2012 34 2 382-387 http / /xuebao. jxau. edu. cn Acta Agriculturae Universitatis Jiangxiensis E - mail ndxb7775@ sina. com 212018 105 W 42 2 min 0. 631 TS202. 3 A 1000-2286 2012 02-0382 - 06 Optimizing Microwave-assisted Extraction Process for Paprika Red Pigments Using Response Surface Methodology DENG Xiang-yuan LIU Yue-han GAO Kun SUN Jun-long College of Biotechnology and Chemical Engineering Jiangsu University of Science and Technology Zhenjiang 212018 China Abstract Hot red peppers are used as raw the material paprika red pigments were prepared with acetone using the method of microwave - assisted organic solvent extraction. The influences of process parameters including microwave output power microwave temperature and microwave time on extraction efficiency of paprika red pigments were compared and analyzed moreover the extraction process was optimized via single-factor tests and response surface experiments. The results showed that the method of microwave-assisted organic solvent extraction was an effective and practicable one for paprika red pigments extraction and the spectral properties and characteristic absorption peak of paprika red pigments were similar to those of standard compound. In addition the most suitable conditions for paprika red pigments extraction were as follows acetone was used as the extraction solvent microwave output power was 105 W microwave temperature was 42 and microwave time was 2 min. When the optimal conditions were met the absorbance value of paprika red pigments reached 0. 631. Key words paprika red pigments extraction process response surface methodology microwave-assisted organic solvent extraction 2011-10 - 19 2012-01 - 10 BK2011493 35290902 1982 E - mail dengxy2009@ 126. com
2 383 1 2 3-4 50% ~ 60% 5 β - VA 6 7 8 9 10 11 12 13 14 15 16 17-18 1 1. 1 60 40 98% Mars UV - 1800PC - 1. 2 1. 2. 1 1 g 90 W 40 2 min 1. 2. 2 1 Fig. 1 The spectral properties and maximum absorption peak of paprika red pigments 0. 02 g 100 ml - 1 1 400 ~ 560 nm 460 nm 19 20 460 nm 1. 2. 3 21 22-23 1 g
384 34 1. 2. 4 1 g 24 - OD 460 Box - Behnken 25 3 X 1 X 2 X 3-1 0 + 1 1 Design Expert 7. 1. 6 Y = β 0 + 3 β i X i + 3 β ij X i X j + 3 β ij X 2 i i = 1 i < j = 1 i = 1 Y OD 460 X i X j β i β ij β ii Tab. 1 1 Box - Behnken Factor levels design of Box - Behnken experiments for optimizing microwave - assisted extraction process of paprika red pigments Independent variables Codes Code levels - 1 0 1 /W Microwave output powers X 1 60 90 120 / Microwave temperatures X 2 35 40 45 /min Microwave time X 3 1 2 3 1. 2. 5-460 nm 2 2. 1 2. 1. 1 1 g 1 8 g /ml 30 60 90 120 150 W 2 min OD 460 2 2 90 ~ 120 W 120 W 60 W 90 W 2 120 W 3 Fig. 2 Effect of different microwave output powers on extraction efficiency of paprika red pigments 2. 1. 2 30 35 40 45 50 3 3 40 ~ 45 35 40 45 3 β 0
