6 6 Vol. 6 No. 6 205 6 Journal of Food Safety and Quality Jun., 205 李 健 *, 安 廷, 刘 宁, 刘 雅 南, 宋 秀 超 (,, 50076) 摘 要 : 目 的 方 法,,,, 结 果 : > > : 50% 640 W 70 s :4(m:V), 9.92 mg/g 结 论,, 关 键 词 : ; ; ; Optimization of the extraction of apple polyphenols by response surfacemicrowave methodology LI Jian *, AN Ting, LIU Ning, LIU YaNan, SONG XiuChao (Key Laboratory for Food Science and Engineering of Heilongjiang Province, College of Food Engineering, Harbin University of Commerce, Harbin 50076, China) ABSTRACT: Objective To obtain the optimum extraction condition of polyphenols contained in apple by microwaveassisted method. Methods Polyphenols in apple were extracted by microwaveassisted method. The effect of power, extraction time, solidliquid ratio and ethanol concentration on the extraction rate of polyphenols was discussed under the influence of microwave. Based on single factor experiments, the optimum extraction was determined by response surface analysis. Results The yield of apple polyphenols was affected by various factors in a descending order as: microwave power, ethanol concentration, microwave extraction time and solidliquid ratio. The optimum extraction condition was as follow: ethanol concentration 50%, microwave power 640 W, extraction time of 70 s, solidliquid ratio :4 (m:v), and the extraction rate of polyphenols was up to 9.92 mg/g. Conclusion From the experimental results, microwaveassisted method is fast and effective, safe and convenient to extract polyphenols contained in apple and can obtain extraction rate better. KEY WORDS: apple polyphenols; microwave assisted; extraction condition; response surface analysis 基 金 项 目 : (252z009) (25499) Fund: Supported by the Technology Research Project of Heilongjiang Province Education Department (252z009) and the Project of Heilongjiang Provincial Education Department (25499) * 通 讯 作 者 :,,, Email: lijian485247@63.com *Corresponding author: LI Jian, Professor, College of Food Engineering, Harbin University of Commerce, No.38 Tongda Street, Daoli District, Harbin 50076, China. Email: lijian485247@63.com
2030 6 引 言 (apple polyphenols, AP),,, AP, [,2] AP, AP E C,, [35], [6] FolinCiocaileu ; [7] ; : [8,9],,,,, [0] [] [2] ; [3] [4], [58], 2 材 料 与 方 法 2. 实 验 材 料 ( ) 2.2 试 剂 与 仪 器 ( 99%, ); (, ); (, ); (, ); (CH283V, ); (BP22S, ); (HR2004, ); (G80F23DCN3LF7, ); (500B, ); (SHB Ⅲ, ) 2.3 实 验 方 法 2.3. 苹 果 多 酚 提 取 的 工 艺 流 程 cm 3 5~8 s [9] 2.3.2 苹 果 多 酚 定 量 的 测 定 福 林 酚 法 (C 7 H 6 O 5 ), 0 mg C 7 H 6 O 5 0 ml ; 0 0. 0.2 0.3 0.4 0.5 0.6 ml C 7 H 6 O 5 0 ml, 0 20 30 40 50 60 mg/l; 37.5 g Na 2 CO 3 250 ml 500 ml,, 500 ml ; : ml C 7 H 6 O 5 0 ml, 5 ml ml 4 min 3 ml 50g/L Na 2 CO 3, 2 h, A 765 nm 3,, Y=0.026X0.0236, r 2 =0.9952, () [20] C V N T(mg/g)= M 000 : C, μg/ml; V, ml; M, g; N,, ; 000 μg mg 2.3.3 单 因 素 试 验 () :20(m:V) 5 g 0 20 30 40 50 60 70 80 90 ()
