Effect of Spray Drying Conditions on Physical and Chemical Properties of Dried Green Tea Extract (Camellia sinensis var. Oolong No 12).

ii

EFFECT OF SPRAY DRYING CONDITIONS ON PHYSICAL AND CHEMICAL

PROPERTIES OF DRIED GREEN TEA EXTRACT (

Camellia sinensis

var. Oolong

No 12)

Sari Wahyuni1, Purwiyatno Hariyadi1, Hanifah Nuryani Lioe1, Natthawuddi Donlao2

1

Departement of Food Science and Technology, Faculty of Agricultural Engineering Technology, Bogor Agricultural University, IPB Darmaga Campus, PO. BOX 220, Bogor, West Java, Indonesia

2_{School of Agro-Industry, Mae Fah Luang University, Muang, Chiang Rai 57100, Thailand}

ABSTRACT

The effect of spray drying conditions on physical and chemical dried green tea (Camellia sinensis var. Oolong No 12) extract were observed. Tea extract was prepared from milled dried tea, dissolved in hot water at temperature 90°C and ratio of dried tea to water 1: 20 (w / v). The time of extraction used was 60 minutes, and pH value was 5.0. Then, tea extract was concentrated with ice maker machine until reached 3, 6 and 9% of total solid, and dried with spray drier with condition inlet air temperatures were 180, 200, 220°C, outlet air temperatures was controlled 75°C, blower speed was adjusted in 2500 rpm. The physical analysis, such as bulk density, color, solubility, hygroscopicity, and the chemical analysis, such as moisture content, total polyphenols content, antioxidant activity (DPPH assay), catechins, and caffeine content were determined. Results showed that different solid concentration of 3, 6, 9% in feed and inlet air temperatures of 180, 200, and 220˚C affected the variation of physical and chemical properties of green tea powder. An increase inlet air temperature, resulted in a significant decrease (p<0.05) in bulk density, hygroscopicity, total polyphenols and antioxidant activity. An increase of solid concentration in feed gave an increase in tea powder solubility, L, a, b value, and antioxidant activity. However, the total polyphenols contents were not affected by the increase. The condition of feed concentrated to 3% and inlet temperature at

220˚C was evaluated with the highest of physical, chemical results and the highest of kg water removal/hour by spray dryer.

41

42 Appendix 1. Condition of Spray Drying Process

Condition of Spray Drying Process Conc. %Total Solid

(oven)

Inlet

Temp. (˚C) Temp. (˚C) Outlet blower speed

Inlet humidity Outlet humidity

3% 3.0529 180 75 2500 69-73% / 32.8˚C 71% / 30.5˚C

3.0529 200 75 2500 62% / 32˚C 59% / 32.8˚C

3.0529 220 75 2500 72-73% / 29.3˚C 67-69% / 30.1˚C

6% 5.9862 180 75 2500 68% / 29.8˚C 70% / 30.1˚C

5.9862 200 75 2500 71% / 29.5˚C 70% / 28.9˚C

5.9862 220 75 2500 75% / 28.9˚C 72% / 29.3˚C

9% 8.9595 180 75 2500 65%/ 31.6˚C 66% / 30.9˚C

8.9595 200 75 2500 70% / 28.9˚C 73% / 27.7˚C

43 Appendix 2. Clasification of Hygrospocity Type of Powder Product (GEA Niro Research

Laboratory) Hygroscopicity

Non hygroscopic: ;<10%

Slightly hygroscopic: 10.1-15%

Hygroscopic: 15.1-20%

Very hygroscopic: 20.1-25%

44 Appendix 3. Data and Calibration Curve of Gallic Acid Standard by Spectrophotometer

Con. Abs.1 Abs.2 Abs.3 Average SD

0 0.0758 0.0756 0.0759 0.0758 0.0002

10 0.2040 0.2166 0.2157 0.2121 0.0070

20 0.3402 0.3243 0.3339 0.3328 0.0080

30 0.4762 0.4515 0.4592 0.4623 0.0126

40 0.5703 0.5941 0.5609 0.5751 0.0171

50 0.7070 0.7258 0.6792 0.7164 0.0133

60 0.8341 0.8265 0.8351 0.8319 0.0047

70 0.9340 0.8864 0.9263 0.9156 0.0256

80 1.0452 1.0402 1.0579 1.0478 0.0091

90 1.1513 1.1698 1.1567 1.1593 0.0095

100 1.2461 1.2966 1.2720 1.2716 0.0253

y = 0.0119x + 0.0966 R² = 0.9987 0.00

0.20 0.40 0.60 0.80 1.00 1.20 1.40

0 20 40 60 80 100 120

A

bs

orbanc

e

Conc. Gallic acid (ug/ml)

Gallic acid calibration curve

45 Appendix 4. Data of Trolox and DPPH preparation; Data of Standard Trolox; Standard Trolox

Calibration Curve by Spectrophotometer Trolox + DPPH preparation

Name MW Weight

Vol.

MeOH Con.

(g) (mL) (mM)

Trolox 250.32 0.0250 10 9987.22

DPPH 394 0.0024 100 60.91

Reaction

Std or sample 50 mL + 2000 mL DPPH incubate at RT for 30 min in a dark place. Measure A 517 nm using MeOH as blank

Standard trolox

Level Con. A 517 %Inhibition

(mM) 1 2 3 mean

1 0 1.0364 0.9335 0.9589 0.9763 0.00

2 200 0.8568 0.8486 0.7278 0.8111 16.92

3 399 0.6424 0.7035 0.7014 0.6824 30.10

4 599 0.5327 0.5294 0.3724 0.4782 51.02

5 799 0.3003 0.2862 0.3013 0.2959 69.69

6 999 0.1476 0.1707 0.1763 0.1649 83.11

y = 0.0851x - 0.6762 R² = 0.9963

-20.00 0.00 20.00 40.00 60.00 80.00 100.00

0 200 400 600 800 1000 1200

%

In

h

ib

ition

Concentract (uM)

Trolox

46 Appendix 5. Data of Concentration Caffeine and Catechin in Mix Standard

Concentration

Con.Mix G GC EGC C EC EGCG CF GCG ECG CG

(µg/mL) 99.9 39.2 40.18 100 97 80 100 40.18 98 49

1 0.20 0.08 0.08 0.20 0.19 0.16 0.20 0.08 0.20 0.10 2 1.00 0.39 0.40 1.00 0.97 0.80 1.00 0.40 0.98 0.49 3 5.00 1.96 2.01 5.00 4.85 4.00 5.00 2.01 4.90 2.45 4 9.99 3.92 4.02 10.00 9.70 8.00 10.00 4.02 9.80 4.90 5 19.98 7.84 8.04 20.00 19.40 16.00 20.00 8.04 19.60 9.80 6 39.96 15.68 16.07 40.00 38.80 32.00 40.00 16.07 39.20 19.60 7 59.94 23.52 24.11 60.00 58.20 48.00 60.00 24.11 58.80 29.40 8 79.92 31.36 32.14 80.00 77.60 64.00 80.00 32.14 78.40 39.20 9 99.90 39.20 40.18 100.00 97.00 80.00 100.00 40.18 98.00 49.00

47 Appendix 6. Data and Curve of Gallocatechin standard

GC

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-GC

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.08 2295 393 896 1344.9 150.1024 0.90 0.087500

2 0.39 ND ND ND ND ND ND ND ND

3 1.96 13472 9022 14117 12204 2774.2 22.73262 12.20 0.160607

4 3.92 117960 98942 99996 105633 10688.8 10.11882 105.63 0.037110 5 7.84 433241 428290 425265 428932 4026.6 0.93874 428.93 0.018278 6 15.68 889802 891797 886389 889329 2734.8 0.30751 889.33 0.017631 7 23.52 1361222 1361419 1354988 1359210 3657.4 0.26908 1359.21 0.017304 8 31.36 1811274 1870638 1809024 1830312 34941.5 1.90904 1830.31 0.017134 9 39.20 2131986 2127202 2292481 2183890 94073.3 4.30760 2183.89 0.017950

y = 57.622x - 43.399 R² = 0.9955

-1000.00 0.00 1000.00 2000.00 3000.00

0.00 10.00 20.00 30.00 40.00 50.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

GC

48 Appendix 7. Data and Curve of Epigallocatechin Standard

EGC

Level Conc Peak area (mV*sec) SD %RSD Peak area

RFE-EGC

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.08 12348 9901 580 7610 6209.6 81.60145 7.61 0.010560

2 0.40 ND ND ND ND ND ND ND ND

3 2.01 46516 45031 39105 43551 3921.0 9.00332 43.55 0.046130

4 4.02 60674 54821 51140 55545 4808.1 8.65615 55.55 0.072338

5 8.04 277513 272498 267033 272348 5241.6 1.92460 272.35 0.029506 6 16.07 846070 838482 838159 840904 4477.1 0.53241 840.90 0.019113 7 24.11 1363869 1366317 1361497 1363894 2410.1 0.17671 1363.89 0.017676 8 32.14 1818552 1878280 1818431 1838421 34519.0 1.87764 1838.42 0.017485 9 40.18 2150500 2153638 2333291 2212476 104640.3 4.72956 2212.48 0.018161

y = 58.038x - 82.110 R² = 0.994 -1000.00

0.00 1000.00 2000.00 3000.00

0.00 10.00 20.00 30.00 40.00 50.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

EGC

49 Appendix 8. Data and Curve of Catechin Standard

C

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-C

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.20 46661 45593 7427 33227 22349.8 67.26408 33.23 0.006019

