<4D F736F F D D D7A3BAE9D1DE2DB6FED0A32DD3D0B8C4B6AF20B3F B2BBD2AAB6AFB0E62E646F63>

Size: px

Start display at page:

Download "<4D F736F F D D D7A3BAE9D1DE2DB6FED0A32DD3D0B8C4B6AF20B3F B2BBD2AAB6AFB0E62E646F63>"

帜洛蒋
7 years ago
Views:

1 5 11 Vol. 5 No Journal of Food Safety and Quality Nov., * 祝洪艳, 林海成, 杨鹤, 王国丽, 赵岩, 郜玉钢, 张连学 (, ) 摘要 : 目的方法, -, SAS, 结果 14 75% 2, 2 h mg/g 结论 -,,,, 关键词 : ; A; ; - Optimization of reflux extraction of jujuboside from semen ziziphi spinosae by central composite design-response surface methodology ZHU Hong-Yan, LIN Hai-Cheng, YANG He, WANG Guo-Li, ZHAO Yan, GAO Yu-Gang, ZHANG Lian-Xue * (College of Chinese Medicinal Materials, Jilin Agricultural University, Changchun , China) ABSTRACT: Objective The extraction of jujuboside from semen ziziphi spinosae was optimized. Methods The content of jujuboside was detected by ultraviolet and visible spectrophotometry, and central composite design (CCD)-response surface methodology was used to study the effects of ethanol concentration, ethanol dosage and extraction time as well as their interactions on the content of jujuboside. A predictive model was developed by SAS software, and the optimum extraction conditions were determined by response surface analysis. Results The optimum reflux extraction conditions were 14 times of 75% ethanol extracted 2 h for 2 times. The average content of jujuboside was mg/g. Conclusion CCD-response surface methodology for optimizing the reflux extraction press of jujuboside was reliable, and the detected content of jujuboside closed to the predictive value. The predicted extraction process was stabled, and it could be used to direct the industria- 基金项目 : (2011BAI03B010602) (2012ZX ) ( JC) ( ) ( ) Fund: Supported by National Key Technology Support Program (2011BAI03B010602), National Science and Technology Major Project (2012ZX ), the Project Development Plan of Science and Technology of Jilin Province ( JC), National Public Scientific Research ( ) and the Project of Education Fund of Jilin Province ( ) * 通讯作者 :,,, zlxbooksea@163.com *Corresponding author: ZHANG Lian-Xue, Professor, College of Chinese Medicine Material in Jilin Agricultural University, Changchun , China. zlxbooksea@163.com

2 11, : lized extraction of jujuboside. KEY WORDS: jujuboside; jujuboside A; extraction; central composite design -response surface methodology 1 引言 (Semen ziziphi spinosae) [Ziziphus jujuba Mill. var. spinosa (Bunge) Hu ex H.F. Chou], [1],, [2,3] [4], [5,6], [7-10],,,,, 2 材料与方法 2.1 材料与仪器,, [Ziziphus jujuba Mill. var. spinosa (Bunge) Hu ex H.F. Chou] ; A (, : ); (, ) UV-6100 ( ); BS210S ( SARTORIUS ); RE-52AA ( ); SHB-Ⅲ ( ),, ( 99.5%, ); ( 99.7%, ); ( 99.0%, ); ( 60~90, ); 2.2 实验方法酸枣仁总皂苷含量测定 (1) 1 A 2.20 mg, 10 ml, 0.22 mg/ml 2 ( 40 ), 6 h,, 5.0 g,,,,,,,,, 10 ml, (2) A ml, 10 ml,, 5% 0.20 ml 0.80 ml,, min, 5 min, 5 ml,,, UV nm [11] (mg/ml),, Y=26.034X , R 2 = ~ mg/ml (3), [(2) ],, (mg/g) 酸枣仁总皂苷提取单因素实验 (1) 6, 70%, 30 min; ( 3:1) ph 4.5, 45 5 h [12] ; 70%, 1 h; 70%, 6 70% ;, 1 h

