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1 6 6 Vol. 6 No 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 (, ) 摘要 : 目的, 方法,, CaCl 2,, ;, L 9 (3 4 ), ;,, 结果 : 3: 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 , 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 ( ) Fund: Supported by the Autumn Plan of 2015 of Hefei University of Technology and the National Natural Science Foundation of China ( ) * 通讯作者 :,,, sunhanjv@163.com *Corresponding author: SUN Han-Ju, Ph. D, Professor, School of Biotechnology and Food Engineering, Hefei University of Technology, Hefei , China. sunhanjv@163.com

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

2 引言 (anthocyanin),,,, [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 ( ); mm ( ); phs-3c ph ( ) 2.3 工艺流程 CaCl 2 CaCl 操作要点 (1): 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 : 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) : g g,, 500 ml, 0.2 mol/l 0.1 mol/l

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.

3 6, : :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) 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%, mm, 50 ml 2.0% CaCl 2, 2.6.1, 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, 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,, 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)

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.

4 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

50 mm,,,, CaCl 2,, 0.50 mm Fig. 3 3 Effect of sodium alginate concentration on imbedding ratio of anthocyanins 3.

5 6, : 2003 (94.54%), A 2 B 1 C 2 D 3, 3: 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, %, A 2 B 1 C 2 D 3, : 3: 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± (0.5) 2(2.0) 2(1.5) 87.88± (0.55) 3(2.5) 3(2.0) 71.22± (1:3) ± ± ±0.03

4 4 CaCl 2 Effect of CaCl 2 concentration on imbedding ratio of anthocyanins 5 Fig.

6 续表 1 A B C D (ml/ml) mm (%) CaCl 2 (%) (%) 7 3(1:4) ± ± ±0.04 K K K R ADBC A 2 B 1 C 2 D 2 4 结论,, : 3: mm 2.0% CaCl 2 2.0%,, 3.0 h 3.5 h, (5.06% 98.42%),,, 4.0 h, ;,,, 参考文献 [1]. [D]. :, Yang S. Extraction and purification of anthosyanin in blank mulberry (Morus nigra Linn) fruit and its characteristic testing [D]. Hefei: Anhui Agricultural University, [2]. [D]. :, Shi J. Study on separation, purification and vivo antioxidative activity of anthocyanins from black rice [D]. Hefei: Hefei University of Technology, [3],,,. [J]., 2014, 17(8): Lou QY, Sun HJ, Chen XY, et al. Study on the formulation of composite health anthocyanin and juice drink [J]. Bev Ind, 2014, 17(8): [4]. [D]. :, Bao XL. Study on extraction and characterization of black rice anthocyanin [D]. Changchun: Jilin Agricultural University, [5]. [D]. :, Li XY. Investigation on separation, purification and biological activity of anthocyanins and polyphenols in blueberry [D]. Tianjin: Tianjin University, [6],. [J]., 2009, 37(11): Li Y, Pang LY. Research progress on microencapsulation technology in food industry [J]. Guizhou Agric Sci, 2009, 37(11): [7],. [J]., 2002, 27(7): Wang DJ, Zhao YR. Application and recent progress of microencapsulation [J]. New Chem Materials, 2002, 27(7): [8], 珺,. [J]., 2011, 1: 3 6, 20. Wu X, Wang J, Huo NX. Microencapsulation technology and its application in food industry [J]. Food Eng, 2011, 1: 3 6, 20. [9],,. [J]., 2003, (17): Su JF, Ren L, Wang LX. Technology and recent progress of microencapsulation [J]. Materials Rev, 2003, 17:

Extraction and purification of anthosyanin in blank mulberry (Morus nigra Linn) fruit and its characteristic testing [D]. Hefei: Anhui Agricultural University, 2012. [2]. [D]. :, 2012. Shi J.

7 6, : 2005 [10],,,. [J]., 2013, 21(34): Yang XL, Yuan Y, Tan YR, et al. Research and applications on nanocapsule technology in functional foods [J]. Food Sci, 2013, 21(34): [11]. [D]. :, Wang X. Study on the preparation of anthocyanins from lonicera edulis turcz microcapsules and their stability [D]. Harbin: Harbin Institute of Technology, [12],. [J]., 2012, 6: Ding BM, Yuan WH. Preparation of proanthocyanjdin microcapsuies by piercing method [J]. Food Mach, 2012, 6: [13],. [M]. :, Wu KG, Chai XH. Food microcapsulation [M]. Beijing: China Light Industry Press, [14]. [D]. :, Huang MY. Study on the extraction, purification and prebiotic activity of rapeseed polysaccharides [D]. Hefei: Hefei University of Technology, [15]. [D]. :, Zhang ML. Study on activity of probiotics and harmful bacteria in vitro and molecular modification of black rice anthocynins [D]. Hefei: Hefei University of Technology, [16],,,. [M]. :, Li JW, Yu RY, Yuan MX, et al. Biochemistry experimental principle and method [M]. Beijing: Peking University Press, [17],. [M]. :, Pan LJ, Chen JQ. Experimental design and data processing [M]. Nanjing: Southeast University Press, 作者简介 ( 责任编辑 : 杨翠娜 ) 娄秋艳, 硕士研究生, 主要研究方向为食品工程 @qq.com 孙汉巨, 博士, 教授, 主要研究方向为农产品的综合利用 sunhanjv@163.com

Ding BM, Yuan WH. Preparation of proanthocyanjdin microcapsuies by piercing method [J]. Food Mach, 2012, 6: 214 218. [13],. [M]. :, 2006. Wu KG, Chai XH. Food microcapsulation [M].

王声文等 :GNC62 数控系统组态和设备调试设计 2 GNC62 系统组态设计原理 2 2 [1] 2 A I/O 1 293

王声文等 :GNC62 数控系统组态和设备调试设计 2 GNC62 系统组态设计原理 2 2 [1] 2 A I/O 1 293 工业技术创新工第 02 业技卷术第创 03 新期 Industrial 2015 年 Technology 6 月 Innovation Industrial Technology Innovation Vol.02 No.03 Jun.2015 GNC62 数控系统组态和设备调试设计王声文, 白彦庆, 刘庆宏, 孙振, 黄岩 (