2 1.00 4381 4718 3579 4226 585.1 13.84539 4.23 0.236630

3 5.00 258152 249477 231391 246340 13653.5 5.542547 246.34 0.020297 4 10.00 496033 462270 474490 477598 17094.7 3.579307 477.60 0.020938 5 20.00 871562 880836 873651 875350 4864.8 0.55575 875.35 0.022848 6 40.00 1613818 1616021 1613928 1614589 1241.4 0.076884 1614.59 0.024774 7 60.00 2425475 2430889 2429159 2428508 2765.1 0.113862 2428.51 0.024707 8 80.00 3225592 3355028 3222453 3267691 75652.3 2.315162 3267.69 0.024482 9 100.00 3805808 3815782 4067067 3896219 148042.7 3.799651 3896.22 0.025666

y = 39.359x + 44.271 R² = 0.999

0.00 1000.00 2000.00 3000.00 4000.00 5000.00

0.00 20.00 40.00 60.00 80.00 100.00 120.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

C

50 Appendix 9. Data and Curve of Epicatechin Standard

EC

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-EC

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.19 44738 43550 40904 43064 1962.7 4.557543 43.06 0.004505

2 0.97 ND ND ND ND ND ND ND ND

3 4.85 229877 219701 205325 218301 12335.7 5.650788 218.30 0.022217 4 9.70 483862 449854 458421 464046 17688.0 3.811684 464.05 0.020903 5 19.40 913945 916884 906668 912499 5259.3 0.576358 912.50 0.021260 6 38.80 1762054 1760126 1758253 1760144 1900.6 0.107978 1760.14 0.022044 7 58.20 2672613 2678775 2676645 2676011 3129.5 0.116948 2676.01 0.021749 8 77.60 3555755 3690704 3549852 3598770 79671.6 2.213856 3598.77 0.021563 9 97.00 4200623 4204674 4453436 4286244 144806.4 3.378398 4286.24 0.022631

y = 45.016x + 16.906 R² = 0.999 0.00

1000.00 2000.00 3000.00 4000.00 5000.00

0.00 20.00 40.00 60.00 80.00 100.00 120.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

EC

51 Appendix 10. Data and Curve of Epigallocatechin gallate Standard

EGCG

Level Conc Peak area (mV*sec) SD %RSD Peak area

RF-EGCG

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.16 35914 32970 22961.3 2081.7 9.066209 22.96 0.006968

2 0.80 ND ND ND ND ND ND ND ND

3 4.00 ND ND ND ND ND ND ND ND

4 8.00 36723 24152 20291.7 8889.0 43.80635 20.29 0.394251

5 16.00 602610 596321 573670 590867 15221.4 2.57611 590.87 0.027079 6 32.00 1795609 1791354 1785725 1790896 4957.9 0.276839 1790.90 0.017868 7 48.00 2896843 2893573 2895324 2895247 1636.4 0.056519 2895.25 0.016579 8 64.00 3884732 4016829 3894688 3932083 73560.8 1.870785 3932.08 0.016276 9 80.00 4627886 4646375 4833889 4702717 113974.1 2.42358 4702.72 0.017011

y = 62.623x - 209.555 R² = 0.992

-1000.00 0.00 1000.00 2000.00 3000.00 4000.00 5000.00 6000.00

0.00 20.00 40.00 60.00 80.00 100.00

Pe

ak

ar

e

a

(m

V*se

c)

Con. (ug/ml)

EGCG

52 Appendix 11. Data and Curve of Gallocatechine gallate Standard

GCG

Level Conc Peak area (mV*sec) SD %RSD _{Peak area RF-GCG}

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.08 ND ND ND ND ND ND ND ND

2 0.40 ND ND ND ND ND ND ND ND

3 2.01 163453 54484.3 #DIV/0! #DIV/0! 54.48 0.036873

4 4.02 56960 49114 49144 51739.3 4521.3 8.738526 51.74 0.077659 5 8.04 372415 375248 360921 369528 7587.3 2.053235 369.53 0.021747 6 16.07 823357 823338 819065 821920 2472.5 0.300823 821.92 0.019554 7 24.11 1284788 1285181 1296132 1288700 6439.0 0.499652 1288.70 0.018707 8 32.14 1729687 1789176 1728673 1749179 34642.4 1.980496 1749.18 0.018377 9 40.18 2073892 2078048 2270978 2140973 112607.1 5.259623 2140.97 0.018767

y = 54.638x - 66.134 R² = 0.9952

-500.00 0.00 500.00 1000.00 1500.00 2000.00 2500.00

0.00 10.00 20.00 30.00 40.00 50.00

Peak

ar

e

a (

m

V*

sec

)

con. (ug/ml)

GCG

53 Appendix 12. Data and Curve of Epicatechin gallate Standard

ECG

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-ECG

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.20 33351 34269 22540 649.1 2.879876 22.54 0.008696

2 0.98 ND ND ND ND ND ND ND ND

3 4.90 170443 163453 160687 164861 5028.1 3.049899 164.86 0.029722 4 9.80 386359 372909 377111 378793 6880.9 1.816546 378.79 0.025872 5 19.60 886511 887579 877589 883893 5485.5 0.620604 883.89 0.022175 6 39.20 1832457 1819321 1826645 1826141 6582.5 0.360459 1826.14 0.021466 7 58.80 2834437 2835000 2832846 2834094 1117.1 0.039418 2834.09 0.020747 8 78.40 3791078 3929398 3783514 3834663 82129.8 2.141772 3834.66 0.020445 9 98.00 4506252 4511335 4565129 4527572 32624.5 0.720573 4527.57 0.021645

y = 47.834x - 38.911 R² = 0.998

-1000.00 0.00 1000.00 2000.00 3000.00 4000.00 5000.00

0.00 20.00 40.00 60.00 80.00 100.00 120.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

ECG

54 Appendix 13. Data and Curve of Catechin Gallate Standard

CG

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-CG

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.10 8168 7645 9716 8510 1076.9 12.65556 8.51 0.011516

2 0.49 ND ND ND ND ND ND ND ND

3 2.45 65801 62792 58652 62415 3589.4 5.750829 62.42 0.039253 4 4.90 158481 151682 153876 154680 3470.0 2.243356 154.68 0.031678 5 9.80 390771 398559 379321 389550 9676.9 2.484124 389.55 0.025157 6 19.60 821299 812873 814387 816186 4491.9 0.550358 816.19 0.024014 7 29.40 1274066 1278920 1276134 1276373 2435.8 0.19084 1276.37 0.023034 8 39.20 1720236 1808215 1729822 1752758 48266.0 2.75372 1752.76 0.022365 9 49.00 2052642 2072100 2065152 2063298 9860.6 0.477905 2063.30 0.023748

y = 43.760x - 28.485 R² = 0.998

-500.00 0.00 500.00 1000.00 1500.00 2000.00 2500.00

0.00 10.00 20.00 30.00 40.00 50.00 60.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

CG

55 Appendix 14. Data and Curve of Caffeine Standard

CF

Level Conc Peak area (mV*sec) SD %RSD Peak area RF-CF

(µg/mL) 1 2 3 Mean (mV*sec)

1 0.20 35046 32729 22592 1638.4 7.252083 22.59 0.008853

2 1.00 8610 8833 8264 8569 286.7 3.345865 8.57 0.116700

3 5.00 182649 177241 167583 175824 7632.3 4.34084 175.82 0.028437 4 10.00 357352 332481 339993 343275 12756.3 3.716041 343.28 0.029131 5 20.00 662590 668568 653289 661482 7699.5 1.163975 661.48 0.030235 6 40.00 1284839 1284653 1283294 1284262 843.5 0.065676 1284.26 0.031146 7 60.00 1946767 1948628 1949767 1948387 1514.4 0.077726 1948.39 0.030795 8 80.00 2605219 2693547 2599419 2632728 52750.3 2.003636 2632.73 0.030387 9 100.00 3089850 3094222 3272598 3152223 104270.4 3.307838 3152.22 0.031724

y = 31.976x + 13.163 R² = 0.999

0.00 1000.00 2000.00 3000.00 4000.00

0.00 20.00 40.00 60.00 80.00 100.00 120.00

Peak

ar

e

a (

m

V*

sec

)

Con. (ug/ml)

CF

56 Appendix 15. Calculation of Total Polyphenols in Tea Powder

Tea ref Wt.sample %DM Extract DF Absorbance Linear eq. C (µg/ml) Total polyphenols (%w/w dry basis)

Powder (g) Volume(mL) 1 2 m b 1 2 1 2 Mean SD

3% 180C

1 2.0031 96.67 250 50 0.5846 0.5442 0.0114 0.0143 50.03 46.48 32.29 30.01

30.55 1.167 2 2.0032 96.67 250 50 0.5458 0.5408 0.0114 0.0143 46.62 46.18 30.09 29.81

3% 200C

1 2.0012 97.24 250 50 0.5045 0.4988 0.0114 0.0143 43.00 42.50 27.62 27.30

27.44 0.146 2 2.0008 97.24 250 50 0.5019 0.4994 0.0114 0.0143 42.77 42.55 27.48 27.34

3% 220C

1 2.0035 96.23 250 50 0.4978 0.4889 0.0114 0.0143 42.41 41.63 27.50 26.99

27.27 0.319 2 2.0008 96.23 250 50 0.4987 0.4883 0.0114 0.0143 42.49 41.58 27.59 26.99

6% 180C

1 2.0042 97.24 250 50 0.5627 0.5527 0.0114 0.0143 48.11 47.23 30.85 30.29

30.69 0.359 2 2.0026 97.24 250 50 0.5667 0.5563 0.0114 0.0143 48.46 47.54 31.10 30.52

6% 200C

1 2.0043 97.33 250 50 0.5556 0.5141 0.0114 0.0143 47.48 43.84 30.43 28.09

29.98 1.334 2 2.0038 97.33 250 50 0.5696 0.551 0.0114 0.0143 48.71 47.08 31.22 30.17

