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1 6 6 Vol. 6 No 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 :,,, 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. lijian485247@63.com

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

2 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] 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 ; ml C 7 H 6 O 5 0 ml, mg/l; 37.5 g Na 2 CO 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 单因素试验 () :20(m:V) 5 g ()

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.

3 6, : %, 800 W, 60 s,, AP (2) :20(m:V) 5 g 50%, 800 W, 20% 40% 60% 80% 00%, 60 s,, AP (3) :20 (m:v) 5 g 50%, 80%, s, AP (4) 5 g, :0 : :2 :3 :4 :5 (m:v) 50%, 80%, 70 s,, AP 微波辅助法提取苹果多酚的工艺优化试验,,, ( A) ( B) ( C)3 Design Expert 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, A /% B /W C /s 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,,

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.

4 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, Fig. 4 4 Effect of the ratio of material to liquid on extraction rate of apple polyphenols 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,

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.

5 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 < A(%) < B(W) C(s AB AC BC < B < < A C 残差失拟值纯误差总和 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

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.

6 (mg/g)= a b C AB BC0.08A 2 0.2B C 2, r 2 =0.9995,, : W, s, 50.64%, :4 (m:v), 9.92 mg/g, W 640 W 4 结论 DE8.0.6 :,,, 0~0.02 mg 2~6 mg/g,,,,,, : 640 W, 70 s, 50%, :4 (m:v),, 9.92 mg/g 参考文献 []. : 7 [J]., 2000, 3(3): Chen CS. Global information on cereals oils and foods: Seventh nnutrient Plant polyphenol function and its exploitation and Utilization [J]. Cereals Oils, 2000, 3(3): [2] Brave L. Polyphenols: Chemistry dietary source, metabolism, and nutritional significance [J]. Nut Rev, 998, 56(): [3],,,. [J]., 20, 32(2): Tian LL, Liu JL, Zheng ZW, et al. Research progress of compounds and physiological functions of apple polyphenol [J]. Sci Teclnol Food Ind, 20, 32(2): [4] Borneman Z, Gokmen V, Nijhuis H. Selective removal of polyphenols and brown colour in apple juices using PES/PVP membranes in a single ultrafiltration process[j]. Separ Purif Technol, 200, 03(22): [5]. [J]., 2002, 9(0): 3. Shou BQ. Eat more apples a lot of benefits [J]. Health Expo, 2002, 9(0): 3. [6],,,. [J]., 203, 34(20): Wang J, Gao Y, Zhao YM, et al. Determination of polyphenols in apple pericarp and apple grunt [J]. Food Res Devel, 203, 34(20): [7]. [D]. :, Yang JR. Establishment of HPLC detection method for apple polyphenols [D]. Jinan: Shandong University, 2006 [8],,,. [J]., 2005, 2(09): Luan Y, Ji BP, Jiang H, et al. Factors influenced the extraction of apple polyenols by organic regents [J]. Food Sci, 2005, 2(09): [9],. [J]., 200, 6(0): Xu JY, Wang Y. Discussion on extraction of apple polyphenols [J]. Value Eng, 200, 6(0): [0],,. [J]., 20, 32(6): Wang Y, Zhang YG, Dai HY. Ultrasonicassisted extraction and stability of flavonoids from apple peel [J]. Food Sci, 20, 32(6): []. [D]. :, Guo J. Study on the extraction, purification and efficacy of apple polyphenols from apple residues [D]. Zhengzhou: Henan Agricultural University, [2]. [D]. :, 204. Li Z. Study on extraction, purification and antioxidant activity of polyphenols from apple peel [D]. Beijing: Chinese Academy of Agricultural Science, 204 [3],,,. [J]., 2007, 29(05): Jin Y, Sun AD, Hu XD, et al. Ultrasonic extraction and antioxidant activities of apple polyphenols [J]. J Beijing Forestry Univ, 2007, 29(05): [4],,. [J]., 202, 33(2): Zhou LP, Yang RH, Zhang Y. Optimization of apple polyphenols

Global information on cereals oils and foods: Seventh nnutrient Plant polyphenol function and its exploitation and Utilization [J]. Cereals Oils, 2000, 3(3): 40 42. [2] Brave L.

7 6, : 2035 extraction with grind balls by response surface methodology [J]. Food Ind Technol, 202, 33(2): [5],,,. [J]., 202, 28(25): Wei Y, Ji BP, Zhou F, et al. Technology optimization of polyphenols extraction from apple pomace [J]. Transact Chin Soc Agric Eng, 202, 28(25): [6]. [J]. ( ), 204, (5): 9 2. Chen BH. Optimized technology of extracting polyphenol from apple pomace with microwave [J]. Acad Period Farm Prod Proc, 204, (5): 9 2. [7],,,. [J]., 2006, 7(06): Ai ZL, Guo J, Wang YH, et al. Microwaveassisted extraction technique of apple polyphenols in apple pomace [J]. Transact CSAE, 2006, 7(06): [8]. [D]. :, its antioxidant in apple residue [D]. Zhengzhou: Henan Agricultural University, [9],,,. Folin [J]., 2008, 25 (): Li J, Nie JY, Li HF, et al. Determination conditions for total polyphenols in fruits and its deriv products by Folinphenol methods [J]. J Fruit Sci, 2008, 25 (): [20]. [D]. :, 203. Cao ZM. Study on the extraction and separation of polyphenols from the myrtle and its fresh keeping [D]. Zhanjiang: Guangdong Ocean University, 203. 作者简介 ( 责任编辑 : 杨翠娜 ) 李健, 本科, 教授, 主要研究方向为食品化学 lijian485247@63.com Li Q. Study on microwave assisted extraction of polyphenols and

Optimized technology of extracting polyphenol from apple pomace with microwave [J]. Acad Period Farm Prod Proc, 204, (5): 9 2. [7],,,. [J]., 2006, 7(06): 88 9. Ai ZL, Guo J, Wang YH, et al.

H 2 SO ml ml 1. 0 ml C 4. 0 ml - 30 min 490 nm 0 ~ 100 μg /ml Zhao = VρN 100% 1 m V ml ρ g

H 2 SO ml ml 1. 0 ml C 4. 0 ml - 30 min 490 nm 0 ~ 100 μg /ml Zhao = VρN 100% 1 m V ml ρ g 16 6 2018 11 Chinese Journal of Bioprocess Engineering Vol. 16 No. 6 Nov. 2018 doi 10. 3969 /j. issn. 1672-3678. 2018. 06. 004 1 2 1 1 1. 330200 2. 330006 4 Box-Behnken 1 25 g /ml 121 92 min 2 6. 284%