琯溪蜜柚皮中精油提取及色素分离工艺研究
摘要
论文题目:琯溪蜜柚皮中精油提取及色素分离工艺研究
学科、专业:工学、食品科学
硕士研究生姓名:于文峰
指导教师:王海鸥副教授
琯溪蜜柚是平和县的地方传统名果,也是我国著名的柚类品种之一。近些年来,琯溪蜜柚已成为平和县的经济支柱产业。2009年,平和县琯溪蜜柚种植面积达4.3万公顷,年产量80万吨,并呈逐年上升趋势,伴随着蜜柚年产量的增加,柚子的加工量也越来越大。柚皮表皮层中的精油和色素含量较高,对琯溪蜜柚果皮表皮层进行深加工,从中提取精油和色素,不仅能提高琯溪蜜柚的附加值,同时也为减少环境污染和资源浪费提供了一条有效的解决途径,对农产品加工技术发展具有积极的推动作用。本文以琯溪蜜柚果皮表皮层为原料,研究精油提取和色素分离的工艺参数,并对其成分进行相关分析,为琯溪蜜柚果皮精油和色素的产业化生产提供理论依据。
论文对水蒸汽蒸馏法提取柚皮精油的工艺进行了研究。确定了精油提取的最佳工艺条件为:提取时间30min,破碎等级D,料液比1:35。在此条件下,精油的提取率为3.945%(干基)。通过GC-MS及GC-MS-O对精油成分进行分析,并结合感官评定,发现组成琯溪蜜柚皮精油特征香味的主要成分是冰片烯、罗勒烯、(E)-4,8-二甲基-1,3,7-壬三烯、芳樟醇、金合欢醇、反式石竹烯、4-萜烯醇、己酸己酯、α-松油醇、吉马烯D、辛酸己酯、诺卡酮、β-月桂烯、苧烯、葵醛、橙花醇。
对水溶性柚皮色素采用大孔树脂吸附法进行分离。通过静态吸附和洗脱试验的测定结果显示,用0.2g树脂对50mL色素液进行吸附,AB-8树脂对色素的平衡吸附率和平衡解吸率分别为57.40%和97.65%。综合考虑,选择AB-8大孔吸附树脂对色素进行分离。采用16×450mm层析柱进行吸附洗脱试验,结果表明,树脂吸附的最佳工艺条件为:温度25℃,上样浓度1.312(吸光值),高径比12:1,吸附流速4BV/h;在此条件下,当色素液吸附量为8BV时,其色素吸附率达91.44%。解吸的最佳工艺条件为:温度25℃,洗脱剂70%乙醇,洗脱流速3BV/h;在此条件下,色素的解吸率为99.47%。通过树脂重复使用性能测定,发现AB-8树脂具有良好的再生能力,经过21次再生后柚皮色素吸附率仅下降1.56%。显色反应试验表明,柚皮色素为黄酮类物质。稳定性试验表明,色素在100℃、pH3-12以及常用食品添加剂中都有较好的稳定性。薄层层析试验、紫外可见分光光度法试验和HPLC-MS对色素成分的分析结果表明,色素的主要成分是柚皮苷,其含量占色素总量的70%左右。
Guanxi pomelo is a kind of well known traditional fruit in Pinghe County, and one of the famous varieties of pomelo in China. In 2009, 43000 hm2 of Guanxi pomelo has planted in the whole county, with 800000 tons of annual output and increasing year by year. As a result, more and more pomelo is used to process. High content of essential oil and pigments is in the external part of pomelo peel. By extracting essential oil and pigments, it will not only improve the added-value of Guanxi pomelo, but also reduce the pollution of the environment and resource waste. In this paper, the external part of Guanxi pomelo peel was used as the raw material to study the processing technology and the components of essential oil and pigment.
In the thesis, the hydro-distillation (HD) technology of essential oil were studied. The results showed that the optimum operation conditions were extracting time 30min, degree of fragmentation D, solid to liquid ratio 1:35 (OD value). The yield of essential oil on dry basis was 3.945% under this condition. The results of GC-MS, GC-MS-O and sensory evaluation showed that the main components of characteristic flavor in Guanxi pomelo peel essential oil were bornylene, (Z)-3,7-dimethyl-1,3,6-Octatriene, (E)-4,8-dimethyl-1,3,7-nonatriene, L-linalool, farnesol, trans-caryophyllene, 4-methyl-1-(1-methylethyl)-3-cyclohexen-1-ol, hexanoic acid, hexyl ester,α-terpineol, germacrene-D, hexyl octanoate, nootkatone,β-myrcene, limonene, decanal and nerol.
Pigment was separated by macroporous resin. AB-8 resin was selected by static adsorption and desorption experiments (resin 0.2g, volume of pigment 50mL). The results showed that the equilibrium adsorption rate was 57.40% and the equilibrium adsorption rate was 97.65%. Chromatographic column (16×450mm) was used for dynamic experiment. The results showed that the optimum adsorption conditions were temperature 25℃, concentration 1.312, column height to diameter ratio 12:1 and flow rate 4BV/h. The adsorption rate processing 8BV is 91.44% under this condition. The optimum desorption conditions were temperature 25℃, eluted by 70% ethanol and flow rate 4BV/h. The desorption rate is 99.47% under this condition. The result of resin reusability experiment showed that AB-8 resin can be long-term reused. The adsorption rate only fell 1.56% after 21 times resin regeneraton.The components of the pigment were analyzed by color reaction, TLC, UV-VIS and HPLC-MS. The results showed that the pigment’s component is the flavonoids, and the main component is naringin which is 70% of the total amount. The results of pigment stability experiment showed that the pigment is stable under 100℃, pH3-12 and common food additives.
