椪柑籽油提取工艺优化及其化学成分分析
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摘要
桠柑是一种受欢迎的水果,桠柑肉多用于鲜食、加工成罐头、饮料等,而桠柑籽却没有被利用。目前,国内外已经对多种水果的副产物进行了分析研究,但国内对桠柑籽的研究较少。本论文拟对桠柑籽油脂的提取工艺及脱脂后的桠柑籽粉末的化学组成进行测定。
在单因试验的基础上,采用Box-Behnken中心组合设计,对桠柑籽油超临界C02萃取工艺中的时间、温度、压力和流量4因素的最优化组合参数进行定量研究,得到并分析上述因素与桠柑籽油提取得率关系的数学模型。结果表明：最佳的工艺条件为萃取压力34.4Mpa、CO2流量25.8 L/h、萃取时间147.6 min、萃取温度39.3℃。在此条件下,桠柑籽油提取得率的理论值为45.95%,经验证,实测值为(45.12±1.36)%(n=3),说明回归模型能较好地预测桠柑籽油的提取得率。
应用气相色谱法测定了湘西桠柑籽油中脂肪酸的含量。其中含有30.88%的油酸,26.11%的亚油酸和29%的软脂酸,不饱和脂肪酸达70.43%。然后对桠柑籽油进行了近红外光谱分析,最大吸收波数在5801,5677,4331和4258 cm-1,在7174和8269cm-1处也可看到弱吸收带。其中,在5801 cm-1处有一个尖峰,为油酸的特有峰(桠柑籽中含有大量的油酸)。5677 cm-1处为饱和脂肪酸(棕榈酸和硬脂酸)的特有峰。近红外光谱法与气相色谱法结果一致,通过两种方法的相互验证,可以确定本实验中两种提取方法以及油脂分析方法的准确性。上述结果说明湘西桠柑籽提取油具有较高营养价值,可做进一步开发利用。
对湘西椪柑籽中的氨基酸、蛋白质、淀粉、含水量、灰分以及矿物元素进行分析研究,结果表明,氨基酸总量为12.11g/100g,含量最高的为谷氨酸,含量为2.50g/100g。含水量为8.13～8.17%,粗蛋白为23.56～25.48%,总糖为10.65～12.39%,灰分为6.66-6.80%。同时,还可以提供很好的Ca, Fe,Cu,Zn等矿物元素,研究将为湘西桠柑籽的综合利用提供理论依据。
Ponkan is a popular fruit, which is used to process into canned food, beverage, and etc. However, its citrus seed has not been used compeletely. Nowadays, the byproducts of a variety of fruit at home and abroad have been were analyzed, but the study on the aspect of Ponkan seed is little. Therefore, oil extraction process of Ponkan seed and chemical composition were analysised and determined in this paper.
In order to make full use of agricultural waste materials-Xiangxi Ponkan seed and increase the extraction efficiency of seed oil from its powder, the influences of time, temperature, pressure and the flux of CO2 on the yield of seed oil from its powder with the supercritical CO2 fluid extraction technique were studied according to the Box-Behnken central composite experimental design based on the single factor test. Analyzed the mathematical model which established by response surface methodology (RSM), and the same time, relationships between studied factors and response of Ponkan seed oil extraction yield were described. Based on the canonical analysis, the optimum conditions were obtained as follows:the extraction pressure is 34.4 Mpa, the flux of CO2 is 25.8 L/h, the extraction time is 147.6 min and the temperature is 39.3℃. Under the optimized extraction conditions, the predictive maximum yield of seed oil is 45.95% and the average validation value is (45.12±1.36)%(n=3), so the model would be used to predict the extraction results well.
Gas chromatography (GC) was used to determine the fatty acids of Xiangxi Ponkan seed oil. The oleic acid, linoleic acid and palmitic acid fell in the range of 30.88%, 26.11% and 29%, respectively. The unsaturated fatty acids was high than 70%. Then near-infrared spectroscopy (NIRS) was used to analysis the citrus oil. Absorption maxima were clearly observed at 5801,5677,4331,4258 cm-1 together with small absorption band at 7174 and 8269 cm-1. By comparison, NIR and GC methods were validated each other, and the same results can be obtained in our work, which demonstrated that our extraction and analysis methods were reliable and accurate. The results indicated that Hunan citrus seed extract oil has a high nutritional value and can do further development and utilization.
Soxhlet extraction was used to extract Xiangxi Ponkan seed, and the content of its nutrient components were determined. After oil extraction, the amino acids, protein, starch, moisture content, ash and mineral elements in powder samples were analyzed. The total Amino acids content was to 12.11 g/100g, the highest concentration of glutamic acid was to2.53 g/100g. The content of water, crude protein, total sugar and ash was to 8.15±0.02, of 24.52±0.96,11.52±0.87,6.73+0.07, respectively. High content of Ca, Fe, Cu, Zn and other minerals were contained in oil sample, the study of this paper will provide a theoretical basis for the comprehensive utilization of Xiangxi Ponkan.
