水酶法提取紫苏籽油脂工艺
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摘要
采用中心组合设计(CCD)-响应面(RSM)优化紫苏籽油脂的水酶法提取工艺。在单因素试验的基础上采用中心组合设计方法,研究了酶的种类、酶解温度、pH、液(mL)固(g)比、加酶量、以及时间相互作用对紫苏油脂提取率的影响。结果显示,拟合得到方程显著,确定的紫苏油脂提取最优条件为:碱性蛋白酶在pH9. 5条件下液(mL)固(g)比9. 97:1、加酶量2. 75%、温度56. 1℃、时间5. 25 h,该条件下紫苏油脂的提取率可达到37. 65%,与理论值38. 3%十分接近,建立的模型真实可靠,确定了紫苏油脂的最佳提取工艺。经气相色谱检测紫苏籽油中含有棕榈酸、硬脂酸、油酸、亚油酸、α-亚麻酸等脂肪酸,水酶法提取紫苏油脂的α-亚麻酸相对含量最高67. 9%,且相对溶剂法及冷榨法理化指标最好。
Central composite design( CCD)-response surface( RSM) was used to optimize the aqueous enzymatic extraction process of Perilla frutescens seed oil. On the basis of single factor experiment,we adopted the central composite design method to study the effects of enzymatic species,enzymatic hydrolysis temperature,pH,liquid-solid ratio,enzyme dosage and time interaction on the extraction rate of Perilla oil. The fitting equation was significant,the optimum conditions for the extraction of Perilla oil were as follows: pH is 9. 5 in alkaline protease,the solid-liquid ratio( g) was 9. 97:1,the amount of enzyme added was 2. 75%,the temperature was 56. 1℃,and the time was 5. 25 h. Under this condition,the extraction rate of Perilla oil could reach 37. 65%,which was very close to the theoretical value of 38. 3%. The established model was true and reliable,and the optimum extraction process of Perilla oil was determined. The Perilla seed oil contains palmitic acid,stearic acid,oleic acid,linoleic acid and alpha-linolenic acid by gas chromatography,the relative content of alpha-linolenic acid in Perilla oil extracted by aqueous enzymatic method was 67. 9%,and the physical and chemical indexes of relative solvent method and cold pressing method were the best.
Central composite design( CCD)-response surface( RSM) was used to optimize the aqueous enzymatic extraction process of Perilla frutescens seed oil. On the basis of single factor experiment,we adopted the central composite design method to study the effects of enzymatic species,enzymatic hydrolysis temperature,pH,liquid-solid ratio,enzyme dosage and time interaction on the extraction rate of Perilla oil. The fitting equation was significant,the optimum conditions for the extraction of Perilla oil were as follows: pH is 9. 5 in alkaline protease,the solid-liquid ratio( g) was 9. 97:1,the amount of enzyme added was 2. 75%,the temperature was 56. 1℃,and the time was 5. 25 h. Under this condition,the extraction rate of Perilla oil could reach 37. 65%,which was very close to the theoretical value of 38. 3%. The established model was true and reliable,and the optimum extraction process of Perilla oil was determined. The Perilla seed oil contains palmitic acid,stearic acid,oleic acid,linoleic acid and alpha-linolenic acid by gas chromatography,the relative content of alpha-linolenic acid in Perilla oil extracted by aqueous enzymatic method was 67. 9%,and the physical and chemical indexes of relative solvent method and cold pressing method were the best.
引文
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11 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5532-2008动植物油脂碘值的测定[S].北京:中国标准出版社,2009:1-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5532-2008 Animal and vegetable fats and oils-Determination of iodine value[S]. Beijing:Standards Press of China,2009:1-1.
12 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5528-2008动植物油脂水分及挥发物含量测定[S].北京:中国标准出版社,2009:1-20.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5528-2008 Animal and vegetable fats and oils-Determination of moisture and volatile matter content[S]. Beijing:Standards Press of China,2009:1-20.
13 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5527-2010动植物油脂折光指数的测定[S].北京:中国标准出版社,2011:3-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5527-2010 Animal and vegetable fats and oils-Determination of refractive index[S]. Beijing:Standards Press of China,2011:3-1.
