Response Surface Optimization on Subcritical Water Extraction of Polysaccharides from Pitaya Stems
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摘要:
目的 为了开发先进的火龙果茎多糖提取方法,采用响应面实验优化亚临界水法提取火龙果茎多糖的工艺,为火龙果茎多糖的亚临界水提取研究提供参考。 方法 在单因素试验基础上,以火龙果茎为原料,采用苯酚一硫酸法进行火龙果茎多糖含量的测定,用超声波预处理辅助,在温度、时间、液料比、pH等4个条件的影响下用响应面法对多糖的提取率进行了分析。 结果 亚临界水提取火龙果茎多糖的最佳条件为:提取温度144 ℃,提取时间19 min,液料比(v/mL∶m/g)为31∶1,pH值5.9;优化条件下火龙果茎多糖的提取率是26.47%。 结论 建立的数学模型可对火龙果茎多糖的提取工艺参数进行分析和预测,采用响应面法优化火龙果茎多糖提取工艺具有可行性。因此,亚临界水法提取火龙果茎多糖具有广阔的应用前景。 Abstract:Objective A subcritical water extraction method was optimized by response surface experiments to extract polysaccharides from pitaya stems. Method On the basis of a single factor test, pitaya stems were extracted using phenol-sulfuric acid to determine the polysaccharide content. To optimize the subcritical water extraction process assisted by ultrasonic pretreatment, water temperature, extraction time, liquid-to-material ratio, and pH were used against polysaccharide extraction rate in a response surface experiment. Result The optimized processing conditions included the applications of water at pH 5.9 and 144 ℃ with a liquid-to-material ratio of 31:1 (mL:g) to extract for 19 m. A polysaccharide extraction rate of 26.47% was achieved. Conclusion The established method appeared adequate for polysaccharide extraction from pitaya stems, and the mathematical model obtained be used to analyze and predict the process parameters. -
Key words:
- Subcritical water /
- extraction rate /
- polysaccharide /
- response surface method
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图 5 各因素交互作用的响应面图
注:A-时间和温度对多糖提取率影响的曲面图;B-液料比和温度对多糖提取率影响的曲面图;C-pH和温度对多糖提取率影响的曲面图;D-液料比和时间对多糖提取率影响的曲面图;E-时间和pH对多糖提取率影响的曲面图;F-液料比和pH对多糖提取率影响的曲面图。
Figure 5. Response plot of interactions between factors
Note: A: surface plot of time and temperature effects on polysaccharide extraction rate; B: surface plot of liquid-to-material ratio and temperature effects on polysaccharide extraction rate; C: surface plot of pH and temperature effects on polysaccharide extraction rate; D: surface plot of liquid-to-material ratio and time effects on polysaccharide extraction rate; E: surface plot of time and pH effects on polysaccharide extraction rate; F: surface plot of liquid-to- material ratio and pH effects on polysaccharide extraction rate.
表 1 响应面分析试验因素与水平
Table 1. Response surface test factors and levels
水平
LevelA温度
Temperature/℃B时间
Time/minC液料比
Liquid-to-material ratio/
(mL·g−1)D pH 1 160 25 50 6 0 150 20 40 5 −1 140 15 30 4 表 2 响应面试验设计及结果
Table 2. Design and results of Box-Behnken experiment
序号
No.A温度
Temperature/
℃B时间
Time/
minC液料比
Liquid-to-material
ratio/(mL·g−1)DpH Y提取率
Extraction
rate/%1 0 0 0 0 20.57 2 −1 1 0 0 21.62 3 −1 −1 0 0 22.52 4 −1 0 0 −1 19.42 5 0 −1 1 0 20.69 6 1 0 1 0 10.39 7 0 1 −1 0 16.78 8 0 0 1 −1 17.98 9 −1 0 1 0 17.17 10 0 0 0 0 22.12 11 0 1 0 1 14.62 12 1 0 0 −1 12.48 13 0 −1 0 1 18.48 14 1 1 0 0 8.74 15 1 0 −1 0 14.21 16 0 0 0 0 23.65 17 −1 0 0 1 24.62 18 0 0 1 1 20.12 19 0 0 −1 1 25.04 20 0 0 0 0 22.62 21 1 −1 0 0 16.68 22 0 −1 −1 0 25.67 23 0 0 −1 −1 23.46 24 0 1 1 0 12.98 25 0 0 0 0 20.78 26 1 0 0 1 14.76 27 0 −1 0 −1 22.01 28 0 1 0 −1 17.00 29 −1 0 −1 0 26.43 表 3 回归模型方差分析结果