在单因试验的基础上,采用Box-Behnken中心组合设计,对桠柑籽油超临界C02萃取工艺中的时间、温度、压力和流量4因素的最优化组合参数进行定量研究,得到并分析上述因素与桠柑籽油提取得率关系的数学模型。结果表明：最佳的工艺条件为萃取压力34.4Mpa、CO2流量25.8 L/h、萃取时间147.6 min、萃取温度39.3℃。在此条件下,桠柑籽油提取得率的理论值为45.95%,经验证,实测值为(45.12±1.36)%(n=3),说明回归模型能较好地预测桠柑籽油的提取得率。
应用气相色谱法测定了湘西桠柑籽油中脂肪酸的含量。其中含有30.88%的油酸,26.11%的亚油酸和29%的软脂酸,不饱和脂肪酸达70.43%。然后对桠柑籽油进行了近红外光谱分析,最大吸收波数在5801,5677,4331和4258 cm-1,在7174和8269cm-1处也可看到弱吸收带。其中,在5801 cm-1处有一个尖峰,为油酸的特有峰(桠柑籽中含有大量的油酸)。5677 cm-1处为饱和脂肪酸(棕榈酸和硬脂酸)的特有峰。近红外光谱法与气相色谱法结果一致,通过两种方法的相互验证,可以确定本实验中两种提取方法以及油脂分析方法的准确性。上述结果说明湘西桠柑籽提取油具有较高营养价值,可做进一步开发利用。
对湘西椪柑籽中的氨基酸、蛋白质、淀粉、含水量、灰分以及矿物元素进行分析研究,结果表明,氨基酸总量为12.11g/100g,含量最高的为谷氨酸,含量为2.50g/100g。含水量为8.13～8.17%,粗蛋白为23.56～25.48%,总糖为10.65～12.39%,灰分为6.66-6.80%。同时,还可以提供很好的Ca, Fe,Cu,Zn等矿物元素,研究将为湘西桠柑籽的综合利用提供理论依据。
Ponkan is a popular fruit, which is used to process into canned food, beverage, and etc. However, its citrus seed has not been used compeletely. Nowadays, the byproducts of a variety of fruit at home and abroad have been were analyzed, but the study on the aspect of Ponkan seed is little. Therefore, oil extraction process of Ponkan seed and chemical composition were analysised and determined in this paper.
In order to make full use of agricultural waste materials-Xiangxi Ponkan seed and increase the extraction efficiency of seed oil from its powder, the influences of time, temperature, pressure and the flux of CO2 on the yield of seed oil from its powder with the supercritical CO2 fluid extraction technique were studied according to the Box-Behnken central composite experimental design based on the single factor test. Analyzed the mathematical model which established by response surface methodology (RSM), and the same time, relationships between studied factors and response of Ponkan seed oil extraction yield were described. Based on the canonical analysis, the optimum conditions were obtained as follows:the extraction pressure is 34.4 Mpa, the flux of CO2 is 25.8 L/h, the extraction time is 147.6 min and the temperature is 39.3℃. Under the optimized extraction conditions, the predictive maximum yield of seed oil is 45.95% and the average validation value is (45.12±1.36)%(n=3), so the model would be used to predict the extraction results well.
Gas chromatography (GC) was used to determine the fatty acids of Xiangxi Ponkan seed oil. The oleic acid, linoleic acid and palmitic acid fell in the range of 30.88%, 26.11% and 29%, respectively. The unsaturated fatty acids was high than 70%. Then near-infrared spectroscopy (NIRS) was used to analysis the citrus oil. Absorption maxima were clearly observed at 5801,5677,4331,4258 cm-1 together with small absorption band at 7174 and 8269 cm-1. By comparison, NIR and GC methods were validated each other, and the same results can be obtained in our work, which demonstrated that our extraction and analysis methods were reliable and accurate. The results indicated that Hunan citrus seed extract oil has a high nutritional value and can do further development and utilization.
Soxhlet extraction was used to extract Xiangxi Ponkan seed, and the content of its nutrient components were determined. After oil extraction, the amino acids, protein, starch, moisture content, ash and mineral elements in powder samples were analyzed. The total Amino acids content was to 12.11 g/100g, the highest concentration of glutamic acid was to2.53 g/100g. The content of water, crude protein, total sugar and ash was to 8.15±0.02, of 24.52±0.96,11.52±0.87,6.73+0.07, respectively. High content of Ca, Fe, Cu, Zn and other minerals were contained in oil sample, the study of this paper will provide a theoretical basis for the comprehensive utilization of Xiangxi Ponkan.
引文
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