6% 220C

1 2.001 97.23 250 50 0.5434 0.5373 0.0114 0.0143 46.41 45.88 29.82 29.48

29.89 0.317 2 2.0006 97.23 250 50 0.5478 0.5499 0.0114 0.0143 46.80 46.98 30.07 30.19

9% 180C

1 2.0023 96.89 250 50 0.5616 0.5118 0.0114 0.0143 48.01 43.64 30.93 28.12

29.68 1.198 2 2.0045 96.89 250 50 0.549 0.5366 0.0114 0.0143 46.90 45.82 30.19 29.49

9% 200C

1 2.0057 97.67 250 50 0.5688 0.5576 0.0114 0.0143 48.64 47.66 31.04 30.41

30.34 0.508 2 2.0036 97.67 250 50 0.5491 0.549 0.0114 0.0143 46.91 46.90 29.97 29.96

9% 220C

1 2.0033 96.78 250 50 0.5314 0.5358 0.0114 0.0143 45.36 45.75 29.24 29.49

30.16 0.925 2 2.0044 96.78 250 50 0.5594 0.5643 0.0114 0.0143 47.82 48.25 30.81 31.09

57 Appendix 16. Calculation of Antioxidant Activity in Tea Powder

Tea Powder ref

Wt.

sample %DM

Extract

Vol DF A517 A 517 sample %Inhibition b m Trolox (mM) Trolox(µmol/100 g db)

(g) (ml) control 1 2 1 2 1 2 1 2 Mean SD %RSD

3% 180C

1 2.0031 96.67 250 50 0.6175 0.4026 0.3836 34.80 37.88 -3.8964 0.1122 344.90 372.33 222644 240347

226.389 27602 12.1923 2 2.0032 96.67 250 50 0.6175 0.4382 0.3699 29.04 40.10 -3.8964 0.1122 293.52 392.10 189466 253099

3% 200C

1 2.0012 97.24 250 50 0.6175 0.4105 0.3859 33.52 37.51 -3.8964 0.1122 333.50 369.01 214225 237033

221.154 11548 5.2217 2 2.0008 97.24 250 50 0.6175 0.4138 0.402 32.99 34.90 -3.8964 0.1122 328.74 345.77 211208 222150

3% 220C

1 2.0035 96.23 250 50 0.6175 0.4072 0.4068 34.06 34.12 -3.8964 0.1122 338.26 338.84 219313 219687

218.805 1119 0.5116 2 2.0008 96.23 250 50 0.6175 0.4098 0.4078 33.64 33.96 -3.8964 0.1122 334.51 337.40 217173 219047

6% 180C

1 2.0042 97.24 250 50 0.6175 0.376 0.3632 39.11 41.18 -3.8964 0.1122 383.30 401.77 245843 257692

247.768 7356 2.9690 2 2.0026 97.24 250 50 0.6175 0.3744 0.3825 39.37 38.06 -3.8964 0.1122 385.60 373.91 247521 240017

6% 200C

1 2.0043 97.33 250 50 0.6175 0.3823 0.3917 38.09 36.57 -3.8964 0.1122 374.20 360.63 239777 231083

235.621 6466 2.7443 2 2.0038 97.33 250 50 0.6175 0.3795 0.3938 38.54 36.23 -3.8964 0.1122 378.24 357.60 242427 229198

6% 220C

1 2.001 97.23 250 50 0.6175 0.3885 0.3995 37.09 35.30 -3.8964 0.1122 365.25 349.38 234670 224469

232.537 6204 2.6681 2 2.0006 97.23 250 50 0.6175 0.3917 0.3836 36.57 37.88 -3.8964 0.1122 360.63 372.33 231748 239261

9% 180C

1 2.0023 96.89 250 50 0.6175 0.3877 0.3675 37.21 40.49 -3.8964 0.1122 366.41 395.56 236084 254870

241.673 9055 3.7470 2 2.0045 96.89 250 50 0.6175 0.3829 0.3881 37.99 37.15 -3.8964 0.1122 373.34 365.83 240284 235453

9% 200C

1 2.0057 97.67 250 50 0.6175 0.3898 0.3634 36.87 41.15 -3.8964 0.1122 363.38 401.48 231868 256182

247.633 11494 4.6415 2 2.0036 97.67 250 50 0.6175 0.3637 0.3744 41.10 39.37 -3.8964 0.1122 401.05 385.60 256174 246309

9% 220C

1 2.0033 96.78 250 50 0.6175 0.4149 0.3697 32.81 40.13 -3.8964 0.1122 327.15 392.39 210923 252985

243.632 23154 9.5038 2 2.0044 96.78 250 50 0.6175 0.3569 0.3772 42.20 38.91 -3.8964 0.1122 410.86 381.56 264751 245870

58 Appendix 17. Chromatogram of polyphenols in dried tea analyzed by HPLC-UV

59 Appendix 18. Calculation of caffeine (CF) and catechin content in dried tea

Rep 1

Sample weight

(g) REP %DM

Final Vol

(mL) DF Rf-i RF-CF

RF-

i/RF-CF

std CF Peak area (mV*sec) Amount(g/100 g db)

Analysis

slope y-intercept 1 2 3 Mean 1 2 3 Mean

2.0062 1 93.95 250 10 0.017659 0.03027 0.58349 31976 13163 284871 292785 297599 291752 0.66 0.68 0.69 0.67 GC 2.0062 1 93.95 250 10 0.018108 0.03027 0.59833 31976 13163 1357782 1375680 1367193 1366885 3.34 3.38 3.36 3.36 EGC 2.0062 1 93.95 250 10 0.023387 0.03027 0.77275 31976 13163 221857 239760 240574 234064 0.67 0.73 0.73 0.71 C 2.0062 1 93.95 250 10 0.021767 0.03027 0.71920 31976 13163 272887 301966 293836 289563 0.77 0.86 0.84 0.82 EC 2.0062 1 93.95 250 10 0.016934 0.03027 0.55951 31976 13163 1938360 1963071 1954490 1951974 4.47 4.53 4.51 4.50 EGCG 2.0062 1 93.95 250 10 0.030265 0.03027 1.00000 31976 13163 608225 666993 655423 643547 2.47 2.71 2.66 2.61 CF 2.0062 1 93.95 250 10 0.019430 0.03027 0.64201 31976 13163 135570 194958 168760 166429 0.33 0.48 0.41 0.41 GCG 2.0062 1 93.95 250 10 0.022058 0.03027 0.72884 31976 13163 238931 263842 240496 247756 0.68 0.76 0.69 0.71 ECG

2.0062 1 93.95 250 10 0.023664 0.03027 0.78188 31976 13163 ND ND ND ND ND ND ND ND CG

Rep 2

Sample weight

(g) REP %DM

Final Vol

(mL) DF Rf-i RF-CF

RF-

i/RF-CF

std CF Peak area (mV*sec) Amount(g/100 g db)

Analysis

slope y-intercept 1 2 3 Mean 1 2 3 Mean

2.0052 2 93.95 250 10 0.017659 0.03027 0.58349 31976 13163 372505 373142 375653 373767 0.87 0.87 0.88 0.87 GC 2.0052 2 93.95 250 10 0.018108 0.03027 0.59833 31976 13163 1600648 1601543 1609840 1604010 3.94 3.94 3.96 3.95 EGC 2.0052 2 93.95 250 10 0.023387 0.03027 0.77275 31976 13163 271846 266352 267316 268505 0.83 0.81 0.82 0.82 C 2.0052 2 93.95 250 10 0.021767 0.03027 0.71920 31976 13163 332979 333864 333816 333553 0.95 0.96 0.96 0.96 EC 2.0052 2 93.95 250 10 0.016934 0.03027 0.55951 31976 13163 2138116 2138777 2137503 2138132 4.93 4.94 4.93 4.93 EGCG 2.0052 2 93.95 250 10 0.030265 0.03027 1.00000 31976 13163 711940 716903 727767 718870 2.90 2.92 2.97 2.93 CF 2.0052 2 93.95 250 10 0.019430 0.03027 0.64201 31976 13163 230921 243071 250220 241404 0.58 0.61 0.63 0.61 GCG 2.0052 2 93.95 250 10 0.022058 0.03027 0.72884 31976 13163 248583 257375 273903 259954 0.71 0.74 0.79 0.75 ECG

60 Appendix 19. Calculation of caffeine (CF) and catechin content in extract tea, concentrated tea 3.6.9% of total solid

Extract

Sample weight

(g) REP

Final Vol

(mL) DF Rf-i RF-CF

RF-i/RF-CF

std CF Peak area (mV*sec) Con. (µg/ml)

Analysis

Slope y-intercept 1 2 Mean 1 2 Mean

3000 1 46000 50 0.017659 0.03027 0.58349 31976 13163 724746 716423 720585 12.98 12.83 12.91 GC 3000 1 46000 50 0.018108 0.03027 0.59833 31976 13163 1813726 1805731 1809729 33.69 33.54 33.62 EGC 3000 1 46000 50 0.023387 0.03027 0.77275 31976 13163 272260 263175 267718 6.26 6.04 6.15 C 3000 1 46000 50 0.021767 0.03027 0.71920 31976 13163 393395 386292 389844 8.55 8.39 8.47 EC 3000 1 46000 50 0.016934 0.03027 0.55951 31976 13163 2288173 2268018 2278096 39.81 39.46 39.63 EGCG 3000 1 46000 50 0.030265 0.03027 1.00000 31976 13163 884386 882134 883260 27.25 27.18 27.21 Caffeine 3000 1 46000 50 0.019430 0.03027 0.64201 31976 13163 493896 516364 505130 9.65 10.10 9.88 GCG 3000 1 46000 50 0.022058 0.03027 0.72884 31976 13163 276527 289784 283156 6.00 6.31 6.15 ECG

