Microsoft Word _排版-二校

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1 7 10 Vol. 7 No Journal of Food Safety and Quality Oct., 2016 郭去非, 周华生 *, 成恒嵩, 戴舒春 (, ) 摘要 : 目的方法 4, B 1 B 2 B 6 B 9 V C 5 结果 4 :, 90 W min;, 550 r/min min;, ( : : =100:200:200 U/g ) 45, ph h;, ~50, 50 ~80 4 结论 4 关键词 : ; ; ; ; Optimization of wall-broken techniques of micro-encapsulation health foods and determination of water-soluble vitamins GUO Qu-Fei, ZHOU Hua-Sheng *, CHENG Heng-Song, DAI Shu-Chun (Wuxi Giant Pharmaceutical Co.Ltd., Wuxi , China) ABSTRACT: Objective To optimize the wall-broken techniques of micro-encapsulation healthy foods and determine the content of water-soluble vitamins. Methods Four kinds of wall-broken techniques including ultrasound, homogenisation, enzymatic and microwave were optimized by orthogonal experiment, and 5 kinds of water-soluble vitamins such as B 1, B 2, B 6, B 9, V C were detected by ultra performance liquid chromatography (UPLC). Results The optimum conditions of 4 wall-broken methods were as follow: ultrasound technology: the power of 90 W, temperature of 65, time of 20 min; homogenisation: speed of 550 r/min, temperature of 60, time of 30 min; enzymatic method: enzyme amount (papain:amylase:acid lipase = 100:200:200 U/each sample), temperature of 45, ph 6.80, time of 6 h; microwave technology: 2 heating stages of room temperature~50, 50 ~80. The statistical analysis showed the vitamin content of each technique was non-significant..conclusion All of 4 kinds of wall-broken methods can be used to detect the water-soluble vitamins in micro-encapsulation healthy foods. KEY WORDS: micro-encapsulation; wall-broken technology; health food; water-soluble vitamins; ultra-high performance liquid chromatography * 通讯作者 :,,. wjzhhsh@126.com *Corresponding author: ZHOU Hua-Sheng, Associate Chief Pharmacist, Wuxi Giant Pharmaceutical Co., Ltd., Wuxi , China, wjzhhsh@126.com

2 10, : 引言, () 1~500 μm, [1,2] B C, ph, [3],,,,, 4,, 2 材料与方法 2.1 材料与仪器供试保健食品 () ( )(); ( ); () 试剂及仪器 ( B %)( B %)( B 6 100%) ( B %) ( C 96.9%)( Sigma ) 20 U/g 40 U/g 20 U/g( Novo Nordisk ) (, Fish Scientific ); (, ); Acquity UPLC ( UV-FLR, Waters ); Mars (); D-2000 (); Kq-2200DE ( ); AE-240 ( Mettler ) 2.2 实验方法, [4,5] 4 (),, ( ), B 1 B 2 B 6 B 9 V C 超声波破壁试验, : 3, L 9 (3 3 ), 1 Table 1 表 1 超声波破壁试验正交表 The orthogonal test of ultrasonic wall-broken A (W) B ( ) C (min) 匀浆搅拌破壁试验,, : 3, L 9 (3 3 ), 2 Table 2 表 2 匀浆搅拌破壁试验正交表 The orthogonal test of homogenisation wall-broken A (r/min) B ( ) C (min) 酶解破壁试验, : : =100:200:200 U/g : ph 3, L 9 (3 3 ) 3 Table 3 表 3 酶解破壁试验正交表 The orthogonal test of enzymatic wall-broken A ( ) B ph C (h) 微波破壁试验 3, 2, 4

3 Table 4 表 4 微波破壁实验条件表 The test conditions of microwave wall-broken ( ) (min) (min) ( ) (min) (min) ( ) (min) (min) 1 ~ ~ ~ ~ ~ ~ 超高效液相色谱法测定水溶性维生素 B 1 B 2 B 6 B 9 V C [5] 0.05 mol/l, 3 结果与分析 3.1 超声波破壁技术 3, 5 Table 5 表 5 超声波破壁正交试验结果 The orthogonal results of ultrasonic wall-broken A B C B 1 (W) ( ) (min) mg/100 g K K K R (R), B 1 A C B, A 3 B 2 C 3, 90 W, 65, 20 min, B mg/100 g 3.2 匀浆搅拌破壁技术 3, 6 Table 6 表 6 匀浆搅拌破壁正交试验结果 The orthogonal results of homogenisation wall-broken A B C B 2 (r/min) ( ) (min) mg/100 g K K K R (R), B 2 A B C A 2 B 3 C 1, 550 r/min, 60, 30 min, B mg/100 g 3.3 酶解破壁技术, ph 3, 7

