kg/hr 4200 kg water + volatile Oil Water 20 kg volatile oil 70% Water 600 kg fine turmeric 800 kg water + 1000 kg turmeric DRYER VACUUM DISTILLATION UNIT STEAM DISTILLATION UNIT OIL SEPARATOR OIL STORAGE Volatile Oil Packaging CRYSTALLIZER 24 Kg Curcuminoid FILTER UNIT EXTRACTION VESSEL
  • 27. Raw Material Sizing (Grinding)/Drying Extraction Filtration Ultrafiltration Spray Dryer Solvent (Deionized Water) Microfiltration Reverse Osmosis PURIFICATION CASE STUDY V: Production of Plant-Based Sugar from Stevia Product (Stevioside: 66%) T = 100 0 C, t = 2 hrs Maltodextrin
  • 28. CASE STUDY V: Production of Plant-Based Sugar from Stevia Sweet Tea (100kg) Deionized Water (2500kg) T = 100 O C t = 2 hrs Water Extract Water Extract (400 kg solution + 2 kg maltodextrin) T feed = 70 O C 1.5 brix EXTRACTOR SPRAY DRYER efficiency = 80% Hot Air 550kg/hr T = 170 O C T 1 = 170 O C T 2 = 103 O C Evaporation Rate = 100 kg/hr Product Flow Rate = 1.75 kg/hr Recovery = 5% Moisture content = 2% Purity = 66% t = 4 hrs PURIFICATION (microfiltration, Ultrafiltration Reverse osmosis) Impurities
  • 29. CASE STUDY VI: Production of Pegaga Powder M EXTRACTOR M M Pegaga (cleaned and ground) Deionized Water BLENDING TANK EVAPORATOR SPRAY DRYER PLATE & FRAME FILTER T = 120 0 C t = 2 hrs T = 70 0 C Water Extract T feed = 70 O C 5 brix Hot Air 306 kg/hr T = 170 O C T 1 = 170 O C T 2 = 103 O C Recovery = 2% from raw material Moisture content = 2% max Water Process Plant Layout for the Production of Pegaga Powder
  • 30. Pegaga Cleaning Sizing Extraction Evaporation Blending Spray Drying Packaging Dehydrated Product Figure 1: Process Flow for the Production of Pegaga Powder