苦杏仁油、苦杏仁甙提取工艺参数的研究
摘要
本文以苦杏仁为原料,正己烷为浸出溶剂,研究了苦杏仁油的提取工艺参数;研究了杏仁油的精炼方法及工艺参数;以苦杏仁粕为原料,采用无水乙醇为浸提溶剂,以苦杏仁甙提取得率为考察指标,研究了苦杏仁甙的热浸提工艺参数及微波辅助浸提工艺参数,实验结果如下:
(1)采用单因素实验及正交试验研究了料液比、浸提时间、提取温度对苦杏仁油提取率的影响,得出最佳提取工艺参数为:料液比1:10、提取温度60℃、提取时间60 min。
(2)苦杏仁油脂精炼采用水化脱胶、碱炼脱酸工艺,通过对活性炭、活性白土2种脱色剂对杏仁油脱色效果的影响研究,选择了活性白土作为脱色剂,并对添加量、脱色温度、进行了研究,得出最优工艺参数为:活性白土添加量为4 %,脱色温度60℃,搅拌10 min。
(3)研究了不同包装材料、添加剂(TBHQ)对杏仁油储藏期间酸值、过氧化值和色差值的影响;得出玻璃瓶包装的效果明显优于塑料包装(PA/PE)的包装效果。TBHQ添加量为0.01 %和0.02 %的油脂抗氧化效果都很显著,油脂氧化过程中产生的过氧化物均较少,6个月后玻璃瓶包装的过氧化值仅为7.6±0.2 meq/kg,而空白对照的过氧化值为23±1 meq/kg,是添加抗氧化剂包装的3.03倍。添加TBHQ的杏仁油颜色变化缓慢,对杏仁油的抗氧化效果起到关键的作用。
(4)根据BOX-Behnken实验设计原理,在单因素和双因子交互作用的基础上,运用SAS8.0数据统计分析软件,采用响应曲面分析法,确定了无水乙醇热浸提法提取苦杏仁甙的最佳组合为:料液比1:13.18,提取时间110 min,提取温度78.6℃,在此条件下提取两次,提取得率可达4.2 %。
(5)研究了微波辅助法提取苦杏仁中的苦杏仁甙的工艺参数,以高效液相色谱法(HPLC)定量测定苦杏仁甙的提取得率,采用单因素和正交试验考察了料液比,提取时间,提取温度对苦杏仁甙提取得率的影响,确定了微波功率为500 W条件下的最佳提取工艺条件:料液比为1:6,提取温度为75℃,时间为15 min,提取2次,苦杏仁甙的提取得率为4.09℅。
In this paper, using the bitter almond as raw material, almond oil was extracted by the solvent which is the hexane; studying the refining methods and the technology parameters;using the apricot-kernel leavings which has extracted oil as raw material,amygdalin was extracted by absolute alcohol, in order to promote the extraction rate of amygdalin;studying the optimized the parameters of amygdalin process by hot dipped and MAE,the results as follows:
(1) the study of the single effect of material and solvent ratio, temperature, time on extracting rate of almond oil is introduced. By using orthogonal test, it is concluded that the optimum condition is 1:10 of material and solvent ratio 60℃, extracting time 60 min.
(2) the refining methods and the technology parameters:removing the phospholipids by water, free fatty acids by lye,sesearching on the effect of de-colorization of two deodorants which are the activated carbon and activated clay in different dosage, Add volume, discoloration temperature, the optimum technological conditions are: the quality of Activated Clay is 4℅, 60℃,10min mixed.
(3) the effect of Lab、peroxide value and acid on almond oil storage period by different materials and doses of TBHQ;the results was the glass is prefer to PA?PE, the effect of antioxidant of 0.01 % and 0.02 % TBHQ were all well,on oil oxidized processing,the peroxide were less.after 6 months,the peroxide of oil which by the glass storage is 7.6±0.2 meq/kg,the collator is 23±1 meq/kg,which is 3.03 times by the glass storaged,the color of almond oil is change slowly by added the TBHQ,which is important to storage almond oil.
(4) according to BOX-Behnken central composition design principle, with SAS8.0-statistical data analysis software and the method of response surface, the optimum extract conditions were obtained, it is concluded that the optimum condition is ration of apricot-kernel powder to absolute alcohol 1∶13.18、time 110min、and extract temperature 78.6℃,under these conditions, two times extracted, the extraction rate of amygdalin is up to 4.2 %.
(5) Extraction technology of the amygdalin from almond with microwave-assisted extraction was studied.the solvent was absolute alcohol,and amygdalin was analyzed by HPLC method. Several factors, such as ratio of material and liquor, extraction time and extraction temperature were investigated and the optimal MAE conditions were obtained from the orthogonal test. Under the microwave power 500W, the optimal MAE conditions are follows: ratio of material and liquor is 1∶6, extraction temperature is 75℃,extraction time is 15min and 2 times extract, the extraction ratio is 4.09℅.