4 10, : 4213 Table 7 表 7 酶解破壁正交试验结果 The orthogonal results of enzymatic wall-broken A B ph C B 6 ( ) (h) mg/100 g K K K R (R), B 6 B A C A 2 B 2 C 3, 45, ph 6.80, 6 h, B mg/100 g 3.4 微波破壁技术 3 8 Table 8 表 8 微波破壁试验结果 The results of microwave wall-broken (mg/100 g) B B B B V C ,,, 1,,, ; 2,, B 1 B 2 B 6, ; 3,, 3.5 不同破壁技术对不同微囊化保健食品中水溶定性维生素的测定, 4, 5, 9 Table 9 表 9 不同破壁技术测定保健食品中水溶性维生素的结果 (n=4) Results of water-soluble vitamins in health foods by different wall-broken techniques (n=4) (mg/100 g) RSD/% B B B B V C B B B B V C B B B B V C B B B B V C

5 , 4 RSD : B %~4.55%, B %~7.32%, B %~7.26%, B %~9.34%, V C 0.76%~5.95%,,, 4 4 讨论,, 4.1 提取液的优化 B 1 B 2 B 6 B 9 V C, [6], (0.01~0.1 mol/l), [7,8], [9] ( ::0.25 mol/l ::7% =70:30:1.5:1.0:0.25, V:V:V:V:V),, B 1 B 2 B 6 ; [10] ; [5] 0.01 mol/l,, 0.05 mol/l ph 6.80,, B 1 B 2 B 6 V C, B 提取温度的优化, 4 65, 60, 45, ~50, 50~80,, 4.3 测定方法的优化, [11], [12,13],, [14],, -, 6 min, B 2, 4.4 几种破壁方法的比较 4,,, ;, ;,, 5 结论, 4, 参考文献 [1],, 堃. [J]., 2009, 28(7): Gao HS, Hao YZ, Li XK. The research of vitamin microcapsule [J]. Herald Med, 2009, 28(7): [2] Gharsalllaoui A, Roudaut G, Chambin O, et al. Applications of spray-drying in microencapsulation of food ingredients [J]. Food Res Int, 2007, 40: [3],. [M]. :, Wu KG, Chai XH. Food microencapsulation technology [M]. Beijing: China Light Industry Press, [4],,. [M]. :, Yang H, Zhong B, Liu QS. Application of mathematical statistics [M]. Beijing: Tsinghua University Press, [5],,,. [J]., 2012, 28(7): Pu MQ, Zhou HS, Cheng HS, et al. Determination of water-soluble vitamins in health foods by UPLC [J]. Mord Food Sci Technol, 2012, 28(7): [6],,. [M]. :, Wang Z, Xu SY, Tang J. Food Chemistry [M]. Beijing: China Light Industry Press, 2012 [7] Chuney K, Tinger K, Analy L. Determination of water soluble vitamins [J]. Chromatogr, 1998, 31(15): [8] Hou W, Wang E. Determination of water soluble vitamins by liquid chromatography with parallel dual-eletrodechemical detector [J]. Talata, 2002, 37: [9],. RP-HPLC V B1 V B2 V B6 [J]., 2005, 9(10): Zhang LL, Zhou HS. Determination of V B1, V B2, V B6 in golden partner vitamins tablet by double channel RP-HPLC [J]. Anhui Med Pharm J, 2005, 9(10): [10],,. RP-HPLC [J]., 2006, 10(1): Zhang LL, Zhou HS, Ye KH. Determination of folic acid in golden partner vitamins tablet by RP-HPLC [J]. Anhui Med Pharm J, 2006, 10(1): [11] GB/T

10, : 4215 [S]. GB/T 5009.197-2003 Determination of thiamine hydrochloride, pyridoxine hydrochloride, niacin, niacinamide and caffeine in health foods [S]. [12] Chandra-Hioe MV, Bucknall MP, Arcot J.

Anal Bioanal Chem, 2011, 401(3): 1035 1042. [13],,,. 9 [J]., 2014, 5(3): 899 904. Ren DD, Xie YF, Liu JJ, et al.

6 10, : 4215 [S]. GB/T Determination of thiamine hydrochloride, pyridoxine hydrochloride, niacin, niacinamide and caffeine in health foods [S]. [12] Chandra-Hioe MV, Bucknall MP, Arcot J. Folate analysis in foods by UPLC-MS/MS: development and validation of a novel,high throughput quantitative assay; folate levels determined in Australian fortified breads [J]. Anal Bioanal Chem, 2011, 401(3): [13],,,. 9 [J]., 2014, 5(3): Ren DD, Xie YF, Liu JJ, et al. Simultaneous determination of nine water-soluble vitamins in foods by high performance liquid chromatography [J]. J Food Saf Qual, 2014, 5(3): [14],,. B [J]., 2009, 25(7): Zhang LL, Zhou HS, Cheng HS. Determination of vitamins B in foods by reversed-phase ion-pair chromatography [J]. Mord Food Sci Technol, 2009, 25(7): 作者简介 ( 责任编辑 : 姚菲 ) 郭去非, 助理工程师, 主要研究方向为药品保健食品质量分析与研究 @163.com 周华生, 副主任药师, 主要研究方向为药品保健食品研制与质量分析 wjzhhsh@126.com

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10