超临界CO_2流体萃取南瓜籽油的研究
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摘要
本文采用超临界CO2萃取技术对南瓜籽油的提取进行了研究。探讨了不同萃取条件(原料预处理、颗粒直径、含水量、投料量、萃取温度、萃取压力、萃取时间、CO2流量、分离压力和分离温度)对南瓜籽油提取率的影响,寻找提取南瓜籽油的最佳工艺参数。研究的内容包括以下几个部分:索氏提取法,溶剂浸泡法和超临界CO2流体萃取法提取南瓜籽油的工艺比较及油的品质分析;超临界CO2流体萃取南瓜籽油的单因素试验;采用四因子二次通用旋转组合设计试验优化超临界CO2流体萃取南瓜籽油的工艺参数得出数学模型;测定南瓜籽和超临界CO2流体萃取南瓜籽油的理化性质;利用GC-MS法分析南瓜籽油脂肪酸组成及测定南瓜籽油的微量元素;分析超临界CO2萃取南瓜籽油过程中南瓜籽颗粒内部传质过程机理;
取得研究成果如下:
1.较适宜的工艺参数:投料量200g、含水率4.50%、物料粒度5mm、萃取温度45℃、萃取压力30Mpa、萃取时间90min、CO2流量15L/h、分离Ⅰ的温度和压力分别为40℃和8 Mpa、分离Ⅱ的温度30℃。南瓜籽油提取率最高值为39.83%;通用旋转组合试验优化工艺参数,数学方程,显然除了b44, b23 ,b34外,其余的回归系数都在不同程度上显著,萃取率最高值时各因素的组合为:X1, 2;X2 ,1;X3 ,-1;X4,1。由主效应模型分析得出各因子对超临界萃取南瓜籽油影响大小顺序;萃取温度>萃取压力>CO2流量>萃取时间。
2.南瓜籽中粗蛋白含量29.05%,粗脂肪含量39.83%,粗纤维含量19.21%,矿物质含量1.96%,含水量4.95% ;南瓜籽油中水分及挥发物/( % ) 0.09,比重(d204) 0.8917,色泽Y20R54,折光指数(20℃)1.4639,酸价(以KOH计)/(mg/g) 0.6,碘价(以I2计)/(g/kg)17.6,皂化价(以KOH计)/(mg/g)168.6,过氧化值/(mg/g)5.7; SCF-CO2萃取的南瓜籽油各项指标均达到国际标准;酸价值随贮藏天数的延长而不断上升;萃取时间延长,油脂的透明度和色泽越来越差;萃取压力越大油脂的颜色加深;分离Ⅰ压力越高透明度、色泽越好;萃取温度越高,油脂色泽和透明度较差;共鉴定出6种化合物;南瓜籽中Zn/ Cu比值为817 ;南瓜籽微量元素:Fe 69μg/g、Ca 608μg/g、Zn 87μg/g、Cu10μg/g、Mn 15μg/g等元素,其中Mg含量是2425μg/g,K含量是3875μg/g。
3.经萃取试验结果及油的品质分析比较,超临界CO2流体萃取法优于索氏提取法和溶剂浸泡法。
4.分析超临CO2萃取南瓜籽油过程中南瓜籽颗粒内部传质过程机理及数学模型方程的推导。
This paper study using supercritical CO2 extraction technology for extracting pumpkin seed oil,discussing the affection of different extraction conditions (pretreatment of raw materials, particle size, moisture content, inventory rating, extraction temperature, extraction pressure, extraction time, CO2 flow, separate pressure and separate temperature)for extracting pumpkin seed ,and finding the best process parameters. The content of the study include the following: the extraction process compare and the quality oil analysis of soxhlet extraction, solvent soaking and supercritical CO2 liquid extraction for extracting pumpkin seed oil; supercritical CO2 liquid extraction of pumpkin seed oil single factor test; GM used four second-rotation experiment design optimization supercritical CO2 extraction process parameters of pumpkin seed oil that mathematical model of pumpkin seeds and supercritical CO2 extraction of the physical and chemical properties of pumpkin seed oil; using GC-MS analysis pumpkin Oil and fatty acid composition of trace elements of pumpkin seed oil; of supercritical CO2 extraction process of pumpkin seed oil Indochina Seeds grain mass transfer process mechanism;
Research results as follows:
1. More appropriate process parameters: inventory rating 200g, 4.50% moisture, the material size 5 mm, the extraction temperature 45℃, extraction pressure 30 Mpa, the extraction time 90 min, CO2 flow 15L/h, the temperature and pressure of separationⅠare 40℃and 8Mpa, the temperature of separationⅡis 30℃. the highest value of pumpkin seed oil extraction rate is 39.83%; General rotation test optimization process parameters, mathematical equations, Besides b44, b23, b34, the rest of the regression coefficients are observably in varying degrees, the extraction rate at the highest value of the factors combination: X1, 2; X2, 1; X3, -1; X4, 1. From the main effects model analysis of the factors we get that the big and small order of the factors affecting supercritical extracting pumpkin seed oil:extraction temperature> extraction pressure> CO2 flow> extraction time.
