MICROENCAPSULATION IN SPICES

Since the prehistoric era, spices and its products are being employed for their medicinal properties. Of all the countries, India has always been home to several spices that are widely used in folk medicine. Among the spices grown in various parts of the world, a major portion of it comes from Asia. While the natural path for enhancing the health and promoting wellness is the need of the hour the emphasis on healthy eating is drawing attention with the referral of spices as the critical ingredients which possess unique flavour profile along with aroma that get slowly degraded and lose their activity thus something called Microencapsulation presents new challenges to food product developers.

1. WELCOME 1

2. Dept. PMA UNIVERSITY OF AGRICULTURAL AND HORTICULTURAL SCIENCES – SHIVAMOGGA COLLEGE OF HORTICULTURE, MUDIGERE Name of the Student I.D.No. Degree Programme Department : Tamanna Arif : MH2TAI240 : Sr. M.Sc . (Hort.) : P SMAC Seminar - I on Microencapsulation in spices 2

3. 1 1 /0 1 /2 20 De p t. P M A 4 What is microencapsulation? History Application of microencapsulation Need for encapsulation in spices Morphology of microcapsules Methods of encapsulation Case studies Conclusion TOPIC DIVISION 3

4. What is microencapsulation? Microencapsulation is defined as a process in which tiny particles or droplets are surrounded by a coating or embedded in a homogeneous or heterogeneous matrix, to give small capsules . Size range : 1 to 1000 μm in diameter 11/01/2020 Dept. PSMAC ( Poshadri and Aparna, 2010 ) 4

5. HISTORY ) In 1932 , introduction of microencapsulation procedure by Bungen burg de John Origin of microencapsulation lies in paper industries by 1940 s Commercial product - microencapsulated ink by America in 1953 (Complex coacervation) Textile industry started introducing many encapsulated products in between 1960 and 1970 Pharmaceutical industry has long used microencapsulation for capsule preparation . Late 1970’s exploration in agriculture, food, cosmetic industries 5

6. The material to be coated is called core material Core materials are either solids, liquids or a mixture of these such as dispersion of solids in liquids . Core material proportion: 20-95% w/w (Bansode et al., 2010) It is a shell or covering material which protect core material from deterioration and evaporation of volatile s. Example: Gums, lipids, proteins, carbohydrates, celluloses etc 0.5-150µm thick (Snehal et al., 2013) 1 1 /0 1 /2 20 Dept. PMA CORE MATERIAL WALL MATERIAL 6

7. Characteristics of wall material Stabilization of core material . Chemically compatible and non reactive . Pliable, stable and non- hygroscopic . Low viscosity . Soluble in an aqueous media or solvent . Inexpensive, food-grade status . Should be flexible, hard, thin, impermeable . Dept. P S MA C ( Saikiran et al ., 2018) 7

8. Commonly used coating materials in food industry Dept. P S MA C Natural polymers Synthetic polymers Proteins : Albumin Gelatin C ol l agen Carbohydrates: Chi t osan Starch Poly dextran Poly starch Gums Gum arabic Sodium alginate Lactides Glycolides Poly alkyl cyano acrylates Poly anhydrides ( Suganya et al., 2017 ) 8

9. Application of microencapsulation Agriculture Animal nutrition (Dubey et al., 2009) 9

10. Dept. PMA Spice oleoresin- complete flavor profile of spices Highly concentrated and viscous Usually volatile and chemically unstable Poor storage life Immiscible in aqueous matrix ( Dubey et al., 2009 ) Why in spices ?? 10

11. Conversion of liquids to free flowing solids Lowers volatility and increases shelf –life of fragrance Masking of odour, taste and activity of encapsulated materials Provide protection from environment and oxidation Controlled release of active compounds Improves bioavailability and stability Need for encapsulation ( Dubey et al., 2009 ) 11

12. Methods of encapsulation Spray- drying Spray chilling Extrusion Fluidized bed coating Lyophilization Coacervation Co-crystallization Inclusion complexation 12

13. 2. Spray chilling Dept. P SMAC ( Saikiran et al ., 2018) 13 Particle size: 20- 200 µm

14. 3. Extrusion Encaps u la t i o n of vola t ile and un s t a b le flav o urs i n glassy carbohydrate matrices . Microcapsules have very long shelf life . Commercially used for encapsulating nutraceutical s . 11/01/2020 Dept. PMA (Quellet et al., 2001) 0.25-2mm (0–500 atm and 70–500°C) 14

15. 4. Fluidized bed coating Also known as suspension coating Principle : Spraying - Evaporation C o a t i n g mat e ri a ls us e d are melted fats, waxes or emulsifiers as shell materials . Particle size: 20 to 1000μm 0 Dept. PMA ( Saikiran et al ., 2018) 15

16. 5. Lyophilization Dept. P S MA C D eh y dra t ion of heat sensitive materials and aromas . Sample frozen (-90 to -40 o C ) Particle Size – 20µm to 5mm ( Shami and Bhasker, 2009) 16