学科、专业:工学、食品科学
硕士研究生姓名:于文峰
指导教师:王海鸥副教授
琯溪蜜柚是平和县的地方传统名果,也是我国著名的柚类品种之一。近些年来,琯溪蜜柚已成为平和县的经济支柱产业。2009年,平和县琯溪蜜柚种植面积达4.3万公顷,年产量80万吨,并呈逐年上升趋势,伴随着蜜柚年产量的增加,柚子的加工量也越来越大。柚皮表皮层中的精油和色素含量较高,对琯溪蜜柚果皮表皮层进行深加工,从中提取精油和色素,不仅能提高琯溪蜜柚的附加值,同时也为减少环境污染和资源浪费提供了一条有效的解决途径,对农产品加工技术发展具有积极的推动作用。本文以琯溪蜜柚果皮表皮层为原料,研究精油提取和色素分离的工艺参数,并对其成分进行相关分析,为琯溪蜜柚果皮精油和色素的产业化生产提供理论依据。
论文对水蒸汽蒸馏法提取柚皮精油的工艺进行了研究。确定了精油提取的最佳工艺条件为:提取时间30min,破碎等级D,料液比1:35。在此条件下,精油的提取率为3.945%(干基)。通过GC-MS及GC-MS-O对精油成分进行分析,并结合感官评定,发现组成琯溪蜜柚皮精油特征香味的主要成分是冰片烯、罗勒烯、(E)-4,8-二甲基-1,3,7-壬三烯、芳樟醇、金合欢醇、反式石竹烯、4-萜烯醇、己酸己酯、α-松油醇、吉马烯D、辛酸己酯、诺卡酮、β-月桂烯、苧烯、葵醛、橙花醇。
对水溶性柚皮色素采用大孔树脂吸附法进行分离。通过静态吸附和洗脱试验的测定结果显示,用0.2g树脂对50mL色素液进行吸附,AB-8树脂对色素的平衡吸附率和平衡解吸率分别为57.40%和97.65%。综合考虑,选择AB-8大孔吸附树脂对色素进行分离。采用16×450mm层析柱进行吸附洗脱试验,结果表明,树脂吸附的最佳工艺条件为:温度25℃,上样浓度1.312(吸光值),高径比12:1,吸附流速4BV/h;在此条件下,当色素液吸附量为8BV时,其色素吸附率达91.44%。解吸的最佳工艺条件为:温度25℃,洗脱剂70%乙醇,洗脱流速3BV/h;在此条件下,色素的解吸率为99.47%。通过树脂重复使用性能测定,发现AB-8树脂具有良好的再生能力,经过21次再生后柚皮色素吸附率仅下降1.56%。显色反应试验表明,柚皮色素为黄酮类物质。稳定性试验表明,色素在100℃、pH3-12以及常用食品添加剂中都有较好的稳定性。薄层层析试验、紫外可见分光光度法试验和HPLC-MS对色素成分的分析结果表明,色素的主要成分是柚皮苷,其含量占色素总量的70%左右。
Guanxi pomelo is a kind of well known traditional fruit in Pinghe County, and one of the famous varieties of pomelo in China. In 2009, 43000 hm2 of Guanxi pomelo has planted in the whole county, with 800000 tons of annual output and increasing year by year. As a result, more and more pomelo is used to process. High content of essential oil and pigments is in the external part of pomelo peel. By extracting essential oil and pigments, it will not only improve the added-value of Guanxi pomelo, but also reduce the pollution of the environment and resource waste. In this paper, the external part of Guanxi pomelo peel was used as the raw material to study the processing technology and the components of essential oil and pigment.
In the thesis, the hydro-distillation (HD) technology of essential oil were studied. The results showed that the optimum operation conditions were extracting time 30min, degree of fragmentation D, solid to liquid ratio 1:35 (OD value). The yield of essential oil on dry basis was 3.945% under this condition. The results of GC-MS, GC-MS-O and sensory evaluation showed that the main components of characteristic flavor in Guanxi pomelo peel essential oil were bornylene, (Z)-3,7-dimethyl-1,3,6-Octatriene, (E)-4,8-dimethyl-1,3,7-nonatriene, L-linalool, farnesol, trans-caryophyllene, 4-methyl-1-(1-methylethyl)-3-cyclohexen-1-ol, hexanoic acid, hexyl ester,α-terpineol, germacrene-D, hexyl octanoate, nootkatone,β-myrcene, limonene, decanal and nerol.
Pigment was separated by macroporous resin. AB-8 resin was selected by static adsorption and desorption experiments (resin 0.2g, volume of pigment 50mL). The results showed that the equilibrium adsorption rate was 57.40% and the equilibrium adsorption rate was 97.65%. Chromatographic column (16×450mm) was used for dynamic experiment. The results showed that the optimum adsorption conditions were temperature 25℃, concentration 1.312, column height to diameter ratio 12:1 and flow rate 4BV/h. The adsorption rate processing 8BV is 91.44% under this condition. The optimum desorption conditions were temperature 25℃, eluted by 70% ethanol and flow rate 4BV/h. The desorption rate is 99.47% under this condition. The result of resin reusability experiment showed that AB-8 resin can be long-term reused. The adsorption rate only fell 1.56% after 21 times resin regeneraton.The components of the pigment were analyzed by color reaction, TLC, UV-VIS and HPLC-MS. The results showed that the pigment’s component is the flavonoids, and the main component is naringin which is 70% of the total amount. The results of pigment stability experiment showed that the pigment is stable under 100℃, pH3-12 and common food additives.
引文
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