Total Solid Concentration 3%

in Feed

Sample weight

(g) REP

Final Vol

(mL) DF Rf-i RF-CF

RF-i/RF-CF

std CF Peak area (mV*sec) Con. (µg/ml)

Analysis

Slope y-intercept 1 2 Mean 1 2 Mean

3000 1 33200 50 0.017659 0.03027 0.58349 31976 13163 988231 982845 985538 17.79 17.69 17.74 GC 3000 1 33200 50 0.018108 0.03027 0.59833 31976 13163 2484161 2476208 2480185 46.24 46.09 46.16 EGC 3000 1 33200 50 0.023387 0.03027 0.77275 31976 13163 450784 449511 450148 10.58 10.55 10.56 C 3000 1 33200 50 0.021767 0.03027 0.71920 31976 13163 526930 527300 527115 11.56 11.56 11.56 EC 3000 1 33200 50 0.016934 0.03027 0.55951 31976 13163 2155309 2147143 2151226 37.48 37.34 37.41 EGCG 3000 1 33200 50 0.030265 0.03027 1.00000 31976 13163 1082207 1082189 1082198 33.43 33.43 33.43 CF 3000 1 33200 50 0.019430 0.03027 0.64201 31976 13163 538571 550328 544450 10.55 10.79 10.67 GCG 3000 1 33200 50 0.022058 0.03027 0.72884 31976 13163 250189 245755 247972 5.40 5.30 5.35 ECG

61 Total Solid Concentration 6% in Feed

Sample weight

(g) REP

Final Vol

(mL) DF Rf-i RF-CF

RF-

i/RF-CF

std CF Peak area (mV*sec) Con. (µg/ml)

Analysis

slope y-intercept 1 2 Mean 1 2 Mean

3000 1 12500 100 0.017659 0.03027 0.58349 31976 13163 1109689 1121969 1115829 20.01 20.23 20.12 GC 3000 1 12500 100 0.018108 0.03027 0.59833 31976 13163 2387101 2409768 2398435 44.42 44.84 44.63 EGC 3000 1 12500 100 0.023387 0.03027 0.77275 31976 13163 414537 413555 414046 9.70 9.68 9.69 C 3000 1 12500 100 0.021767 0.03027 0.71920 31976 13163 533424 543292 538358 11.70 11.92 11.81 EC 3000 1 12500 100 0.016934 0.03027 0.55951 31976 13163 2035480 2048974 2042227 35.39 35.62 35.50 EGCG 3000 1 12500 100 0.030265 0.03027 1.00000 31976 13163 1052792 1072202 1062497 32.51 33.12 32.82 CF 3000 1 12500 100 0.019430 0.03027 0.64201 31976 13163 570885 580379 575632 11.20 11.39 11.29 GCG 3000 1 12500 100 0.022058 0.03027 0.72884 31976 13163 236771 237443 237107 5.10 5.11 5.10 ECG

Total Solid Concentration 9% in Feed Sample

weight

(g) REP

Final Vol

(mL) DF Rf-i RF-CF

RF-

i/RF-CF

std CF Peak area (mV*sec) Con. (µg/ml)

Analysis

slope y-intercept 1 2 Mean 1 2 Mean

3000 1 7500 175 0.017659 0.03027 0.58349 31976 13163 737299 712478 724889 13.21 12.76 12.99 GC 3000 1 7500 175 0.018108 0.03027 0.59833 31976 13163 1871115 1850280 1860698 34.77 34.38 34.57 EGC 3000 1 7500 175 0.023387 0.03027 0.77275 31976 13163 266980 256880 261930 6.13 5.89 6.01 C 3000 1 7500 175 0.021767 0.03027 0.71920 31976 13163 394101 374581 384341 8.57 8.13 8.35 EC 3000 1 7500 175 0.016934 0.03027 0.55951 31976 13163 2061450 2013713 2037582 35.84 35.01 35.42 EGCG 3000 1 7500 175 0.030265 0.03027 1.00000 31976 13163 854981 789738 822360 26.33 24.29 25.31 CF 3000 1 7500 175 0.019430 0.03027 0.64201 31976 13163 457776 422651 440214 8.93 8.22 8.57 GCG 3000 1 7500 175 0.022058 0.03027 0.72884 31976 13163 248191 258250 253221 5.36 5.59 5.47 ECG

62 Appendix 20. Calculation of caffeine (CF) and catechin content in green tea powder 3% solid concentration in feed and inlet air temp. 220˚C

Powder 3% solid

220C

Sample weight

(g) REP %DM

Final Vol

(mL) DF Rf-i RF-CF

RF-i/RF-CF

std CF Peak area (mV*sec) Amount(g/100 g db)

Analysis

slope y-intercept 1 2 Mean 1 2 Mean

2.0035 1 96.23 250 15 0.017659 0.03027 0.58349 31976 13163 810066 807415 808741 2.83 2.82

2.99 GC

2.0008 2 96.23 250 15 0.017659 0.03027 0.58349 31976 13163 910884 886293 898589 3.19 3.10 2.0035 1 96.23 250 15 0.018108 0.03027 0.59833 31976 13163 1891281 1887849 1889565 6.84 6.82

7.37 EGC

2.0008 2 96.23 250 15 0.018108 0.03027 0.59833 31976 13163 2200945 2165960 2183453 7.97 7.85 2.0035 1 96.23 250 15 0.023387 0.03027 0.77275 31976 13163 293857 265655 279756 1.32 1.19

1.34 C

2.0008 2 96.23 250 15 0.023387 0.03027 0.77275 31976 13163 338476 294514 316495 1.53 1.32 2.0035 1 96.23 250 15 0.021767 0.03027 0.71920 31976 13163 413102 390454 401778 1.75 1.65

1.83 EC

2.0008 2 96.23 250 15 0.021767 0.03027 0.71920 31976 13163 483199 431462 457331 2.06 1.83 2.0035 1 96.23 250 15 0.016934 0.03027 0.55951 31976 13163 1941451 1902778 1922115 6.56 6.43

7.02 EGCG

2.0008 2 96.23 250 15 0.016934 0.03027 0.55951 31976 13163 2259771 2182904 2221338 7.66 7.39 2.0035 1 96.23 250 15 0.030265 0.03027 1.00000 31976 13163 915351 852677 884014 5.49 5.11

5.64 CF

2.0008 2 96.23 250 15 0.030265 0.03027 1.00000 31976 13163 1028135 959656 993896 6.18 5.77 2.0035 1 96.23 250 15 0.019430 0.03027 0.64201 31976 13163 417699 383604 400652 1.58 1.45

1.64 GCG

2.0008 2 96.23 250 15 0.019430 0.03027 0.64201 31976 13163 502914 425621 464268 1.92 1.61 2.0035 1 96.23 250 15 0.022058 0.03027 0.72884 31976 13163 232834 243061 237948 0.97 1.02

1.06 ECG

63 Appendix 21. SAS output

The SAS System 10:07 Wednesday. November 29. 2000 1 corr_Sari

The CORR Procedure

9 Variables: GC EGC C EC EGCG CF GCG ECG Trolox

Simple Statistics

Variable N Mean Std Dev Sum Minimum Maximum GC 18 2.84500 0.19196 51.21000 2.49000 3.15000 EGC 18 6.74000 0.66102 121.32000 5.77000 8.53000 C 18 1.44722 0.14442 26.05000 1.21000 1.64000 EC 18 1.85556 0.27350 33.40000 1.60000 2.85000 EGCG 18 6.03722 0.85724 108.67000 4.09000 7.53000 CF 18 5.28833 0.35705 95.19000 4.59000 5.97000 GCG 18 1.54167 0.11952 27.75000 1.33000 1.76000 ECG 18 0.95944 0.14098 17.27000 0.63000 1.12000 Trolox 18 235024 11939 4230425 216679 255311

Pearson Correlation Coefficients. N = 18 Prob > |r| under H0: Rho=0

GC EGC C EC EGCG CF GCG ECG Trolox GC 1.00000 -0.13351 0.57534 0.37545 -0.12170 0.43662 0.23421 0.13900 0.11001 0.5974 0.0125 0.1247 0.6305 0.0700 0.3496 0.5823 0.6639 EGC -0.13351 1.00000 -0.02335 -0.02557 0.34124 0.01794 0.12560 -0.08755 -0.17041 0.5974 0.9267 0.9198 0.1658 0.9437 0.6195 0.7298 0.4990 C 0.57534 -0.02335 1.00000 0.60476 -0.08806 0.34488 -0.12785 0.14842 0.55958 0.0125 0.9267 0.0078 0.7282 0.1610 0.6132 0.5567 0.0157 EC 0.37545 -0.02557 0.60476 1.00000 -0.00929 0.09889 -0.34490 0.21732 0.46615 0.1247 0.9198 0.0078 0.9708 0.6962 0.1610 0.3864 0.0512 EGCG -0.12170 0.34124 -0.08806 -0.00929 1.00000 0.68895 0.59501 0.86246 -0.23031 0.6305 0.1658 0.7282 0.9708 0.0016 0.0092 <.0001 0.3579 CF 0.43662 0.01794 0.34488 0.09889 0.68895 1.00000 0.70498 0.80279 -0.20416 0.0700 0.9437 0.1610 0.6962 0.0016 0.0011 <.0001 0.4164 GCG 0.23421 0.12560 -0.12785 -0.34490 0.59501 0.70498 1.00000 0.52230 -0.29023 0.3496 0.6195 0.6132 0.1610 0.0092 0.0011 0.0262 0.2427 ECG 0.13900 -0.08755 0.14842 0.21732 0.86246 0.80279 0.52230 1.00000 -0.06356 0.5823 0.7298 0.5567 0.3864 <.0001 <.0001 0.0262 0.8022

64 Appendix 22. Duncan’s test results for physical properties in green tea powders

22.1 Bulk density

Trt N

Subset

1 2 3 4 5 6

9%, 220C 3 .393300

6%, 220C 3 .397167

6%, 200C 3 .400033

6%, 180C 3 .406867

3%, 220C 3 .426167

3%, 200C 3 .427800

3%, 180C 3 .451100

9%, 200C 3 .452200

9%, 180C 3 .501400

Sig. 1.000 .081 1.000 .306 .487 1.000

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = 3,61E-006.