2. the crude protein content of pumpkin seed is 29.05%, fat content 39.83%, crude fiber content 19.21%, mineral content1.96%, water content 4.95%; pumpkin seed oil in the water and volatiles/(%) 0.09, but the share ( d204) 0.8917, color Y20R54, refractive index (20℃) 1.4639, acid value (KOH) /(mg/g) 0.6, the price of iodine (I2)/(g/kg) 17.6, saponification value (KOH ) /(mg/g) 168.6, peroxide value/(mg/g) 5.7. SCF-CO2 extraction of pumpkin seed oil all targets were reached international standards; acid storage with the value of the extension of the number of days the rising; extraction time extension of the transparency and color of oil getting worse; greater pressure on the oil extraction color deepenedⅠpressure from the higher transparency, better color; extraction higher the temperature, color and transparency of oil poor were identified six kinds of compounds; South Seeds of Zn/Cu ratio was 817; pumpkin seeds Trace Elements: 69μgFe/g, Ca 608μg/g, Zn 87μg/g, Cu 10μg/g, Mn 15μg/g, and other elements, including Mg content 2425μg/g, K content 3875μg/g, respectively.
3. By the test results and the quality of analysis and comparison, supercritical CO2 extraction method is better than soxhlet extraction and solvent soaking.
4. Analysis internal mass transfer process and the derivation of mathematical model equations in the process of supercritical CO2 extraction of pumpkin seed oil.
取得研究成果如下:
1.较适宜的工艺参数:投料量200g、含水率4.50%、物料粒度5mm、萃取温度45℃、萃取压力30Mpa、萃取时间90min、CO2流量15L/h、分离Ⅰ的温度和压力分别为40℃和8 Mpa、分离Ⅱ的温度30℃。南瓜籽油提取率最高值为39.83%;通用旋转组合试验优化工艺参数,数学方程,显然除了b44, b23 ,b34外,其余的回归系数都在不同程度上显著,萃取率最高值时各因素的组合为:X1, 2;X2 ,1;X3 ,-1;X4,1。由主效应模型分析得出各因子对超临界萃取南瓜籽油影响大小顺序;萃取温度>萃取压力>CO2流量>萃取时间。
2.南瓜籽中粗蛋白含量29.05%,粗脂肪含量39.83%,粗纤维含量19.21%,矿物质含量1.96%,含水量4.95% ;南瓜籽油中水分及挥发物/( % ) 0.09,比重(d204) 0.8917,色泽Y20R54,折光指数(20℃)1.4639,酸价(以KOH计)/(mg/g) 0.6,碘价(以I2计)/(g/kg)17.6,皂化价(以KOH计)/(mg/g)168.6,过氧化值/(mg/g)5.7; SCF-CO2萃取的南瓜籽油各项指标均达到国际标准;酸价值随贮藏天数的延长而不断上升;萃取时间延长,油脂的透明度和色泽越来越差;萃取压力越大油脂的颜色加深;分离Ⅰ压力越高透明度、色泽越好;萃取温度越高,油脂色泽和透明度较差;共鉴定出6种化合物;南瓜籽中Zn/ Cu比值为817 ;南瓜籽微量元素:Fe 69μg/g、Ca 608μg/g、Zn 87μg/g、Cu10μg/g、Mn 15μg/g等元素,其中Mg含量是2425μg/g,K含量是3875μg/g。
3.经萃取试验结果及油的品质分析比较,超临界CO2流体萃取法优于索氏提取法和溶剂浸泡法。
4.分析超临CO2萃取南瓜籽油过程中南瓜籽颗粒内部传质过程机理及数学模型方程的推导。
This paper study using supercritical CO2 extraction technology for extracting pumpkin seed oil,discussing the affection of different extraction conditions (pretreatment of raw materials, particle size, moisture content, inventory rating, extraction temperature, extraction pressure, extraction time, CO2 flow, separate pressure and separate temperature)for extracting pumpkin seed ,and finding the best process parameters. The content of the study include the following: the extraction process compare and the quality oil analysis of soxhlet extraction, solvent soaking and supercritical CO2 liquid extraction for extracting pumpkin seed oil; supercritical CO2 liquid