Table 3. Analysis of variance for fitted regression model
项目
Source平方和
Sum of
squares自由度
df均方
Mean
squareF P 显著性
Signi
ficanceModel 527.00 14 39.14 9.24 <0.0001 ** A-温度 247.61 1 247.70 58.46 <0.0001 ** B-时间 98.10 1 98.1 23.15 0.0003 ** C-液料比 86.73 1 86.73 20.47 0.0005 ** D-pH 2.33 1 2.33 0.55 0.4704 AB 12.39 1 12.39 2.92 0.1093 AC 7.40 1 7.40 1.75 0.2076 AD 2.13 1 2.13 0.50 0.4898 BC 0.35 1 0.35 0.082 0.7786 BD 0.33 1 0.33 0.078 0.7841 CD 0.078 1 0.078 0.019 0.8937 A2 72.30 1 72.30 17.06 0.0010 ** B2 32.69 1 32.69 7.71 0.0148 * C2 2.36 1 2.36 0.56 0.4675 D2 3.36 1 3.36 0.79 0.3882 残差 Residual 59.32 14 4.24 失拟项 Lack of fit 52.68 10 5.27 3.17 0.1385 误差项 Pure error 6.64 4 1.66 注:*表示显著影响(P<0.05),**表示极显著影响(P<0.01)。
Note:* :significant influence(P<0.05),** : extremely significant influence(P<0.01). -
[1] 陈冠林. 红肉火龙果色素提取、纯化、抗氧化及其调血脂作用的研究[D]. 广州: 广东药学院, 2013.CHEN G L. Studies on extraction, purification, antioxidant and lipid-regulating effects of pigments from red pitaya[D]. Guangzhou: Guangdong Pharmaceutical University, 2013. (in Chinese). [2] 鲁青, 张超凤, 严美婷, 等. 超声波-酶解辅助提取火龙果皮色素的工艺优化 [J]. 食品研究与开发, 2019, 40(17):68−72. doi: 10.12161/j.issn.1005-6521.2019.17.013LU Q, ZHANG C F, YAN M T, et al. Optimization of ultrasonic-enzymatic hydrolysis assisted extraction process of pigment from pitaya peel [J]. Food Research and Development, 2019, 40(17): 68−72.(in Chinese) doi: 10.12161/j.issn.1005-6521.2019.17.013 [3] SOEDJATMIKO H, CHRISNASARI R, HARDJO P H. The effect of fermentation process on physical and chemical characteristics of pitaya (Hylocereus polyrhiuzus [F. A. C. Weber] Britton & Rose) stem flour [J]. IOP Conference Series: Earth and Environmental Science, 2019, 293(1): 1−2. [4] 马若影, 杨慧强, 李国胜, 等. 亚临界水提取红心火龙果茎多糖及其抗氧化活性 [J]. 食品工业科技, 2017, 38(10):286−290.MA R Y, YANG H Q, LI G S, et al. Study on the extraction and antioxidant activity of polysaccharide from red pulp Hylocereus undatus stem by subcritical water [J]. Science and Technology of Food Industry, 2017, 38(10): 286−290.(in Chinese) [5] 徐曼旭, 于国萍, 付饶, 等. 薏米多糖亚临界水萃取工艺的优化 [J]. 食品工业, 2014, 35(1):94−97.XU M X, YU G P, FU R, et al. Optimization of extracting technology for polysaccharide of Coix seed by subcritical water [J]. The Food Industry, 2014, 35(1): 94−97.(in Chinese) [6] 包怡红, 邓启. 响应面法优化亚临界水萃取黑木耳多糖工艺 [J]. 食品与生物技术学报, 2016, 35(10):1053−1060. doi: 10.3969/j.issn.1673-1689.2016.10.007BAO Y H, DENG Q. Optimization of subcritical water extraction of polysaccharides from Auricularia auricular by response surface methodology [J]. Journal of Food Science and Biotechnology, 2016, 35(10): 1053−1060.(in Chinese) doi: 10.3969/j.issn.1673-1689.2016.10.007 [7] 刘焕燕, 郑光耀, 贺亮, 等. 亚临界水提取无花果多糖的工艺研究 [J]. 食品与发酵科技, 2017, 53(4):20−26.LIU H Y, ZHENG G Y, HE L, et al. Study on subcritical water extraction of polysaccharide from Ficus carica linn [J]. Sichuan Food and Fermentation, 2017, 53(4): 20−26.