3 3720 5,, (2), 30% 50% 70% 80% 95%, 10:1, 2 h, (3), 70%, 8:1 10:1 12:1 15:1 20:1, 2 h, (4), 70%, 10:1, h,, (5), 70%, 10:1, 1 h, , 酸枣仁总皂苷提取工艺的中心组合 - 响应面分析实验设计, (X 1 ) (X 2 ) (X 3 ) ( 1),, SAS,,, Origin, 表 1 酸枣仁总皂苷提取工艺的中心组合实验设计因素水平表 Table 1 Factors and levels of CCD design for jujuboside from semen ziziphi spinosae X 1 (%) X 2 (ml/g) X 3 (h) 酸枣仁皂苷最优提取工艺的验证实验 3,,, 3 结果与分析 3.1 酸枣仁总皂苷提取单因素实验不同提取方法对酸枣仁总皂苷含量的影响, 1 1, 70%, [12],,,,,,, Fig. 1 1 (n=3) Effect of different extraction method on the content of jujuboside (n=3)

4 11, : 乙醇浓度对酸枣仁总皂苷含量的影响, 2 2, 70%, ; 70%, ; 70%,,,, 50%~80% 液固比对酸枣仁总皂苷含量的影响 70%, 3 3,, 8:1 10:1, ; 10:1,,, 10:1~15: 提取时间对酸枣仁总皂苷含量的影响 70%,, 4 Fig. 2 2 (n=3) Effect of ethanol concentration on the content of jujuboside (n=3) Fig. 3 3 (n=3) Effect of solvent-to-solid ratio on the content of jujuboside (n=3) Fig. 4 4 (n=3) Effect of extraction time on the content of jujuboside (n=3)

5 ,, 2 h,, 1~2 h 提取次数对酸枣仁总皂苷含量的影响 70%, 5 5, 2 1, 3 4,,, 酸枣仁皂苷提取的中心组合设计实验结果 SAS ( 2),, : Y= X X X X X 2 X X X 3 X X 3 X X 2 3 ; 3, 4, 5 Fig. 5 5 (n=3) Effect of extraction times on the content of jujuboside (n=3) 表 2 酸枣仁总皂苷的提取工艺中心组合设计实验设计及结果 Table 2 CCD matrix and results of jujuboside from semen ziziphi spinosae X 1 (%) X 2 (ml/g) X 3 (h) (mg/g) (mg/g) S1 0(65.0) 0(12.5) 0(1.5) S S S4 1(73.9) 1(14.0) 1(1.8) S (1.2) S6 1 1(11.0) S S8 1(56.1) S S S S (50.0) S (80.0) S (10.0) S (15.0) S (1.0) S (2.0)

6 11, : Table 3 表 3 回归系数显著性检验表 Significance test of each coefficient in the developed regression model t P X * X X X ** X 2 X ** X ** X 3 X X 3 X X : P<0.05, * ; P<0.01, ** Table 4 表 4 回归模型方差分析 Analysis of variance for the developed regression model F P < ** < ** ** * Table 5 表 5 模型岭脊回归分析 Ridge analysis for the developed regression model X 1 X 2 X