14 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5518-2008粮油检验粮食、油料相对密度的测定[S].北京:中国标准出版社,2009:1-20.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5518-2008 Inspection of grain and oil-Determination of relatively density of grain and oilseeds[S]. Beijing:Standards Press of China,2009:1-20.
15 .吴锦波,吴振,朱国君,等.紫苏饼粕浓缩蛋白溶解性与乳化特性的研究[J].中国粮油学报,2011,26(2):55-58.Wu J B,Wu Z,Zhu G J,et al. Solubility and emulsifying properties of Perilla seed meal protein concentrate[J].Journal of the Chinese Cereals and Oils Association,2011,26(2):55-58.
16 . Shah S,Sharma A,Gupta M N. Extraction of oil from Jatropha curcas L. seed kernels by combination of ultrasonication and aqueous enzymatic oil extraction[J]. Bioresource Technology,2005,96(1):121-123.
17 . Wani A A,Sogi D S,Grover L,et al. Effect of temperature,alkali concentration,mixing time and meal/solvent ratio on the extraction of watermelon seed proteins-a response surface approach[J]. Biosystems Engineering,2006,94(1):67-73.
18 . Wani A A,Kaur D,Ahmed I,et al. Extraction optimization of watermelon seed protein using response surface methodology[J]. LWT-Food Science and Technology,2008,41(8):1514-1520.
19 .王朵,程方,王赛璐,等.响应面中心组合设计法优化制备载磁活性炭[J].环境工程学报,2016,10(8):4079-4086.Wang D,Cheng F,Wang S L,et al. Optimization of magnetic activated carbon with response surface central composite design methodology[J]. Chinese Journal of Environmental Engineering,2016,10(8):4079-4086.
20 .尹延霞,朱奇峰,刘汉杰,等.中心组合实验设计响应面法优化α淀粉酶抑制剂筛选条件[J].西南师范大学学报:自然科学版,2015,40(4):83-88.Yin Y X,Zhu Q F,Liu H J,et al. On optimization screening conditions ofα-amylase inhibitor by central composite design coupled with response surface methodology[J].Journal of Southwest China Normal University:Natural Science Edition,2015,40(4):83-88.
2 .姚正颖,赵银纤,侯北伟,等. 3种脂溶性酚类对紫苏籽油的抗氧化作用研究[J].中国油脂,2017,42(5):92-95.Yao Z Y,Zhao Y X,Hou B W,et al. Antioxidation effects of three liposoluble phenols on Perilla seed oil[J]. China Oils and Fats,2017,42(5):92-95.
3 . Zhang X,Wu W,Zheng Y L,et al. Essential oil variations in different Perilla L. accessions:chemotaxonomic implications[J]. Plant Systematics and Evolution,2009,281(1-4):1-10.
4 .李占君,张琳,祖元刚,等.二氧化碳超临界提取塔拉籽油及其品质分析[J].植物研究,2015,35(3):467-470.Li Z J,Zhang L,Zu Y G,et al. Tara oil extraction by supercritical carbon dioxide and its quality[J]. Bulletin of Botanical Research,2015,35(3):467-470.
5 .孙谦,胡中海,孙志高,等.响应面法优化超临界CO2流体萃取红橘种子油[J].西南师范大学学报:自然科学版,2016,41(2):46-52.Sun Q,Hu Z H,Sun Z G,et al. On optimization of supercritical carbon dioxide extraction of oil from tangerine seeds with response surface methodology[J]. Journal of Southwest China Normal University:Natural Science Edition,2016,41(2):46-52.
6 .孟庆焕,祖元刚,王化,等.酶法辅助乙醇优选牡丹种皮总黄酮[J].植物研究,2015,35(4):628-631.Meng Q H,Zu Y G,Wang H,et al. Enzyme assisted ethanol extraction of total flavonoids from peony episperm[J].Bulletin of Botanical Research,2015,35(4):628-631.
