6 6 Vol. 6 No. 6 2015 6 Journal of Food Safety and Quality Jun., 2015 娄 秋 艳, 孙 汉 巨 *, 王 鑫, 章 萍 萍, 谢 玉 鹏, 张 曼 莉, 王 霄 (, 230009) 摘 要 : 目 的, 方 法,, CaCl 2,, ;, L 9 (3 4 ), ;,, 结 果 : 3:1 0.45 mm 2.0% CaCl 2 2.0%; 4.0 h, 结 论, 关 键 词 : ; ; ; ; Study on preparation of microcapsules of anthocyanins from black rice LOU Qiu-Yan, SUN Han-Ju *, WANG Xin, ZHANG Ping-Ping, XIE Yu-Peng, ZHANG Man-Li, WANG Xiao (School of Biotechnology and Food Engineering, Hefei University of Technology, Hefei 230009, China) ABSTRACT: Objective To develop a kind of microcapsule of anthocyanins from black rice, which can arrive to the intestinal successfully with a sustained release and exert the prebiotic efficacy of anthocyanins. Methods Using the orifice method, the imbedding ratio of anthocyanins as evaluation index and the wall-core ratio, aperture of needle, sodium alginate mass fraction, and CaCl 2 concentration as factors, the conditions of making microcapsule were determined by single-factor experiments. On this basis, the preparation technology was optimized by orthogonal experiment. At last, the sustained-release function of microcapsules was verified by releasing experiment in the human stomach and intestine simulation liquid. Results The optimum preparation process was as follow: wall-core ratio 3:1, aperture of needle 0.45 mm, sodium alginate 2.0% and CaCl 2 2.0%. The microcapsules could maintain in the stomach simulation liquid for 4.0 h or more, and release slowly in the intestine simulation liquid. Conclution The microcapsules made with the orifice method could reach the intestinal canal successfully, release slowly and exert the prebiotics efficacy of anthocyanins. KEY WORDS: anthocyanins; sustained release; microcapsule; prebiotics; technology research 基 金 项 目 : 2015 (31171787) Fund: Supported by the Autumn Plan of 2015 of Hefei University of Technology and the National Natural Science Foundation of China (31171787) * 通 讯 作 者 :,,, E-mail: sunhanjv@163.com *Corresponding author: SUN Han-Ju, Ph. D, Professor, School of Biotechnology and Food Engineering, Hefei University of Technology, Hefei 230009, China. E-mail: sunhanjv@163.com
2000 6 1 引 言 (anthocyanin),,,, 27 72 [1,2], ph ph 2, ; ph 2~6, ; ph>7, [3],, [4,5],,, (microencapsulation),,,,, (microcapsule), 0.1~10000 μm [6-8], ; [9,10],, ;, [11-13] (prebiotic),,, [14], ( ), [15],,,,,,,, 2 材 料 与 方 法 2.1 材 料 与 试 剂 ( 25%, ); (, ); (, ); (, ); (, ); (, ); 2.2 仪 器 及 设 备 AR1140 ( ); SHZ-D(Ⅲ)( ); SHA-BA ( ); 722E ( ); 0.45 0.50 0.55 0.60 mm ( ); phs-3c ph ( ) 2.3 工 艺 流 程 CaCl 2 CaCl 2 2.4 操 作 要 点 (1): 1.5 2.0 2.5 3.0 g, 90,,, 100 ml, 1.5% 2.0% 2.5% 3.0%(m:V) (2) : 73.0 mg,, 100 ml, 0.73 mg/ml (3)CaCl 2 : 0.5 1.0 1.5 2.0 2.5 g CaCl 2,, 100 ml, 0.5% 1.0% 1.5% 2.0% 2.5%(m:V) CaCl 2 (4): 16.4 ml (1 mol/l),, 1000 ml, ph 1.2 (5) : 17.805 g 9.605 g,, 500 ml, 0.2 mol/l 0.1 mol/l