(1)采用单因素实验及正交试验研究了料液比、浸提时间、提取温度对苦杏仁油提取率的影响,得出最佳提取工艺参数为:料液比1:10、提取温度60℃、提取时间60 min。
(2)苦杏仁油脂精炼采用水化脱胶、碱炼脱酸工艺,通过对活性炭、活性白土2种脱色剂对杏仁油脱色效果的影响研究,选择了活性白土作为脱色剂,并对添加量、脱色温度、进行了研究,得出最优工艺参数为:活性白土添加量为4 %,脱色温度60℃,搅拌10 min。
(3)研究了不同包装材料、添加剂(TBHQ)对杏仁油储藏期间酸值、过氧化值和色差值的影响;得出玻璃瓶包装的效果明显优于塑料包装(PA/PE)的包装效果。TBHQ添加量为0.01 %和0.02 %的油脂抗氧化效果都很显著,油脂氧化过程中产生的过氧化物均较少,6个月后玻璃瓶包装的过氧化值仅为7.6±0.2 meq/kg,而空白对照的过氧化值为23±1 meq/kg,是添加抗氧化剂包装的3.03倍。添加TBHQ的杏仁油颜色变化缓慢,对杏仁油的抗氧化效果起到关键的作用。
(4)根据BOX-Behnken实验设计原理,在单因素和双因子交互作用的基础上,运用SAS8.0数据统计分析软件,采用响应曲面分析法,确定了无水乙醇热浸提法提取苦杏仁甙的最佳组合为:料液比1:13.18,提取时间110 min,提取温度78.6℃,在此条件下提取两次,提取得率可达4.2 %。
(5)研究了微波辅助法提取苦杏仁中的苦杏仁甙的工艺参数,以高效液相色谱法(HPLC)定量测定苦杏仁甙的提取得率,采用单因素和正交试验考察了料液比,提取时间,提取温度对苦杏仁甙提取得率的影响,确定了微波功率为500 W条件下的最佳提取工艺条件:料液比为1:6,提取温度为75℃,时间为15 min,提取2次,苦杏仁甙的提取得率为4.09℅。
In this paper, using the bitter almond as raw material, almond oil was extracted by the solvent which is the hexane; studying the refining methods and the technology parameters;using the apricot-kernel leavings which has extracted oil as raw material,amygdalin was extracted by absolute alcohol, in order to promote the extraction rate of amygdalin;studying the optimized the parameters of amygdalin process by hot dipped and MAE,the results as follows:
(1) the study of the single effect of material and solvent ratio, temperature, time on extracting rate of almond oil is introduced. By using orthogonal test, it is concluded that the optimum condition is 1:10 of material and solvent ratio 60℃, extracting time 60 min.
(2) the refining methods and the technology parameters:removing the phospholipids by water, free fatty acids by lye,sesearching on the effect of de-colorization of two deodorants which are the activated carbon and activated clay in different dosage, Add volume, discoloration temperature, the optimum technological conditions are: the quality of Activated Clay is 4℅, 60℃,10min mixed.
(3) the effect of Lab、peroxide value and acid on almond oil storage period by different materials and doses of TBHQ;the results was the glass is prefer to PA?PE, the effect of antioxidant of 0.01 % and 0.02 % TBHQ were all well,on oil oxidized processing,the peroxide were less.after 6 months,the peroxide of oil which by the glass storage is 7.6±0.2 meq/kg,the collator is 23±1 meq/kg,which is 3.03 times by the glass storaged,the color of almond oil is change slowly by added the TBHQ,which is important to storage almond oil.
(4) according to BOX-Behnken central composition design principle, with SAS8.0-statistical data analysis software and the method of response surface, the optimum extract conditions were obtained, it is concluded that the optimum condition is ration of apricot-kernel powder to absolute alcohol 1∶13.18、time 110min、and extract temperature 78.6℃,under these conditions, two times extracted, the extraction rate of amygdalin is up to 4.2 %.
(5) Extraction technology of the amygdalin from almond with microwave-assisted extraction was studied.the solvent was absolute alcohol,and amygdalin was analyzed by HPLC method. Several factors, such as ratio of material and liquor, extraction time and extraction temperature were investigated and the optimal MAE conditions were obtained from the orthogonal test. Under the microwave power 500W, the optimal MAE conditions are follows: ratio of material and liquor is 1∶6, extraction temperature is 75℃,extraction time is 15min and 2 times extract, the extraction ratio is 4.09℅.
引文
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[2]于希志.我国杏产业发展中的几个障碍因素和解决途径[J].落叶果树,2009(5):7-11.
[3]张青,赵峰.新疆杏资源与产业化发展[J].北方果树,2009(4):40-41.
[4]热依曼·牙森,玉苏甫·阿布里提甫.新疆杏资源及其开发利用[J].新疆农业科学,2005,42(增):49-51.
[5]林培军.崔乃然天山野果林资源-伊犁野果林综合研究[M].北京:中国林业出版社,2004:46.
[6]吴时敏.功能性油脂[M].中国轻工业出版社,2001:22-26.
[7]陈宁.高值天然保健食品—杏仁[J].中国烹饪,1997(3):20.
[8]徐淑英,陈邦杰,师梓文,等.杏仁油和沙棘籽油的组成及理化常数[J].中国油脂,1992,(60):20-27.
[9] Marrone,C.,Poletto,M.,Reverehon,E.,et al.Almond oil exaction by supercritical CO2 experiments and modeling [J].Chemical Engineering Science,1998,53(21):3711-3718.
[10]蓝琳.高营养价值的坚果——杏仁[J].中国食品工业,1999,6(l1):33.
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