(in Chinese) [8] KO MIN-JUNG, NAM HWA-HYUN, CHUNG MYONG-SOO. Subcritical water extraction of bioactive compounds from Orostachys japonicus A. Berger (Crassulaceae). [J]. Scientific Reports, 2020, 10(1): 1627−1633. [9] DONG-SHIN KIM, SANG-BIN LIM. Kinetic study of subcritical water extraction of flavonoids from citrus unshiu peel [J]. Separation and Purification Technology, 2020: 250. DOI: 10.1016/j.seppur.2020.117259. [10] 杨诗奇, 张晨, 李超, 等. 亚临界水在生物大分子中的应用进展 [J]. 食品工业, 2020, 41(6):262−264.YANG S Q, ZHANG C, LI C, et al. Research progress of subcritical water technology in biomacromolecules [J]. The Food Industry, 2020, 41(6): 262−264.(in Chinese) [11] 赵超. 超声强化亚临界水提取枸杞多糖的研究[D]. 广州: 华南理工大学, 2014.ZHAO C. Ultrasound-enhanced subcritical water extraction of polysaccharides from Lycium barbarum L[D]. Guangzhou: South China University of Technology, 2014. (in Chinese). [12] QIN X. Optimization of the ultrasonic assisted extraction of polysaccharides from dendrobium huoshanense by response surface method [J]. Medicinal Plant, 2012, 3(8): 78−80. [13] 史伟国, 白国栋, 宗希明, 等. 星点设计-响应面法优化超声提取脱皮马勃粗多糖工艺 [J]. 中国野生植物资源, 2018, 37(5):4−7. doi: 10.3969/j.issn.1006-9690.2018.05.002SHI W G, BAI G D, ZONG X M, et al. Optimization of ultrasound-assisted crude polysaccharide extraction from lasiosphaera fenzlii by central composite design-response surface methodology [J]. Chinese Wild Plant Resources, 2018, 37(5): 4−7.(in Chinese) doi: 10.3969/j.issn.1006-9690.2018.05.002 [14] PAWLOWSKI T M, POOLE C F. Extraction of thiabendazole and carbendazim from foods using pressurized hot (subcritical) water for extraction: A feasibility study [J]. Journal of Agricultural and Food Chemistry, 1998, 46(8): 3124−3132. doi: 10.1021/jf980016x [15] LI B, YANG Y, GAN Y, et al. On-line coupling of subcritical water extraction with high-performance liquid chromatography via solid-phase trapping [J]. Journal of Chromatography. A, 2000, 873(2): 175−184. doi: 10.1016/S0021-9673(99)01322-9 [16] 赵健, 王二霞. 亚临界水萃取技术及其在肉品检测中的应用 [J]. 肉类研究, 2008(11):65−68. doi: 10.3969/j.issn.1001-8123.2008.11.017ZHAO J, WANG E X. Sub-critical water extraction and the application in meat detection [J]. Meat Research, 2008(11): 65−68.(in Chinese) doi: 10.3969/j.issn.1001-8123.2008.11.017 [17] SMITH R M. Extractions with superheated water [J]. Journal of Chromatography A, 2002, 975: 31−46. doi: 10.1016/S0021-9673(02)01225-6 [18] 郭宏垚, 李冬, 雷雄, 等. 花椒多酚提取工艺响应面优化及动力学分析 [J]. 食品科学, 2018, 39(2):247−253. doi: 10.7506/spkx1002-6630-201802039GUO H Y, LI D, LEI X, et al. Optimization by response surface methodology and kinetics of extraction of polyphenols from Chinese prickly ash [J]. Food Science, 2018, 39(2): 247−253.(in Chinese) doi: 10.7506/spkx1002-6630-201802039 [19] 李丹丹. 枸杞多糖的提取及其水解物的研究[D]济南: 齐鲁工业大学, 2014.LI D D. Study on extraction and hydrolysates of Lycium barbarum polysaccharides[D] Jinan: Qilu University of Technology, 2014. (in Chinese).