22.2 L value

trt N

Subset

1 2 3 4 5 6 7

6%, 180C 3 68.0733

9%, 180C 3 70.3767

3%, 200C 3 70.8933

3%, 220C 3 71.1367

3%, 180C 3 71.9533

6%, 200C 3 72.4167

6%, 220C 3 73.0467

9%, 220C 3 73.8067

9%, 200C 3 74.4100

Sig. 1.000 1.000 .327 .071 1.000 1.000 1.000

Means for groups in homogeneous subsets are displayed. Based on observed means.

65 22. 3 a value

trt N

Subset

1 2 3 4 5 6

3%, 180C 3 3.5033

3%, 220C 3 3.8633

6%, 220C 3 4.1333

6%, 200C 3 4.1367

3%, 200C 3 4.1500

9%, 220C 3 4.8733

6%, 180C 3 4.9100

9%, 200C 3 5.4233

9%, 180C 3 5.7933

Sig. 1.000 1.000 .810 .577 1.000 1.000

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,006. 22. 4 b value

trt N

Subset

1 2 3 4 5

3%, 180C 3 30.0767

6%, 220C 3 30.6467 30.6467

6%, 200C 3 31.1967

3%, 220C 3 31.9733

3%, 200C 3 33.5633

6%, 180C 3 34.0500

9%, 220C 3 34.3100

9%, 200C 3 37.3133

9%, 180C 3 37.3733

Sig. .126 .138 1.000 .060 .868

Means for groups in homogeneous subsets are displayed. Based on observed means.

66 22. 5 Solubility

trt N

Subset

1 2 3 4

6%, 200C 2 75.5550

6%, 220C 2 75.5550

6%, 180C 2 77.6500 77.6500

3%, 200C 2 78.6350

3%, 180C 2 79.6700

3%, 220C 2 80.0300

9%, 200C 2 87.9600

9%, 180C 2 89.5400 89.5400

9%, 220C 2 91.1700

Sig. .098 .071 .180 .168

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = 1,184.

22. 6 Hygroscopicity

trt N

Subset

1 2 3 4 5

3%, 220C 3 8.8367

6%, 220C 3 10.8700

9%, 200C 3 12.3733

9%, 220C 3 12.5200

6%, 200C 3 12.6900

3%, 200C 3 15.7433

6%, 180C 3 15.9433

9%, 180C 3 16.5667 16.5667

3%, 180C 3 17.8333

Sig. 1.000 1.000 .633 .221 .054

Means for groups in homogeneous subsets are displayed. Based on observed means.

67 23. Duncan’s test results for chemical properties in green tea powders

23. 1 Moisture content

trt N

Subset

1 2 3 4

9%, 200C 3 2.3267

6%, 200C 3 2.6733

3%, 200C 3 2.7600

6%, 180C 3 2.7633

6%, 220C 3 2.7700

9%, 180C 3 3.1133

9%, 220C 3 3.2233

3%, 180C 3 3.3333

3%, 220C 3 3.7700

Sig. 1.000 .402 .057 1.000

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,016.

23. 2 Total Polypenols

trt N

Subset

1 2

3%, 220C 2 27.2650

3%, 200C 2 27.4350

9%, 180C 2 29.6850

6%, 220C 2 29.8900

6%, 200C 2 29.9800

9%, 220C 2 30.1600

9%, 200C 2 30.3400

3%, 180C 2 30.5500

6%, 180C 2 30.6900

Sig. .791 .172

Means for groups in homogeneous subsets are displayed.

Based on observed means.

68 23. 3 Antioxidant Activity

trt N

Subset

1 2 3

3%, 220C 2 2.1880E5

3%, 200C 2 2.2115E5

3%, 180C 2 2.2639E5 2.2639E5

6%, 220C 2 2.3254E5 2.3254E5 2.3254E5 6%, 200C 2 2.3562E5 2.3562E5 2.3562E5

9%, 180C 2 2.4167E5 2.4167E5

9%, 220C 2 2.4363E5 2.4363E5

9%, 200C 2 2.4763E5

6%, 180C 2 2.4777E5

Sig. .061 .055 .086

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = 52289566,056. 23. 4 Catechins

trt N

Subset

1 2 3 4

6%, 200C 2 19.2750

6%, 220C 2 20.4250 20.4250

9%, 220C 2 20.5950 20.5950 20.5950 6%, 180C 2 20.6900 20.6900 20.6900

3%, 200C 2 21.1400 21.1400 21.1400 21.1400 3%, 180C 2 21.7700 21.7700 21.7700 21.7700

9%, 180C 2 22.2350 22.2350 22.2350

9%, 200C 2 22.9700 22.9700

3%, 220C 2 23.2250

Sig. .052 .136 .061 .091

Means for groups in homogeneous subsets are displayed. Based on observed means.

69 23. 5 Caffeine

caffeine

Duncan

trt N

Subset 1

6%, 180C 2 4.9600

6%, 200C 2 5.0200

3%, 200C 2 5.0900

9%, 180C 2 5.1600

6%, 220C 2 5.3650

9%, 220C 2 5.3650

3%, 180C 2 5.3700

9%, 200C 2 5.6300

3%, 220C 2 5.6350

Sig. .123

Means for groups in homogeneous subsets are displayed.

Based on observed means.

The error term is Mean Square(Error) = ,132.

70 24. Duncan’s test results for single catechins in green tea powders

24. 1 Gallocatechin (GC)

trt N

Subset

1 2 3 4

3%, 200C 2 2.5350

3%, 180C 2 2.6950 2.6950

9%, 200C 2 2.7450 2.7450 2.7450

6%, 180C 2 2.8200 2.8200 2.8200 2.8200

6%, 200C 2 2.8200 2.8200 2.8200 2.8200

9%, 180C 2 2.8650 2.8650 2.8650

3%, 220C 2 2.9850 2.9850

9%, 220C 2 3.0550

6%, 220C 2 3.0850

Sig. .051 .211 .091 .068

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,014. 24. 2 Epigallocatechin (EGC)

trt N

Subset

1 2

9%, 220C 2 5.8600

6%, 220C 2 6.1650 6.1650

6%, 200C 2 6.4700 6.4700

3%, 200C 2 6.6700 6.6700

6%, 180C 2 6.6750 6.6750

3%, 180C 2 6.8850 6.8850

9%, 200C 2 7.0350 7.0350

3%, 220C 2 7.3700

9%, 180C 2 7.5300

Sig. .087 .054

Means for groups in homogeneous subsets are displayed.

Based on observed means.

71 24. 3 Catechin (C)

trt N

Subset

1 2 3 4

3%, 200C 2 1.2450

3%, 180C 2 1.3200 1.3200

3%, 220C 2 1.3400 1.3400

6%, 180C 2 1.3950 1.3950

6%, 200C 2 1.4250 1.4250 1.4250

6%, 220C 2 1.4800 1.4800 1.4800

9%, 200C 2 1.5900 1.5900

9%, 180C 2 1.5900 1.5900

9%, 220C 2 1.6400

Sig. .059 .086 .075 .083

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,006. 24. 4 Epicatechin (EC)

trt N

Subset

1 2

3%, 200C 2 1.6550

6%, 220C 2 1.7300

6%, 180C 2 1.7400

6%, 200C 2 1.7500

3%, 180C 2 1.7650

3%, 220C 2 1.8250 1.8250

9%, 200C 2 1.8700 1.8700

9%, 180C 2 1.9900 1.9900

9%, 220C 2 2.3750

Sig. .229 .060

Means for groups in homogeneous subsets are displayed.

Based on observed means.

72 24. 5 Epigallocatechin gallate (EGCG)

trt N

Subset

1 2 3

6%, 200C 2 4.6150

6%, 220C 2 5.4250 5.4250

6%, 180C 2 5.6150 5.6150

9%, 220C 2 5.7100 5.7100

9%, 180C 2 5.8900 5.8900

3%, 180C 2 6.4900 6.4900

3%, 200C 2 6.5200 6.5200

3%, 220C 2 7.0150

9%, 200C 2 7.0550

Sig. .069 .075 .059

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,247. 24. 6 Gallocatechin gallate

trt N

Subset 1

9%, 220C 2 1.4100

6%, 200C 2 1.4500

9%, 180C 2 1.4600

3%, 200C 2 1.5300

9%, 200C 2 1.5750

6%, 180C 2 1.6000

3%, 180C 2 1.6050

6%, 220C 2 1.6100

3%, 220C 2 1.6350

Sig. .126

Means for groups in homogeneous subsets are displayed.

Based on observed means.

The error term is Mean Square(Error) = ,015.

73 24. 7 Epicatechin gallate

trt N

Subset

1 2

6%, 200C 2 .7350

6%, 180C 2 .8550 .8550

9%, 180C 2 .9100 .9100

6%, 220C 2 .9250 .9250

3%, 200C 2 .9850 .9850

3%, 180C 2 1.0150 1.0150

9%, 220C 2 1.0500

3%, 220C 2 1.0600

9%, 200C 2 1.1000

Sig. .058 .090

Means for groups in homogeneous subsets are displayed.

Based on observed means.

1

I. INTRODUCTION

A.