extraction of pumpkin seed oil single factor test; GM used four second-rotation experiment design optimization supercritical CO2 extraction process parameters of pumpkin seed oil that mathematical model of pumpkin seeds and supercritical CO2 extraction of the physical and chemical properties of pumpkin seed oil; using GC-MS analysis pumpkin Oil and fatty acid composition of trace elements of pumpkin seed oil; of supercritical CO2 extraction process of pumpkin seed oil Indochina Seeds grain mass transfer process mechanism;
Research results as follows:
1. More appropriate process parameters: inventory rating 200g, 4.50% moisture, the material size 5 mm, the extraction temperature 45℃, extraction pressure 30 Mpa, the extraction time 90 min, CO2 flow 15L/h, the temperature and pressure of separationⅠare 40℃and 8Mpa, the temperature of separationⅡis 30℃. the highest value of pumpkin seed oil extraction rate is 39.83%; General rotation test optimization process parameters, mathematical equations, Besides b44, b23, b34, the rest of the regression coefficients are observably in varying degrees, the extraction rate at the highest value of the factors combination: X1, 2; X2, 1; X3, -1; X4, 1. From the main effects model analysis of the factors we get that the big and small order of the factors affecting supercritical extracting pumpkin seed oil:extraction temperature> extraction pressure> CO2 flow> extraction time.
2. the crude protein content of pumpkin seed is 29.05%, fat content 39.83%, crude fiber content 19.21%, mineral content1.96%, water content 4.95%; pumpkin seed oil in the water and volatiles/(%) 0.09, but the share ( d204) 0.8917, color Y20R54, refractive index (20℃) 1.4639, acid value (KOH) /(mg/g) 0.6, the price of iodine (I2)/(g/kg) 17.6, saponification value (KOH ) /(mg/g) 168.6, peroxide value/(mg/g) 5.7. SCF-CO2 extraction of pumpkin seed oil all targets were reached international standards; acid storage with the value of the extension of the number of days the rising; extraction time extension of the transparency and color of oil getting worse; greater pressure on the oil extraction color deepenedⅠpressure from the higher transparency, better color; extraction higher the temperature, color and transparency of oil poor were identified six kinds of compounds; South Seeds of Zn/Cu ratio was 817; pumpkin seeds Trace Elements: 69μgFe/g, Ca 608μg/g, Zn 87μg/g, Cu 10μg/g, Mn 15μg/g, and other elements, including Mg content 2425μg/g, K content 3875μg/g, respectively.
3. By the test results and the quality of analysis and comparison, supercritical CO2 extraction method is better than soxhlet extraction and solvent soaking.
4. Analysis internal mass transfer process and the derivation of mathematical model equations in the process of supercritical CO2 extraction of pumpkin seed oil.
引文
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