6, : 2001 15.45:4.55, ph 6.8 [16] 2.5 花 青 素 微 胶 囊 制 备 的 评 价 标 准, (1): CV 1 1 C2V2 Y 100% CV 1 1 : Y (%); C 1 (mg/ml); V 1 (ml); C 2 (mg/ml); V 2 (ml) 2.6 花 青 素 微 胶 囊 制 备 单 因 素 试 验 2.6.1 壁 芯 比 对 花 青 素 包 埋 率 的 影 响 5 1 ml 0.73 mg/ml, 2:1 3:1 4:1 5:1 6:1(V:V) 2.0%, 0.45 mm 50 ml 2.0% CaCl 2, -0.1 MPa,,,, 515 nm (OD),,, (1) 2.6.2 针 头 孔 径 对 花 青 素 包 埋 率 的 影 响 4 1 ml 0.73 mg/ml, 3:1(V:V) 2.0%, 0.45 0.50 0.55 0.60 mm, 50 ml 2.0% CaCl 2, 2.6.1, 2.6.3 海 藻 酸 钠 对 花 青 素 包 埋 率 的 影 响 4 1 ml 0.73 mg/ml, 3:1(V:V) 1.5% 2.0% 2.5% 3.0%, 0.50 mm, 50 ml 2.0% CaCl 2, 2.6.1, 2.6.4 CaCl 2 对 花 青 素 包 埋 率 的 影 响 5 1 ml 0.73 mg/ml, (1) 3:1(V:V) 2.0%,, 0.50 mm, 50 ml 0.5% 1.0% 1.5% 2.0% 2.5% CaCl 2, 2.6.1, 2.7 花 青 素 微 胶 囊 制 备 正 交 试 验, L 9 (3 4 ) [17], : (2:1 3:1 4:1), (0.45 mm 0.50 mm 0.55 mm), (1.5% 2.0% 2.5%), CaCl 2 (1.0% 1.5% 2.0%),, 2.8 花 青 素 微 胶 囊 在 胃 肠 模 拟 液 中 的 释 放 试 验 2 1 ml 0.73 mg/ml,,, 50 ml 50 ml,, 37 50 r/min, 0.5 h, (2) CV 4 4 Z 100% CV Y 3 3 : Z (%); Y (%); C 3 (mg/ml); V 3 (ml); C 4 (mg/ml); V 4 (ml) 3 结 果 与 分 析 3.1 壁 芯 比 对 花 青 素 包 埋 率 的 影 响 ( 1),, ;,,, 2:1~6:1 1, 2:1,,, ; 3:1 (70.82%);,,,,,, CaCl 2, (2)
2002 6, 3:1 3.3 海 藻 酸 钠 对 花 青 素 包 埋 率 的 影 响 3,, 2.0%(87.74%),,,,,,,,,,,,, 2.0% 1 (%) Fig. 1 Effect of wall-core ratio on imbedding ratio of anthocyanins 3.2 针 头 孔 径 对 花 青 素 包 埋 率 的 影 响 2, 0.45 mm,, 0.50 mm, (85.18%), 0.50 mm,,,, CaCl 2,, 0.50 mm Fig. 3 3 Effect of sodium alginate concentration on imbedding ratio of anthocyanins 3.4 CaCl 2 对 花 青 素 包 埋 率 的 影 响 CaCl 2 4, CaCl 2, 1.5%(95.16%);, CaCl 2 CaCl 2,, CaCl 2, Na + Ca 2+,,, CaCl 2 1.5% Fig. 2 2 Effect of aperture of needle on imbedding ratio of anthocyanins 3.5 花 青 素 微 胶 囊 制 备 最 佳 工 艺 的 确 定 1 1, : CaCl 2, 4
6, : 2003 (94.54%), A 2 B 1 C 2 D 3, 3:1 0.45 mm 2.0% CaCl 2 2.0% A 2 B 1 C 2 D 2, A 2 B 1 C 2 D 3 A 2 B 1 C 2 D 2, 94.69 93.12%, A 2 B 1 C 2 D 3, : 3:1 0.45 mm 2.0% CaCl 2 2.0% 3.6 花 青 素 在 胃 及 肠 模 拟 液 中 的 缓 释, 4.0 h,, 4.0 h,,,,, 5,, 4.0 h,, 3.0 h (5.06%),, 4.0 h,, 3.5 h (98.42%),,,,,,,,, Fig. 4 4 CaCl 2 Effect of CaCl 2 concentration on imbedding ratio of anthocyanins 5 Fig. 5 The releasing of anthocynins in the stomach and intestine simulated liquid Table 1 表 1 花 青 素 微 胶 囊 制 备 正 交 试 验 结 果 Results of making microcapsule of anthocyanins A B C D (ml/ml) mm (%) CaCl 2 (%) (%) 1 1(1:2) 1(0.45) 1(1.5) 1(1.0) 75.68±0.03 2 1 2(0.5) 2(2.0) 2(1.5) 87.88±0.03 3 1 3(0.55) 3(2.5) 3(2.0) 71.22±0.05 4 2(1:3) 1 2 3 94.54±0.03 5 2 2 3 1 76.72±0.04 6 2 3 1 2 83.22±0.03
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