17. 6. Coacervation Known as Phase separation method Core material is dispersed in the solution of coating material. The shell starts to precipitate from the solution. Commonly used wall material- Gum arabic and gelatin . Particle size: 10–800µm Dept. P S MA C (Nicolaas and Shimoni , 2010) 17

18. Schematic representation of coacervation Dept. P S MA C (Nicolaas and Shimoni , 2010) Contd . . 18

19. 7. Co-crystallization Dept. P S MA C New encapsulation process W all material – Sucrose Flow-chart of co-crystallization process Sucrose syrup (supersaturated state ) Addition of core material Vigorous Mec hani c al agi t at i on Nucleat i on Cry s t a l l ize Agitation is continued Agglomerates are discharged Dried (Sanjoy Kumar Das et al. , 2011) 19

20. 8. Inclusion complexation Achieving encapsulation - molecular level Encapsulating medium - β-cyclodextrin Guest molecules – entrapped (dimensionally) by hydrophobic interaction . Internal cavity - 0.65nm diameter Particle size - 0.001– 0. 01µm Dept. P S M AC (Poshadri and Aparna, 2010) 20

21. Dept. PMA Diffusion T emper a tu r e sensitive Solvent- activated Pressure activated Swelling pH -controlled Controlled release m e cha n ism (Jeyakumari et al .,2016) 21

22. 1 1 /0 1 /2 20 5 22

23. Type Oleoresin t 1/2 (weeks) Gum arabic t 1/2 (weeks) Modified starch t 1/2 (weeks) EP - - Y=‒0.0097x +4.601 R²= 0.921 71.44 Y= ‒0.0126x + 4.601 R² = 0.959 55 TP Y= ‒0.125x + 4.604 R² = 0.994 55.44 Y= ‒0.0057x + 4.604 R² = 0.943 121.57 Y= ‒0.0054x + 4.603 R² = 0.958 120.33 TV Y= ‒0.0295x + 4.606 R² = 0.999 23.49 Y= ‒0.0269x + 4.605 R² = 0.997 25.76 Y= ‒0.0263Xx+ 4.618 R² = 0.972 26.34 NV Y= 0.0098x + 4.6045 R² = 0.999 70.71 Y= 0.0089x+ 4.6007 R² = 0.981 77.86 Y= 0.0167x+ 4.5969 R² = 0.981 41.49 Dept. P S MA C Table 1. Analysis for *EP, TP, TV and NV in free and encapsulated oleoresin Oleoresin at 2.5 % based on carrier material used R 2 indicated correlation coefficient ( Shaikh et al ., 20 06) *EP- Entrapped piperine TP- Total piperine TV- Total volatiles NV- Non-volatiles 23

24. Dept. P S MA C (b) Modified starch HiCap-100 Size: 7-20 µm Nearly spherical with smooth surface Size: 5-15 µm Nearly spherical with smooth surface ( Shaikh et a l., 20 06) 24 Fig. 1. Scanning electron microscopic image of spray dried microcapsules (a) Gum arabic

25. Dept. P S MA C ( Xiao et al ., 2014 ) MEY- Microencapsulation Yield MEE- Microencapsulation Efficiency 25 Fig. 2. Effect of emulsification temperature on the morphology, efficiency and yield of capsanthin microcapsules

26. Dept. P S MA C Fi g . 3 . E f fe c t of w al l con c ent r a t i on on t h e morp h olog y , efficiency and yield of capsanthin microcapsules ( Xiao et al ., 2014 ) MEY- Microencapsulation Yield MEE- Microencapsulation Efficiency 26

27. Dept. P S MA C Fig. 4 . E f fe c t of co r e to w all ratio on the mor pholog y , efficiency and yield of capsanthin microcapsules ( Xiao et al ., 2014 ) MEY- Microencapsulation Yield MEE- Microencapsulation Efficiency 27

28. Fig. 4 Effect of temperature on the stability of capsanthin in microcapsules Fig. 5 .Stability of capsanthin in microcapsule in dark (a) and outdoor light (b) (Xiao et al ., 2014) (a) Dark (b) Outdoor light 28

29. Optimum conditions for capsanthin microencapsulation - emulsification temperature 45°C, wall concentration 15 g/l and core to wall ratio 1:2 (w/w) Under these conditions, droplets in emulsion were even in size distribution without agglomeration . Microencapsulation increased the stability of capsanthin against heat and light . Dept. P S MA C Xiao et al ., 2014 29

30. Dept. PMA ( Balasubramani et al ., 2015 ) 30 Fig. 6. Effect of process parameters on encapsulation efficiency of garlic

31. Dept . P S MA C Fig. 7. Determination of optimum conditions Fig. 8. Scanning electron microscopic image of microcapsules ( Balasubramani et al ., 2015 ) 31