BACKGROUND

Tea is globally one of the most popular and lowest cost beverages, next only to water. Tea is consumed by a wide range of age groups in all levels of society. The tea plant (Camellia sinensis) has been widely used for over 5000 years for its specific aroma, taste, and putative positive physiological functions. According to statistics from the Food and Agricultural Organization (FAO) of United Nations 2008, production and consumption of tea are steadily increasing. The worldwide production of tea in 2006 reached up to 3.60 million ton and the worldwide consumption reached up to 3.64 million ton. Over past decade, world tea consumption has increased by 2.7% annually. The main tea-producing countries are China, India, Sri Lanka, Kenya, Turkey, Indonesia, and Vietnam, which accounted for 28.73, 25.93, 8.60, 8.59, 5.49, 5.15, and 3.65%, respectively, of the 2006 output of total global tea production (Hicks, 2008).

Freshly harvested tea leaves are processed differently to produce specific types of tea such as green, oolong, and black tea. Of all the tea consumed in the world, 78% is black tea, 20% is green tea, and 2% is oolong tea. The green tea consumption in Indonesia was 3.13 thousand tons in 2005, while black tea consumption was more than green tea consumption, 67.9 thousand tons in 2005. FAO projected that world green tea production would grow at a faster rate than black tea by 2.0% annually, to reach 1097.7 thousand tons by 2016 (Ho et al, 2005). Green tea is heated and dried to avoid enzymatic oxidation. Green tea contains polyphenols, and most of the green tea polyphenols (GTPs) are flavonols, commonly known as catechins. Tea polyphenols have been known for their antioxidant activity and antimutagenic and anticarcinogenic properties (Yang et al 2007).

Traditionally, tea is prepared from its dried young leaves and leaf buds, made into a beverage by steeping the leaves in boiling water. But today, tea powder is being developed because it has many advantages such as more practical, simple transport economics, and simply

to prolong product’s shelf-life. Tea powder could be applied as functional food and as non food

product, like handbody, shampoo, and toothpaste. Food products being developed are tea-rice, tea-noodles, tea-cake, tea-biscuits, tea-wine, tea-candy, tea-ice cream (Hicks 1998). There are several method for produce tea powder, one of them is spray drying method.

Spray drying is one-step continuous processing operation that can transform feed from a fluid state into a dried form by spraying the feed into a hot drying medium (Okos et al, 2007). A short processing time, usually between three and thirty seconds and controlled operational conditions make the spray drying as an effective and unique method for various products, especially heat sensitive products and its retaining the high quality properties such as color, flavor, and nutrients.

The quality of a food powder is judged by the amount of physical and chemical degradation occuring during the dehydration process. There are many researchs were did by researchers to know the effect of spray drying on powder characteristic. At this research, different of feed concentrations and spray dryer inlet air temperatures were used to evaluate its effects on physicochemical properties of the spray-dried green tea extract. This information

2 however is necessary to establish processing conditions to produce value-added powder green tea as there is an increasing demand for herbal tea products in the market.

B.

OBJECTIVES

The objectives of this research were to investigate the effect of total solid concentration in feed and inlet air temperatures on physical and chemical properties of green tea powder which was produced by spray dryer.

3

II.

LITERATURE REVIEW

A.

TEA

Tea, one of the most popular beverages consumed worldwide, is a processed product from the leaves of tea plant (Camellia sinensis). The taxonomy of tea is shown in Table 1 and the figure of tea plant shown in Figure 1.

Table 1. The classify the taxonomy of tea

Common name: Tea

Kingdom: Plantae

Division: Spermatophyta

Subdivision: Angiospermae

Class: Dicolyledone

Ordo: Guttiferales

Family: Theaceae

Genus: Camellia

Species: Camellia sinensis

The worldwide production of tea in 2006 reached up to 3.60 million ton and the worldwide consumption reached up to 3.64 million ton. Over past decade, world tea consumption has increased by 2.7% annually. Tea Production of Indonesia in 2006 reached up to 187.9 thousand of tonnes. (Hicks, 2008). Indonesia, a country with more than 222 million people, produces more than 150,000 tons of tea per year, exporting 80% of it, with the balance consumed by domestic people. The large population provides a ready workforce, as well as a promising market for tea consumption.

Tea products are usually classified as white tea, green tea, oolong tea, and black tea, categorized by manufacturing process as shown in Figure 2.

4 Tea is consumed in different parts of the world as white, green, black, or oolong tea. White and green tea are known as unfermented tea. The polyphenol oxidase enzyme of green tea is inactivated by steaming. Oolong tea is produced by withering and half fermenting the leaves.

Thus oolong tea is called “semi-fermented tea”. Black tea is known as fermented tea because the

leaves are fermented, allowing enzymic oxidation of the polyphenols. Processing tea differently results in variation of chemical component in tea (Hara, 2000). The chemical component of tea are presented in Table 2.

Table 2. Composition (%) of green tea, black tea, infusion

Compound Green Tea* Black Tea* Infusion*

Protein 15 15 Trace

Amino Acids 4 4 3.5

Fiber 26 26 0

Other carbohydrates 7 7 4

Lipids 7 7 Trace

Pigments 2 2 Trace

Mineral 5 5 4.5

Phenolic compounds 30 5 4.5

Oxidixed phenolic compounds 0 25 4.5

*Data refer to dry weight of tea leaves (Chako et al, 2010) Fresh leaves

Withering

Drying

(A) (B)

Fermenting Rolling by tea roller, rotor vane

or CTC Fresh leaves

Withering

Drying Fresh leaves

Solar withering

Pan firing Indoor withering

and rolling

Rolling Mass breaking

Drying Fresh leaves

Rolling Primary

drying-rolling Steaming

Secondary drying-rolling

Final drying-rolling

Drying

(C) (D)

Figure 2. The manufacturing process of tea: (A) white tea, (B) green tea, (C) oolong tea, and (D) black tea (Hara, 2000)

5 In process of green tea production, tea leaves are steamed immediately after harvesting and the enzymes are inactivated at the initial stage. Therefore, the composition of green tea is simple and similar to that in the fresh tea leaves. Green tea contains polyphenols, which include flavanols, flavandiols, flavonoids, and phenolic acids; these compounds may account for up to 30% of the dry weight. Most of the green tea polyphenols (GTPs) are flavonols, commonly known as catechins accounting for up to 30% of the dry weight of the leaves,. which are composed of eight kinds of catechins and their derivatives slightly deviates depending on the species of tea plant and the season of harvesting.

There are eight major catechins in green tea: (+)-catechin (C), epicatechin (EC), (-)-gallocatechin (GC), (-)-epi(-)-gallocatechin (EGC), (-)-catechin gallate (CG), (-)-(-)-gallocatechin gallate (GCG), (-)-epicatechin gallate (ECG), and (-)-epigallocatechin gallate (EGCG). The major Epigallocatechin gallate (EGCG) is the major component of the polyphenolic fraction of green tea, it makes up about 10-50% of total green tea catechins. EGCG is also most potent antioxidant of polyphenol type of tea, is at least 100 times more effective than vitamin C and 25 times more effective than vitamin E. The antioxidant activity increase in the following order: EC<ECG<EGC<EGCG (Meterc et al, 2007). The percentage of major polyphenols in tea are shown in Table 3.

Table 3. The percentage of major polyphenols in tea

Compound Green Tea Oolong Tea Black Tea

EC 0.74 – 1.00 0.21 – 0.33 –

ECG 1.67 – 2.47 0.99 – 1.66 0.29 – 0.42

EGC 2.60 – 3.36 0.92 – 1.08 –

EGCG 7.00 – 7.53 2.93 – 3.75 0.39 – 0.60

(Yamanishi, 1995)

Caffeine (1,3,7-trimetylxantine, C8H10N4O2) is a plant alkaloid, one of the few plant products which the general public is readily familiar because of its occurence in beverages such as coffee and tea, as well as various soft drinks. Caffeine extract from tea is added to some pain-relief medicines. Caffeine compound is well known for its stimulant effect and is present at 2-4% of dried tea leaf weight, depending on the types and quality of teas (Yoshida et al, 1999).

Studies using animal models show that green tea catechins provide some protection against degenerative diseases. Green tea catechins could also act as antitumorigenic agents (Roomi et al, 2007) and as immune modulators in immunodysfunction caused by transplanted tumors or by carcinogen treatment. Green tea consumption has also been linked to the prevention of many types of cancer, including lung colon, esophagus, mouth, stomach, small intestine, kidney, pancreas, and mammary glands (Koo, 2004). This beneficial effect has been attributed to the presence of high amounts of polyphenols, which are potent antioxidants. In particular, green tea may lower blood pressure and thus reduce the risk of stroke and coronary heart disease. Some animal’s studies suggested that green tea might protect against the development of coronary heart disease by reducing blood glucose levels and body weight (Tsuneki et al, 2004).

6

Figure 3. Structures of the major catechin and caffeine in tea (Zuo et al, 2002)

The stability of a functional ingredient is fundamental to elaborate a nutraceutical product ecause changes in the ingredient may affect its nutritional value (e.g. antioxidant capacity, composition, and bioavailability). The stability of the grape seed extract (GSE) was evaluated based on changes in their main individual phenolic compounds, as well as changes in their antioxidant activity and browning. pH affects the stability of polyphenolic compounds and that a between 4 and 5 confers more stability to catechins and their isomers and polymers than more alkaline or acidic values(Tabart, 2009). The concentration of catechins was more stable than the concentration of the rest of compounds. According Pardo et al 2011, the catechins and antioxidant activity in grape seed extract generally showed decreases after the thermal. The

(-)- Epicatechin gallate (ECG) (-)- Epigallocatechin (EGC)

(-)- Epigallocatechin gallate (EGCG) (-)- Catechin gallate (CG)

(-)- Catechin (C) (-)- Epicatechin (EC)

7 decrease in ECG and EGCG may have affected the antioxidant activity of the extracts because these phenolic compounds are known to have more scavenging power than the flavan-3-ols that clearly increased: gallic acid, gallocatequin, and catechin), due to their stearic conformation and the presence of the gallate group joined to the C ring treatments,but they were not always significant (p<0.05).

