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1 , Vol. 11, No. 2, pp. 85-9, Jun. 21 X Evaluation of Retrogradation in Microwave Cooked Rice Using X-ray Diffraction Method. Saki YOSHIDA, Mika FUKUOKA, and Noboru SAKAI Tokyo University of Marine Science and Technology, Konan, Minato-ku, Tokyo , Japan Progress of retrogradation of rice grain which was cooked by microwave heating was evaluated using X-ray diffraction (XRD) method. Cooked rice grains were not powdered but made to paste and measured directly. A lot of samples were able to be measured by this convenient method. The polarization microscopy was also conducted for visualization of retrogradation. The differences in retrogradation observed by XRD were found between rice grains in the cooking container like differences in cooking properties such as moisture content and degree of gelatinization. Progress of retrogradation was observed after 12 hours from beginning of storage at 5. Using Avrami equation, kinetic parameters of retrogradation were calculated. Rate constant of retrogradation was greatly affected by moisture content of cooked rice grain. In the case of low moisture content gave a high rate constant for retrogradation. Keywords: retrogradation, rice grain, microwave heating, X-ray diffraction, polarization microscopy 1 [1] Fax: , fukuoka@kaiyodai.ac.jp DSC - X [2-7] DSC BAP [1,3-7]BAP DSC [5,7] [8] [1,3] X [1,3,9,1]

2 86 X g g 6 W g MHz 712 Fluoroptic thermometer, Luxtron Fig. 1 JNK-R1 T cc fiber-optic thermometer 4.4cm 17cm 1cm 3cm Fig. 1 Container of cooking rice by microwave heating. The diameter of the container was 17 cm, and height was 1 cm. Uncooked Rice grain layer : 3 cm in height from the bottom of the container, Water layer : 4.4 cm in height from the bottom. The aluminum tape was put in the lid and the bottom in the container Fig BX5 Fig m 2.4 X Fig. 1 5 g 1.5 g X PET X 5 X X MiniFlex II X CuK3 kv15 ma mm X X 2 X Cr Speak Cr 1 1 S cr S cr S peak S cr K 2 Sonneveld-Visser [11] K 2 Rachinger [12] X

3 XRD U(t) Avrami CrtCri U ( t) 2 Cr Cr f Cr i 5 Cr f Cr t t U(t) t Avrami 3 [12,13] U ( t) 1exp( kt n ) 3 k t n Avrami Cr Avrami Cr f Avrami n Fig i Fig Fig. 4 5 X Fig X X Temperature () 5 Microwave heating heating Electric electric rice-cooker Power ON Power OFF Time (min) Fig. 2 The temperature history at the center point of the container during microwave heating. A measured position was as shown in Fig. 1. Fig. 3 Water content of cooked rice grain at position, and in the container as shown in Fig. 1, and rice grain cooked by electric rice cooker.

4 degree) degree degree Fig. 4 Changes of X-ray diffractograms of cooked rice during storage at 5., and corresponds to the different position in the container as shown in Fig. 1. The numbers show the storage time every 12 hours Fig. 5 Fig. 3, 12 Fig. 3, 72 [13,14] 3.3 Fig. 6 Fig. 5 Changes of relative crystallinity of cooked rice during storage at 5., and corresponds to the position in the container as shown in Fig. 1. The lines indicate the best fitting curves of Eq.(3). Fig. 6 Retrograded cooked rice section with different storage time at every 24 hours., and corresponds to the position in the container as shown in Fig. 1.

5 XRD 89 [15]Fig. 6 [15] [16] [16] X Fig. 5 X 3.4 Cr Avrami 3 Avrami Cr f Table 1 Fig. 5 Cr f Avrami NMR Avrami [13] I NMR X NMR [13] Table 1 Avrami parameters for retrogradation of cooked rice Sample Water content (d.b) (-) Cr f n a k(day -n ) b a Avrami exponent of time b Avrami rate constant of crystallite growth 4

6 9 X 1 6W 2X 3 3 X 4Avrami Avrami 1) M. Nakamura, K. Kainuma; Biochemistry experiment method 19 Starch, Related glucidic experiment method (Seibutukagaku Jikkenhou 19 Denpun, Kanren tousitsu Jikkenhou), Japan Scientific Societies Press, Tokyo, Japan, 1998, pp.72-77, , ) M. Fukuoka; Starch Gelatinization arid Retrogradation (in Japanese). Refrigeration., 78( 97), (23). 3) Y. Ikawa, C.Kikuchi, S. Kanehira, Y.Murakawa, S. Ijiri; Comparative Study on Evaluation Methods for Retrogradation of Cooked Rice at the Early Stage (in Japanese). Japan J. Appl. Glycosci., 49, (22). 4) M. Otahara, K. Hatae, A. Shimada; Objective Evaluation of Staling of Cooked Rice (in Japanese). J. Home Economics of Japan., 46, (1995). 5) A. Mizuno, M. Mitsuiki, M. Motoki; Effect of Crystallinity on the Glass Transition Temperature of Starch. J. Agric Food Chem., 46, (1998). 6) LIMA I, SINGH R P.; Objective measurement of retrogradation in cooked rice during storage. J Food Qual., 16(5), (1993). 7) S. Kitamura, Gelatinization and senescence of starch (especially, analysis by DSC) (in Japanese). Japan. Starch., 37, (1992). 8) Y. Ikawa, C. Kouno(Kikuchi); Multiple Evaluation of Cooked Rice Retrogradation in Early Stage of Storage (in Japanese). Japan J. Appl. Glycosci., 52, (25). 9) RIBOTTA P D, LEON A E, CUFFINI S, ANON M C; The staling of bread: an X-ray diffraction study. Eur. Food Res. Technol., 218, (24). 1) BAYER R. K., BALTA-CALLEJA F. J.; Nanostructure of Potato Starch. II. Structure of a Highly Crystalline Gel Obtained by Retrogradation Using X-Ray Diffraction Techniques. J. Appl. Polym. Sci., 14, (27). 11) E. J. Sonneveld, J. W. Visser; Automatic collection of powder data from photographs. J. Appl. Cryst., 8, 1-7(1975). 12) A. Guinier; Theory and practice of X-ray crystallography (X-senn Kesshougaku no Riron to Jissai. Rigaku electric company, Tokyo, Japan, 1967, p ) YAO Y, DING X; Pulsed Nuclear Magnetic Resonance (PNMR) Study of Rice Starch Retrogradation. Cereal Chem., 79, (22). 14) FARHAT I A, BLANSHARD J M V, MITCHELL J R; The Retrogradation of Waxy Maize Starch Extrudates: Effects of Storage Temperature and Water Content. Biopolymers., 53, (2). 15) C. Shinoda, M. Fukuoka, H. Watanebe; Visualizing the Progress of Starch Gelatinization in a Rice Grain during Cooking (in Japanese). J. Cook. Sci. Jpn., 34, (21). 16) T. Nagata, A. Horikane., Advanced measurement of agricultural products and food, Measurement of rice grain internal structure by MRI (nuclear magnetic resonance imaging) (in Japanese). J. Agric., Forestry and Fisheries Res., 24, 5-11 (21). DSC BAP X X 12 Avrami

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