32. EE(%) CR(%) Watercontent (% dry basis) Solubility(%) MD:GA(75:25) 11.78 ± 0.51g 40.35 ± 1.01h 4.81 ± 0.06a 91.69 ± 0.04d MD:GA(50:50) 24.60 ± 0.49e 49.59 ± 0.00f 2.14 ± 0.04de 96.50 ± 0.05ab MD:GA(25:75) 40.56 ± 0.05b 65.46 ± 0.13b 2.40 ± 0.08d 95.65 ± 0.25bc GA (100) 16.73 ± 0.19f 24.87 ± 0.18k 4.12 ± 0.05b 92.57 ± 0.28cd GA:MS(25:75) 32.74 ± 0.15d 68.43 ± 0.44a 1.58 ± 005f 99.25 ± 0.00a GA:MS(50:50) 45.23 ± 0.04a 59.15 ± 0.19d 2.14 ± 0.05de 95.63 ± 0.53bc MS (100) 11.84 ± 1.70g 55.48 ± 0.17e 1.01 ± 0.06gh 96.80 ± 0.45ab MD:MS(75:25) 20.72 ± 0.35f 31.33 ± 0.00j 2.90 ± 0.00c 97.35 ± 0.15ab MD:MS(50:50) 7.96 ± 0.38h 35.41 ± 0.00i 1.30 ± 0.01fg 97.88 ± 0.83ab MD:MS(25:75) 18.94 ± 1.32f 41.61 ± 0.36h 0.84 ± 0.16h 95.90 ± 0.02abc MD (100) 36.37 ± 1.36c 36.02 ± 0.74i 2.98 ± 0.03c 97.75 ± 0.45ab MD:GA:MS(17:66:17) 31.51 ± 0.03d 36.35 ± 0.32i 2.78 ± 0.68c 96.90 ± 0.02ab MD:GA:MS(33:33:33) 33.84 ± 0.39d 45.21 ± 0.39g 2.35 ± 0.24de 97.33 ± 0.07ab MD:GA:MS(66:17:17) 33.18 ± 0.29d 54.82 ± 0.08e 2.78 ± 0.44c 85.35 ± 0.50e MD:GA:MS(17:17:66) 31.23 ± 0.60d 61.98 ± 0.35cd 2.10 ± 0.09de 86.83 ± 0.48e Table 2: Properties of turmeric oleoresin microcapsules produced with different wall material formulations. ( Canohiguita et al ., 2015) 32

33. Dept. P S MA C Fig. 9 . Response surface and contour plots for Moisture content Fig 10 . Response surface and contour plots for Particle size ( Noshad et al., 2015) 33

34. Dept. P S MA C Fig. 12 . Morphology of microcapsules at optimal model point (184°C, 8.5%. 0.36%) Fig . 11 . Response surface and contour plots for Encapsulation efficiency (Noshad et al., 2015) 34

35. Optimal condition for vanillin microencapsulation found in 184ºC with 8.5 per cent malto dextrin concentration and 0.3 6 per cent vanillin concentration to obtain maximum encapsulation efficiency ( 58.3% ) and minimum moisture content ( 3.153g/100g ) and particle size ( 6.95µ ) Dept. P S MA C (Noshad et al., 2015) 35

36. Table. 3 . Overview of microencapsulation in various spices E n caps u lat e d material Wall material Method Remarks Cardamom oleoresin (Savitha, 2005) Gum arabic, M altodextrin , modified starch Spray- drying Gum arabic was found to be better wall material than maltodextrins and modified starch Turmeric oleoresin (Kshirsagar et al., 2008) Gum arabic and maltodextrin Spray - drying Gum Arabic supplemented with 1% pullulan proved to be a better wall material in terms of stability and film forming ability for encapsulation of turmeric oleoresin Ethyl vanillin (Verica et al ., 2008) Alginate gel Extrusion Release of ethyl vanillin occurs at about 260°C Dept. P S MA C (Ren u and Z ehr a , 2015) 36

37. E n caps u lat e d material Wall material Method Remarks Ginger oleoresin (Kadam et al .,2010) Acacia gum Spray- drying Inlet temperature of 160°C was optimum in encapsulating ginger oleoresin Star –anise oleoresin ( Wang et al., 2011) Maltodextrin and soy protein Spray- drying Encapsulate of 5% oleoresin with 20% maltodextrin and 7.5% soy protein at an inlet temperature of 180°C was considered as best Nutmeg oleoresin (Arshad et al., 201 4 ) Gum arabic, Native and modified sorghum starches Spray- drying The highest oil retention of 95% with 84.07% encapsulation efficiency was achieved when GA: NA starch was used in the fraction of 25:75. Dept. PSMAC Contd . . (Renu and Zehra, 2015) 37

38. Dept. P S MA C 38

39. S.No. Encapsulated oleoresin Price (Rs/kg) 1. Black pepper 1850 2. Cardamom 7000 3. Turmeric 2500 4. Ginger 1350 5. Garlic 1000 6. Nutmeg 1200 Dept. P S MA C https:// www.synthite.com 39

40. CHALLENGES To produce effective encapsulated products, the appropriate selection of coating material is a great challenge. Multidisciplinary based research approach and consideration of industrial requirements and constraints has to be carried out. 40

41. Conclusion Dept. P S MA C 41

42. 1 1 /0 1 /2 20 Dept. PMA 53 42