B.

FOOD POWDER

A major reason for production in powder form is simply to prolong shelf-life of the ingredient by reducing water content; otherwise the ingredient would be degraded in its natural biological environment. Another important reason is simple transport economics, because reducing water content reduces mass and costs of the ingredient to be transported (Gustavo et al, 2010).

Food ingredient powders must possess a number of functionalities which can be broadly classified as: powder handling capability; reconstitution/ recombination ability and ingredient functionality in the food product to be consumed. Poor handling during manufacture, storage and transport causes many problems which are quite common, such as no or irregular flow out of hoppers and silos and problems associated with stickiness and caking of powders. Production and processing will determine the properties of particles and powder, such as particle size distribution, shape, surface properties and moisture content. They will also influence ingredient functionality, for example, higher temperatures may cause denaturation of proteins and coating may prevent the ingredient functionality from being destroyed by oxidation (Aguilera et al, 2008).

It is well known that ingredient functionality in powder form may degrade over time between manufacture and final application. This depends on the sensitivity of the individual ingredient and its exposure over time to temperature, moisture and oxygen in the air. Some ingredients are encapsulated and some powders are coated in an effort to prevent its degradation and protect its functionality outlinedsome of the functional properties of food powders and particulates (Lillford, 2002).

Powders are important ingredients in a large variety of food formulations and they are responsible for the development important product characteristics such as texture, flavour, colour and nutritional value. Most of the powders will be used in some sort of wet formulation and therefore their functionality will depend on their interaction with water. Because the influence of drying parameters is not the same for all materials, optimal drying conditions vary depending on the final objective: volatile retention, preservation of enzymatic activity and avoidance of protein denaturation, fat oxidation or crystallisation. Usually, the resulting powder is made of dry particles with an average size of 30 microns and mean water activity around 0.2. The powder outlet temperature is typically less than 100°C and the residence time is of seconds (Huntington, 2004).

All these characteristics will have some effect on handling properties of powders such as: bulk and tapped densities, particle density, mixing with other powders, storage; wettability and solubility, porosity, specific area (rehydration, instantisation); flowability (size, surface asperities), friability and creation/existence of dust, stability in specific atmosphere and medium (oxidation, humidification, active component release) (Huntington, 2004).

Study on quality evaluation instant green tea powder showed that the important quality attributes for a green tea sample was rated as taste > flavor > color > strength. Among the quality

8 attributes, taste was the strongest attribute for both instant tea and green tea granules produced, and strength was the weakest attribute. (Sinija, 2011).

C.

FREEZE CONCENTRATION

Concentration of fluid foods by freezing involves lowering the temperature of the product in a sufficiently controlled manner to partially freeze the product, resulting in a slurry of ice crystals in a fluid concentrate. If formed under the appropriate conditions, these ice crystals will be very pure. That is, very little product will be incorporated within the ice crystals. The ice crystals are then removed in some way with a minimum of liquid carryover, resulting in a concentrated product. The basic components of a freeze concentration system, as shown in Figure 4.

Freeze concentration is appliable to many food concentration, such as citrus fruit juices, vinegar, coffee, tea, sugar syrups, dairy product, and aroma extract. The major advantage of using a freeze concentration process as opposed to evaporation or reverse osmosis are related to the low temperature operation suitable for sensitive food products without the loss of product quality. In addition, the solid-liquid separation in freeze concentration results in no losses of the more volatile flavors and aromas, as occur in evaporation. The disadvantages of freeze concentration compared to evaporation and reverse osmosis have include higher capital cost, higher operating costs, and excessive loss of product during the ice separation (Hartel, 1992).

D. SPRAY DRYING

Spray drying is one-step continuous processing operation that can transform feed from a fluid state into a dried form by spraying the feed into a hot drying medium. The product can be a single particle or agglomerates. The feed can be a solution, paste, or a suspension. This process has become one of the most important methods for drying liquid foods to powder form. The principal of spray drying as shown in Figure 5.

Feed Crystal Nucleation

Crystal Growth

Separation Crystal Slurry

Concentrate Ice

9 The main advantages of spray drying are the following:

• Product properties and quality are more effectively controlled

• Heat-sensitive foods, biologic products, and pharmaceuticals can be dried at atmospheric pressure and low temperatures. Sometimes inert atmosphere is employed.

• Spray drying permits high tonnage production in continuous operation and relatively simple equipment

• The product comes into contact with the equipment surfaces in an anhydrous condition, thus simplifying corrosion problems and selection of material of construction

• Spray drying produces relatively uniform, spherical particles with nearly the same proportion of nonvolatile compounds as in the liqiud feed.

The principal disadvantages of spray drying are as follows:

• Spray drying generally fails if a high bulk density product is required

• In general it is not flexible. A unit designed for fine atomization may not be able to produce a coarse product, and vice versa.

• For given capacity, evaporation rates larger than other types of dryers are generally required due to high liquid content requirement. The feed must be pumpable. Pumping power requirement is high

• There is a high initial investment compared to other types of continuous dryers.

• Product recovery and dust collection increases the cost of drying (Xin and Mujumdar, 2010) Spray drying consist of four process stages:

1. Atomization of feed into a spray

The formation of spray and the contacting of the spray with air, are the characteristic features of spray drying. The selection and operation of the atomizer is of supreme importance in achieving economic production of top quality products. The selection of the atomizer type depend upon the nature of the feed and desire characteristics of the dried product. In all atomizer types, increased amounts of energy available for liquid atomization result in sprays having samLler droplet sizes. If, the available atomization energy is held constant but the feed rate is increased, sprays having Figure 5. Spray Dryer. 1, feed reservoir; 2, feed pump; 3, product feed pipeline; 4, atomizer; 5, drying chamber; 6, air fan; 7, air heater; 8, hot air duct; 9, a mixture of dried product and air-carrying duct; 10, cyclone separator; 11, heavy powder falling down; 12, product tank; 13,exhaust air (Sharma et al, 2000).

10 larger droplet sizes will result. Rotary atomizers are used to produce a fine to medium coarse product (mean size 30-130 µm), while nozzle atomizers are used to produce a coarse product (mean size 120-250 µm).

2. Spray-air contact (mixing and flow)

Product and air pass through the dryer in co-current flow, they pass through the dryer in the same direction. This arrangement is widely used, especially if heat-sensitive products are involved. Spray evaporation is rapid, the drying air cools accordingly, and evaporation times are short. The product is not subject to heat degradation.

3. Drying of spray (moisture/ volatiles evaporation)

As soon as droplet of the spray come into contact with the drying air, evaporation takes place from saturated vapour film which is quickly established at the droplet surface. The temperature at the droplet surface approximate to the wet-bulb temperature of the drying air. A substantial part of the droplet evaporation takes place when the droplet surfaces are saturated and cool. Drying chamber design and air flow rate provide a droplet residence time in the chamber, so that the desired droplet moisture removal is completed and product removed from dryer before product temperatures can rise to the outlet drying air temperature of the chamber. Hence, there is little likehood of heat damage to the product.

4. Separation of dried product from the air

Total recovery of dried product takes place in the separation equipment. This system places great importance on the separation efficiency of the equipment. Separation of dried product from the air influences powder properties by virtue of mechanical handling involved during the separation stage. Axcessive mechanical handling can produce powders having a high percentage of fines. (Master, 1991)

There are many variables in spray dryer that give an effect on powder product, such as inlet temperature, feed solid content, drying temperature difference, and feed temperature. Increase of inlet temperature can decrease the heat requirement of the dryer for producing a given product rate because product dried quickly. Increase in feed solids (for a given production rate) from 50% to 60% reduces the heat load by nearly 50%. Spray drying is an expensive method of evaporating volatiles and thus to obtain optimum heat utilization condition the spray dryer should always fed with the maximum solids feedstock possible. The higher the temperature difference (ie. Inlet drying air temperature minus outlet drying air temperature), the lower the heat requirement to produce a unit weight of product of constant residual moisture content from a constant solid feedstock. Feed temperature, particularly in existing plants, can also be optimized. Increasing feed temperature reduces the heat required to produce a unit weight of dried product. Preheating of feed is normally carried out to reduce feed viscosities, thereby improving atomization performance and to present feed crystallization that can cause atomizer blokage (Master, 1991).

11

III.

RESEARCH METHODOLOGY

A.

MATERIALS AND INSTRUMENTS

1. Materials

Dried green tea (var. Oolong No 12) was supplied by Boonrod Tea Factory (Thailand). Chemical reagents with analytical grade such as folin-ciocalteu (10% v/v) and gallic acid were supplied by Fluka (Buchs, Switzerland), anhydrous sodium carbonate and potassium hexacyanoferrate [K3Fe(CN)6] were purchased from Merck (Darmstadt, Germany), standard HPLC of caffeine and catechins were purchased from Sigma-Aldrich (St. Louis, Missouri, USA), acetonitrile, trifluoroacetic acid (TFA) and methanol (HPLC-grade) were purchased from Fluka (Buchs, Switzerland, trolox ((±)-6-Hydroxy-2,5,7,8-tetramethylchromane-2-carboxylic acid) and DPPH (2,2-diphenyl-1-picryhydrazyl) were purchased from Aldrich (Steinheim, Germany). monosodium phosphate monohydrate, Disodium phosphate heptahydrate and trichloroacetic acid (TFA) were purchased from Fluka (Buchs, Switzerland), citric acid (food grade), potassium mitrute salt (food grade). Then, distilled water, filter paper No 1 and No 4.

