1. Present by Pitchvipa Prommas Advisor Dr. Apinan Soottitantawat Co-advisor Dr. Uracha Ruktanonchai Encapsulation of menthol in rice starch by spray drying 1

2. Contents Introduction Literature reviews Objectives Experimental Scopes of research 2

3. Introduction 3

4. 4 Cooling Powder

5. Menthol Ref. https://commons.wikimedia.org/wiki/File:Menthol_Reaktionen1.svg 5

6. 6 Talcum Magnesium Silicate or [Mg 3 Si 4 O 10 (OH) 2 ]

7. 7 Commercial cooling powder Talcum is toxic Menthol is high volatile

8. Rice starch Ref. http://library.uru.ac.th/webdb/images/charpa_rice_products.html Thailand has 20,194 tons of rice starch in each year 8

9. 9 Encapsulation core High temperature o2o2 Humidity

10. Encapsulation Fluidized Bed Coacervation Spray Drying Encapsulation 10

11. Encapsulation Coacervation Spray Drying Fluidized Bed 11 core wallcoating

12. Spray drying Low cost Text Encapsulation Simple method 12 Easy to scale up

13. Spray Dryer 13 Ohkawara type L-8 Heater Inlet air temp. (120-180 ºC) Atomizer (30,000 rpm) Cyclone Pump (25 ml/min) Drying chamber Powder Outlet air temp. (65-70ºC) Feed liquid 1. Atomization of liquid feed 2. Evaporation of water 3. Powder separation by cyclone

14. Experimental 14

15. Experimental Preparation of encapsulated menthol powder Analysis of menthol powder 15

16. 8000 rpm, 2 min 8000 rpm, 1 min -Inlet temp 120-180  C -Flow rate 25 and 35 ml/min -Atomizer speed 30000 rpm Preparation of encapsulated menthol powder Melted menthol Rice starch -Casein as surfactant -Maltodextrin -Distilled water

17. - Morphology by SEM JSM-6060 encapsulated powders 17 Analysis of menthol powder Ref. http://www.speciation.net/Database/Instruments/JEOL/JSM6060-;i19

18. encapsulated powders 18 Analysis of menthol powder -Menthol content by GC-2014 Retention (%) = R2 x 100 R1 R1 = initial menthol content in feed R2 = menthol content retained in the powder product

19. 19 encapsulated powders Analysis of menthol powder - Water content by vacuum dryer ADP-21 Water content ＝ W1-W2-[M1-M2] W1 = weight of encapsulated powder before drying W2 = weight of encapsulated powder after drying for 20 hr M1 = weight of menthol in encapsulated powder before drying M2 = weight of menthol in encapsulated powder after drying for 20 hr

20. 20 Expected results

21. Applying the encapsulation technique for cosmetic industry or pharmaceutical industry Applying the encapsulation technique for cosmetic industry or pharmaceutical industry Getting long lasting cooling powder 21

22. 22 Results

23. Improving retention by adding casein and maltodextrin Comparison with commercial powder 23 -Inlet temperature -Feed flow rate -Atomizer speed Spray drying parameter

24. 24 Effect of surfactant

25. 25 Retention (%) Emulsion size (μm) control1.811.85 with casein 5%4.04.09 Menthol 20 wt % dry basis

26. 26 Menthol 20 wt % dry basis ControlWith casein 5%

27. Effect of maltodextrin content

28. Maltodextrin Content (%) Retention (%) Particle size (μm) Water content (%) 013.5428.6 536.7445.5 1073.7546.2 2057.1484.1 Casein 5 wt%, Menthol 10 wt% dry basis

29. MD = 0% MD = 10% MD = 5% MD = 20% Casein 5 wt %, Menthol 10 wt % dry basis

30. 30 MD = 0%MD = 5%MD = 10%MD = 20% Casein 5 wt%, Menthol 10 wt % dry basis

31. Emulsion size distribution MD = 0% MD = 5% MD = 20% MD = 10%

32. 32

33. Effect of inlet temperature

34. Inlet temperature ( ° C) Retention (%) Particle size (μm) Water content (%) 12063.1527.9 14054.4566.4 16048.2585.3 18048.8542.9 Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

35. 120 ° C 140 ° C160 ° C 180 ° C Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

36. 36 120 ° C 140 ° C160 ° C 180 ° C Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

37. 37

38. 38 Emulsion size distribution 120 ° C140 ° C 160 ° C180 ° C

39. Effect of feed flow rate

40. Feed flow rate (ml/min) Retention (%) Particle size (μm) Water content (%) 2573.7546.2 3540.8428.5 Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

41. 41 Emulsion size distribution Flow 35 ml/min Flow 25 ml/min

42. Flow 35 ml/min Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

43. 43

44. 44 Effect of atomizer speed

45. 45 Atomizer speed(rpm) Retention (%) Particle size (μm) Water content (%) 1000063.1527.9 3000073.7546.2 Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

46. 46 10000 rpm30000 rpm Casein 5 wt%, Menthol 10 wt%, Maltodextrin 10 wt%

47. 47 Emulsion size distribution 10000 rpm30000 rpm

48. 48

49. 49 Comparison between encapsulated powder and commercial powder

50. 50 Sample mg menthol/ g powder Powder size (μm) Morphology Encapsulated powder 80.2 54 Commercial powder 6.0 66

51. Conclusion 51

52. 52 Conclusion Adding maltodextrin can get more retention. Spray drying parameter ► Lower inlet temperature ► Lower feed flow rate ► Higher atomizer speed

53. Thank You Q&A 53