6, : 203 00%, 800 W, 60 s,, 2.3.2 AP (2) :20(m:V) 5 g 50%, 800 W, 20% 40% 60% 80% 00%, 60 s,, 2.3.2 AP (3) :20 (m:v) 5 g 50%, 80%, 0 20 30 40 50 60 70 80 90 00 s, 2.3.2 AP (4) 5 g, :0 : :2 :3 :4 :5 (m:v) 50%, 80%, 70 s,, 2.3.2 AP 2.3.4 微 波 辅 助 法 提 取 苹 果 多 酚 的 工 艺 优 化 试 验,,, ( A) ( B) ( C)3 Design Expert 8.0.6 3 3 表 微 波 辅 助 提 取 苹 果 多 酚 因 素 水 平 Table Microwave assisted extraction of apple polyphenols reference factors and levels Fig. Effect of ethanol concentration on apple polyphenol content, (AP),, 50%, AP, AP,, AP, AP, 50% 3..2 微 波 功 率 对 苹 果 多 酚 含 量 的 影 响 50%, :20 (m:v), 60 s, 2 0 + A /% B /W C /s 40 50 60 480 640 80 60 70 80 3 结 果 与 讨 论 3. 单 因 素 试 验 3.. 乙 醇 浓 度 对 苹 果 多 酚 含 量 的 影 响, 00% 30%,,, Fig. 2 2 Effect of microwave power on the apple polyphenols content 2, AP,,
2032 6,,,,, AP 640 W, AP 3..3 微 波 提 取 时 间 对 苹 果 多 酚 含 量 的 影 响 50% 640 w :20 (m:v), 3 4,,,, :4(m:V),,,, :4(m:V) 3.2 响 应 曲 而 优 化 试 验 3.2. 回 归 模 型 的 建 立 及 统 计 检 验 2, DesignExpert 8.0.6( DE 8.0.6), 3 表 2 微 波 辅 助 提 取 苹 果 多 酚 响 应 面 分 析 试 验 结 果 Table 2 Microwave assisted extraction of apple polyphenols reference response and the analysis of experimental results A /% B /W C /s mg/g Fig. 3 3 Effect of time on Extraction of apple polyphenol content 3,,,, ;,,, AP, 70 s,, 70 s 3..4 料 液 比 对 苹 果 多 酚 提 取 得 率 的 影 响 50% 640 W 70 s, 4 0 6.38 2 0 6.22 3 0 6.2 4 0 7.3 5 0 6.4 6 0 6.92 7 0 6.42 8 0 6.23 9 0 6.2 0 0 6.93 0 0 0 9.96 2 0 0 0 9.92 3 0 0 0 9.9 4 0 6.56 5 0 0 0 9.88 6 0 7.32 7 0 0 0 9.92 Fig. 4 4 Effect of the ratio of material to liquid on extraction rate of apple polyphenols 3.2.2 微 波 辅 助 法 提 取 苹 果 多 酚 各 因 素 间 的 交 互 作 用 640 W, AP 5,, 70 s, 6,
第6期 李 2033 健, 等: 微波辅助响应曲面法优化提取苹果多酚工艺 Table 3 表 3 回归方程系数显著性检验表 regression equation coefficient significant test table 变异来源 平方和 自由度 均方 F值 P值 模型 0.4 9 0.046 553.59 < 0.000 A(%) 0.002520 0.002520 85.67 < 0.000 B(W) 0.000000250 0.000000250 0.004249 0.9499 C(s 0.0007 0.0007 5.82 0.0467 AB 0.000440 0.000440 4.89 0.0626 AC 0.000 0.000 0.000.0000 BC 0.0000002500 0.0000002500 0.008497 0.929 2 0.08 0.08 2752.3 < 0.000 B2 0.020 0.020 692.84 < 0.000 2 0.084 0.084 2842.6 < 0.000 A C 残差 0.0002059 9 0.00002942 失拟值 0.000707 5 0.00005692 6.47 0.055 纯误差 0.00003520 4 0.000008800 总和 0.4 6 r2=0.9995, Adjr2=0.9989, Prer2=0.9932, Adeq Precision=9.938 一定范围内与提取温度的上升和乙醇浓度的提高呈 正比, 温度过高 乙醇浓度过大后, 多酚的含量减少 乙醇浓度对多酚提取率的影响小于微波功率 固定乙醇浓度为 50%, 提取时间与功率对苹果 多酚提取率的交互作用如图 7 所示, 微波功率升高 时间延长, 多酚提取率逐渐增加后减少 微波功率对 多酚提取率的影响大于微波时间 图 5 乙醇浓度与微波处理的时间对多酚提取率的交互影响 Fig. 5 Interactive effects of ethanol concentration and rate of microwave treatment time on the extraction of polyphenols 图 7 微波时间与微波功率对多酚提取率的交互影响 Fig. 7 The interaction effect of the rate of microwave time and microwave power on the extraction of apple polyphenols 利用 DE8.0.6, 通过响应面法优化微波辅助提 图 6 乙醇浓度与微波功率对多酚提取率的交互影响 Fig. 6 Interactive effects of ethanol concentration ratio and microwave power on the extraction of polyphenols 取苹果中多酚的工艺, 由表 3 可知, P 值小于万分之 一, 表明该二次多项回归模型高度显著, 依照列出 的表 3 建立苹果多酚得率的二次多项数学模型 : 多
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