7 Fig. 6 Response surface and contour lines of the content of Jujuboside

8 11, : , (X 1 ) (P<0.05);, (X 2 ) (X 1 ) (P<0.01);, (X 1 ) (X 2 ) (P<0.01), (X 3 ), (X 1 ) (X 2 ), P>0.3, : Y= X X X X 2 X X 2 2,,, P<0.3, : Y= X X X X X 2 X X X 3 X X 3 X X 2 3 4, (P<0.01), (P<0.05) R 2 =0.9859, P>0.05, 5, 75.0%, 13.9 ml/g, 2, 1.7 h, mg/g 3.3 酸枣仁皂苷提取的响应面优化与预测分析, Origin ( 6), ( 0), 6, (X 1 ) (X 2 ) (X 3 ),,, : (X 1 )75%~80%; (X 2 )14~15 ml/g; (X 3 )1.9~2 h, 75%, 14:1, 2, 2 h 3.4 优选酸枣仁皂苷提取工艺的验证实验, 75%, 14:1, 2, 2 h, 3, mg/g, mg/g,, 4 讨论 [13],, 82.3%, 1:22.3, h,,,,, 75%, 14:1, 2, 2 h, 3.426%, [14] [15],,, 参考文献 [1]. (2010 Ⅰ )[M]. :, 2010: Pharmacopoeia Commission of People s Republic of China. Pharmacopoeia of people s republic of China: 2010 Part Ⅰ[M]. Beijing: Chinese Medical Science and Technology Press, 2010: [2]. 60 [J]., 2014, 28(6): 53. Kang J. 60 cases of insomnia treatment efficacy suanzaoren decoction [J]. J Pract Trad Chin Int Med, 2014, 28(6): 53. [3]. [J]., 2014, 29(1): Ding DZ. Examples of suanzaoren decoction on mental illness [J]. China J Trad Chin Med Pharm, 2014, 29(1): [4],,. [J]., 2013, 28(4): Zhang XW, Zhao Q, Wei YH. Research progress of biology characteristics and chemical constituents of semen ziziphi spinosae [J]. China J Chin Med, 2013, 28(4):

9 [5] Cao JX, Zhang QY, Cui S Y, et al. Hypnotic effect of jujubosides from semen ziziphi spinosae [J]. J Ethnopharm, 2010, 130: [6] You ZL, Xia Q, Liang FR, et al. Effect on the expression of GABA A receptor subunits by jujuboside A treatment in rat hippocampal neurons [J]. J Ethnopharm, 2010, 128: [7],,,. [J]., 2011, 17(11): Wang Y, Wei N, Xu S, et al. Optimization of water extraction technology of ziziphi spinosae Semen by orthogonal design with multitargets [J]. J Hainan Med Univ, 2011, 17(11): [8],,,. A B [J]., 2012, 40(9): Wu CQ, Chen GH, Guo DS, et al. Extraction technology of jujuboside A and jujuboside B by ultrasonic reflux method [J]. Jiangsu Agric Sci, 2012, 40(9): [9],. A [J]. ( ), 2011, 32(5): Zhang X, Chen FS. Optimization of extraction of jujuboside A from semen ziziphi spinosae [J]. J Henan Univ Technol(Nat Sci Ed), 2011, 32(5): [10],,,. [J]., 2005, 30(10): Wang XL, Zhang YJ, Chen MX, et al. Optimization study on extraction technology of the seed of ziziphus jujube var. spinosa by orthogonal design with multi-targets [J]. China J Chin Mater Med, 2005, 30(10): [11]. [D]. :, 2005: Yao Y. Study on the extraction technology and composition of semen ziziphi spinosae [D]. Beijing: Capital Normal University, 2005: [12],,,. [J]., 2008, 42(9): Zhang MC, Xie JB, Zhang JY, et al. Optimum extraction conditions of ziziphus jujuba with complex phosphoesterasum [J]. Shanghai J Trad Chin Med, 2008, 42(9): [13]. [J]., 2013, 34(10): Ye ZM. Response surface optimization extraction of saponins from semen ziziphi spinosae [J]. Food Ind, 2013, 34(10): [14],,,. [J]. ( ), 2009, 37(10): Li Y, Jin AX, Liang ZS, et al. Optimization of the extraction technics of total flavones from semen ziziphi spinosae and its mathematical model [J]. J Northwest A F Univ (Nat Sci Ed), 2009, 37(10): [15]. [J]., 2013, 34(16): Zhao JC. Optimization of protein extraction from ziziphi spinosae semen by response surface methodology [J]. Food Sci, 2013, 34(16): 作者简介 ( 责任编辑 : 杨翠娜 ) 祝洪艳, 讲师, 博士, 主要研究方向为中药研究开发 popzhy@163.com 张连学, 教授, 博导, 主要研究方向为药用植物栽培与加工 zlxbooksea@163.com

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%