2. Instruments

The main instruments were JMC-miniLAB spray dryer ( Euro Best Technology, ltd, Thailand), ice cream maker and centrifuge (March Cool Industry Co.ltd, Thailand), hydrolic press (Owner Food Machinery Co.ltd, Thailand), hand refractometer (1-32˚Brix ATAGO Model N-2E, Japan), color analyzer (Colorquest XE HunterLab, Hunter Associates Laboratory, Inc, Virginia-USA), a spectrophotometer (UV Vis. Biochrom/Libra S22, England), HPLC C18, oven, disc mill, analytical balance, pH meter, vacuum pump.

B.

EXPERIMENTAL DESIGN

This research was divided into two parts. The preliminary research were investigation on the chemical properties of raw material (dried green tea leaves) involved moisture content, total polyphenol content, antioxidant activity, catechins, and caffeine. In experiment I (Figure 6), production of concentrated green tea was made from extract green tea and increased its concentration with ice cream maker, and then determine its chemical properties. In experiment II (Figure 7), production of green tea powder was made from concentrated green tea which dried with spray dryer, and then determine its physical and chemical properties.

1.

Production of Concentrated Green Tea

Dried green tea was milled with a disc mill into the small size of green tea. Milled green tea was extracted dissolved in the temperature of the hot water: 90°C and with regarding water: 1: 20 (w / v). The time of extraction used was 60 minutes, and pH value was 5,0 (Butsoongnern, 2006). Tea that has been extracted was filtered by clothes sheet and pressed by press machine to obtain the pure extract of green tea. Green tea extracts were analyzed TDS (total dissolved solids) with Refractometer and oven method. After that, green tea extract was concentrated with Freeze concentration method and it used ice maker

12 machine. The way of that machine working is turn on the power, paddle, and compressor buttons. After 10 minutes, compressor was turned off and wait the ice was released from the wall. Repeat this step for several times and it will resulting in a slurry of ice crystals in a fluid concentrate. The ice crystals were then removed in some way, in this study it used centrifuge machine for separate the ice crystals and a concentrated product. This step was continued until concentrated tea contain of total solid about 3, 6, and 9%, which was measured with refractometer and confirmated with oven method.

2.

Production of Green Tea Powder

Production of green tea powder with spray drying method is shown at Figure 7. Figure 6. Flow chart of green tea concentrated making

Figure 7. Flow chart of spray drying process

Chemical Analysis: Moisture content, Total

polyphenol content, antioxidant activity, catechins, and caffeine Dried green tea leaves

Milling

Extraction

Filtering Green tea Extract

Freeze Concentration

Concentrated Green Tea Extract (3,6,9%)

Green tea extract concentrated (3,6,9%)

Spray Drying Green tea powder

Characteristic of Final product

inlet air temperatures: 180, 200, 220°C

Physical: bulk density, color,

solubility, hygroscopicity

Chemical: Moisture content, Total polyphenol content, antioxidant activity, catechins, and caffeine

13 Green tea extract that was concentrated by ice maker until its concentration reached 3, 6 and 9%, were dried with spray drier. The operational conditions of the spray drying were as follows: inlet air temperatures were 180, 200, 220°C, outlet air temperatures is controlled about 75°C, blower speed was adjust in 2500 rpm. . To control outlet temperature at 75˚C, the pressure air and feed rate were increased or decreased. The pressure air and feed rate were affected by inlet air temperature, an increase inlet air temperature, the pessure air and feed rate increased. After spray drying process has done, characteristic of final product should be analyzed. The physical and chemical characteristics of final products were evaluated.

3.

Method of Analysis

3.1. Bulk density (Bhandari et al., 1992)

Bulk density was determined by the tapping method. Two grams of powder were loosely weighed into 10 mL graduate cylinder. The cylinder containing the powder was tapped on a flat surface to a constant volume. The final volume was recorded and bulk density was calculated by dividing the sample weight by the volume.

3.2. Color Analysis (Quek et al., 2007)

Color values of dried samples (L, a, and b) were measured by using ColorQuestXE/Hunter Lab (USA).

3.3. Solubility (%) (Sanphakdee, 2007)

Weigh powder sample 0,5 g and mixed with 50mL of distilled water (25˚C) in an 100mL beaker glass. Then it was agitated using a magnetic stirer (size 2 mm X 7mm) at a speed of 600rpm. The residue was filtrated on a filter paper No 4 and using the vacuum pump. The filter paper with an insoluble solid was placed in an oven set at 102 ± 2˚C until the weight was constant. The solubility(%) was calculated by using the following equation:

( )

Where m1 is weight of filter paper and insoluble solid after dried by oven, m2 is weight of dried filter paper, and m is weight of powder sample.

3.4. Hygroscopicity (%) (Jaya and Das, 2004, modification)

A saturated solution of potassium nitrite salt (equilibrium relative humidity = 79.5±2% at 20ºC) was kept in glass wash bottle having two passage for air inlet and outlet. A diaphragm type vacuum pump was used to suck the air through the salt solution. Take filter paper in pump and weigh it until constant, then add powder sample 0,5 g and it was spread uniformLy in the filter paper. The increase in weight of the sample at every 15 min was noted. This measurement was continued till the difference between two succesive weighings not exceed by 0.5%. The entire operation was carried out in a room maintained at 20ºC.

72 24. 5 Epigallocatechin gallate (EGCG)

trt N

Subset

1 2 3

6%, 200C 2 4.6150

6%, 220C 2 5.4250 5.4250

6%, 180C 2 5.6150 5.6150

9%, 220C 2 5.7100 5.7100

9%, 180C 2 5.8900 5.8900

3%, 180C 2 6.4900 6.4900

3%, 200C 2 6.5200 6.5200

3%, 220C 2 7.0150

9%, 200C 2 7.0550

Sig. .069 .075 .059

Means for groups in homogeneous subsets are displayed. Based on observed means.

The error term is Mean Square(Error) = ,247. 24. 6 Gallocatechin gallate

trt N

Subset 1

9%, 220C 2 1.4100

6%, 200C 2 1.4500

9%, 180C 2 1.4600

3%, 200C 2 1.5300

9%, 200C 2 1.5750

6%, 180C 2 1.6000

3%, 180C 2 1.6050

6%, 220C 2 1.6100

3%, 220C 2 1.6350

Sig. .126

Means for groups in homogeneous subsets are displayed.

Based on observed means.

The error term is Mean Square(Error) = ,015.

73 24. 7 Epicatechin gallate

trt N

Subset

1 2

6%, 200C 2 .7350

6%, 180C 2 .8550 .8550

9%, 180C 2 .9100 .9100

6%, 220C 2 .9250 .9250

3%, 200C 2 .9850 .9850

3%, 180C 2 1.0150 1.0150

9%, 220C 2 1.0500

3%, 220C 2 1.0600

9%, 200C 2 1.1000

Sig. .058 .090

Means for groups in homogeneous subsets are displayed.

Based on observed means.

38

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Purwiyatno Hariyadi, Hanifah Nuryani Lioe, Natthawuddi Donlao. 2011.

SUMMARY

Tea is globally one of the most popular and lowest cost beverages, next only to water. Nowadays, tea powder is being developed because it has many advantages such as more practical, simple transport economics, and simply to prolong product’s shelf-life. There are several method to produce tea powder, one of them is spray drying method. The objectives of this research are to investigate the effect of solid concentration in feeds and inlet air temperatures of spray dryer on physical and chemical properties of green tea powder.

In the preliminary research, chemical composition of raw materials involved moisture content, total polyphenols, antioxidant activity, caffeine, and catechin content were determined. In experiment I, production of concentrated green tea was made from extract green tea and increase its concentration with ice cream maker. In experiment II, production of green tea powder with JMC-minilab spray dryer. The resulted green tea powder were then analyzed for its physical properties (such as bulk density, color, solubility, and hygroscopicity) and chemical properties (such as moisture content, total polyphenol content, antioxidant activity catechins, and caffeine contain).

Results showed that dried green tea (Camellia sinensis var. Oolong No 12) contains moisture content 6.05 ± 0.06% w/w wb, total polyphenol 14.98 ± 0.42% db, antioxidant activity 141.5 ± 6.88 mmol Trolox/100 g db, caffeine 2.77 ± 0.23 g/100 g db, and catechin 12.04 ± 1.20 g/100 g db. There is a linear relationship between ˚brix from refractometer and total solid of oven method with regression y = 0.842x + 0.142, R2= 0.997. Limited concentration of concentrated tea with ice cream maker machine until 11% total solid. Concentrated tea more than 11% total solid, it will deposit at the wall machine and decreased percentage of freeze concentration recovery. Therefore, parameter solid concentration in feed that used were 3,6, and 9%.

The quality of product especially chemical quality is greatly influenced by production method. The effect of green tea powder production method such as extraction, freeze concentration, and spray drying on its chemical properties such as total polyphenols content, catechins, caffeine, and antioxidant activity have been studied. Amount of total polyphenols, catechins, caffeine, and antioxidant activity of sample decreases significantly (p<0.05) after it was treated by different process such as extraction, concentration, and spray drying. Base on the results, the powder with treatment solid concentration 3% in feed and inlet temperature 220˚C has the highest chemical yield and powder with treatment total solid concentration 9% in feed and 180˚C has the lowest one.

The different solid concentration 3, 6, 9% in feed and inlet air temperatures of 180, 200, and 220˚C affected physical and chemical properties of green tea powder. An increase inlet air temperature, resulted in a significant decrease (p<0.05) in bulk density, hygroscopicity, total polyphenols and antioxidant activity. An increase of solid concentration in feed gave an increase in tea powder solubility, L, a, b value, and antioxidant activity. However, the total polyphenols contents were not affected by the increase of solid concentration.

The physical results of green tea powder are bulk density of the powder variated between 0.3933-0.5014 g/mL, L value variated between 68.07-74.41, a value variated between 3.50-5.79, b value variated between 30.08-37.37, solubility variated between 75.56-91.17%db, hygroscopicity 8.84-17.84%. The chemical results of green tea powder are moisture content variated between