2 385 2. 1. 3 1 2 4 6 8 min 5 4 4 2 min 3 Fig. 3 Effect of different microwave temperatures on extraction efficiency of paprika red pigments 1 2 3 min 3 2. 2 2. 2. 1 4 Fig. 4 Effect of different microwave time on extraction efficiency of paprika red pigments 1 2 2 Tab. 2 2 Experimental design and corresponding results for response surface experiments /W Test code Microwave output powers / Microwave temperatures /min Microwave time /OD 460 Absorbance values 1 60 35 2 0. 544 2 90 40 2 0. 621 3 90 40 2 0. 632 4 120 45 2 0. 627 5 60 45 2 0. 554 6 90 35 1 0. 521 7 120 40 1 0. 568 8 90 40 2 0. 631 9 60 40 1 0. 562 10 90 35 3 0. 558 11 60 40 3 0. 548 12 90 45 1 0. 566 13 120 40 3 0. 582 14 120 35 2 0. 556 15 90 45 3 0. 601 16 90 40 2 0. 622 17 90 40 2 0. 616
386 34 Box - Benhnken 17 12 5 2. 2. 2 Design Expert 7. 1. 6 2 3 OD 460 = 0. 62 + 0. 016 + 0. 021 + 9 10-3 + 0. 015 + 7 10-3 - 5 10-4 - 0. 025 2-0. 029 2-0. 035 2 Tab. 3 3 Analysis of variance for the fitted quadratic equation and significance test of the regression coefficients in it Variance sources Sum of squares Degree of freedom Mean square F Value of F P F > F α Value of Significance P Model 0. 020 9 2. 185 10-3 13. 95 0. 001 1 ** Microwave output powers 1. 953 10-3 1 1. 953 10-3 12. 47 0. 009 6 ** Microwave temperatures 3. 570 10-3 1 3. 570 10-3 22. 79 0. 002 0 ** Microwave time 6. 480 10-4 1 6. 480 10-4 4. 14 0. 081 4 Microwave output powers Microwave temperatures 9. 302 10-4 1 9. 302 10-4 5. 94 0. 045 0 * Microwave output powers Microwave time 1. 960 10-4 1 1. 960 10-4 1. 25 0. 300 2 Microwave temperatures Microwave time 1. 000 10-6 1 1. 000 10-6 6. 384 10-3 0. 938 6 2 2. 700 10-3 Microwave output powers 2 2 3. 498 10-3 Microwave temperatures 2 2 4. 889 10-3 Microwave time 2 1 2. 700 10-3 17. 24 0. 004 3 ** 1 3. 498 10-3 22. 33 0. 002 1 ** 1 4. 889 10-3 31. 21 0. 000 8 ** Residual 1. 096 10-3 7 1. 566 10-4 Lack of fit 9. 073 10-4 3 3. 024 10-4 6. 39 0. 052 5 Pure error 1. 892 10-4 4 4. 730 10-5 Cor total 0. 021 16 R 2 = 0. 947 2 Adjusted R 2 = 0. 879 3 Adeq Precision = 9. 743 ** 0. 01 * 0. 05 ** significant at 0. 01 level * significant at 0. 05. 3 3 P = 0. 001 1 < 0. 01 P = 0. 052 5 > 0. 05 Adjusted R 2 = 0. 879 3 Adeq Precision = 9. 743 4 P 0. 05 2 2 2
2 387 2. 2. 3 104. 45 W 42. 46 2. 18 min 0. 634 105 W 42 2 min 0. 631 1% 3 1 2 105 W 42 2 min 0. 631 1. J. 2009 3 6 88-90. 2. J. 2006 31 10 49-53. 3. J. 2004 15 6 22-25. 4. J. 1999 14 1 21-25. 5. J. 2003 26 2 37-41. 6. J. 1997 13 1 5-6. 7. J. 2002 18 5 34-35. 8. J. 2003 3 30-32. 9. J. 2005 41 3 17-22. 10. J. 2005 32 5 52-54. 11. J. 2009 36 1 66-69. 12. J. 2006 17 3 50-53. 13. J. 2011 40 5 92-94. 14. J. 2006 27 10 92-93. 15. J. 2008 24 6 96-101. 16. J. 2001 29 2 70-73. 17. J. 2005 21 2 153-156. 18 Song J Z Mo S F Yip Y K et al. Development of microwave assisted extraction for the simultaneous determination of isoflavonoids and saponins in radix astragali by high performance liquid chromatography J. J Sep Sci 2007 30 6 819-824. 19. J. 2004 31 1 15-17. 20 Hornero - Méndez D Mínguez-Mosquera M I. Rapid spectrophotometric determination of red and yellow isochromic carotenoid fractions in paprika and red pepper oleoresins J. J Agric Food Chem 2001 49 8 3584-3588. 21. J. 2008 29 8 307-309. 22. J. 2003 20 6 4-6. 23. J. 2009 37 34 17085-17087. 24. J. 2004 32 11 29-31. 25. J. 2006 22 6 42-45.