7 .周启超,姚欢欢,陈凤丽,等.响应面法优选牡丹果荚中丹皮酚和芍药苷提取工艺的研究[J].植物研究,2014,34(2):271-275.Zhou Q C,Yao H H,Chen F L,et al. Optimization of microwave-assisted extraction of paeoniflorin and paeonol from peony pod using response surface methodology[J].Bulletin of Botanical Research,2014,34(2):271-275.
8 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5538-2005动植物油脂过氧化值测定[S].北京:中国标准出版社,2006:12-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5538-2005 Animal and vegetable fats and oils-Determination of peroxide value[S]. Beijing:Standards Press of China,2006:12-1.
9 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5530-2005动植物油脂酸值和酸度测定[S].北京:中国标准出版社,2006:12-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5530-2005 Animal and vegetable fats and oils-Determination of acid value and acidity[S]. Beijing:Standards Press of China,2006:12-1.
10 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5534-2008动植物油脂皂化值的测定[S].北京:中国标准出版社,2009:1-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5534-2008 Animal and vegetable fats and oils-Determination of saponification value[S]. Beijing:Standards Press of China,2009:1-1.
11 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5532-2008动植物油脂碘值的测定[S].北京:中国标准出版社,2009:1-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5532-2008 Animal and vegetable fats and oils-Determination of iodine value[S]. Beijing:Standards Press of China,2009:1-1.
12 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5528-2008动植物油脂水分及挥发物含量测定[S].北京:中国标准出版社,2009:1-20.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5528-2008 Animal and vegetable fats and oils-Determination of moisture and volatile matter content[S]. Beijing:Standards Press of China,2009:1-20.
13 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5527-2010动植物油脂折光指数的测定[S].北京:中国标准出版社,2011:3-1.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5527-2010 Animal and vegetable fats and oils-Determination of refractive index[S]. Beijing:Standards Press of China,2011:3-1.
14 .中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 5518-2008粮油检验粮食、油料相对密度的测定[S].北京:中国标准出版社,2009:1-20.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China,Standardization Administration of China. GB/T 5518-2008 Inspection of grain and oil-Determination of relatively density of grain and oilseeds[S]. Beijing:Standards Press of China,2009:1-20.
15 .吴锦波,吴振,朱国君,等.紫苏饼粕浓缩蛋白溶解性与乳化特性的研究[J].中国粮油学报,2011,26(2):55-58.Wu J B,Wu Z,Zhu G J,et al. Solubility and emulsifying properties of Perilla seed meal protein concentrate[J].Journal of the Chinese Cereals and Oils Association,2011,26(2):55-58.
16 . Shah S,Sharma A,Gupta M N. Extraction of oil from Jatropha curcas L. seed kernels by combination of ultrasonication and aqueous enzymatic oil extraction[J]. Bioresource Technology,2005,96(1):121-123.
17 . Wani A A,Sogi D S,Grover L,et al. Effect of temperature,alkali concentration,mixing time and meal/solvent ratio on the extraction of watermelon seed proteins-a response surface approach[J]. Biosystems Engineering,2006,94(1):67-73.
18 . Wani A A,Kaur D,Ahmed I,et al. Extraction optimization of watermelon seed protein using response surface methodology[J]. LWT-Food Science and Technology,2008,41(8):1514-1520.
19 .王朵,程方,王赛璐,等.响应面中心组合设计法优化制备载磁活性炭[J].环境工程学报,2016,10(8):4079-4086.Wang D,Cheng F,Wang S L,et al. Optimization of magnetic activated carbon with response surface central composite design methodology[J]. Chinese Journal of Environmental Engineering,2016,10(8):4079-4086.
20 .尹延霞,朱奇峰,刘汉杰,等.中心组合实验设计响应面法优化α淀粉酶抑制剂筛选条件[J].西南师范大学学报:自然科学版,2015,40(4):83-88.Yin Y X,Zhu Q F,Liu H J,et al. On optimization screening conditions ofα-amylase inhibitor by central composite design coupled with response surface methodology[J].Journal of Southwest China Normal University:Natural Science Edition,2015,40(4):83-88.