【作者】 刘玲娜；

【导师】 冯光炷；

【作者基本信息】 河南工业大学 ， 生物化工， 2010， 硕士

【摘要】 磷脂酰胆碱(PC)是一种重要生理活性物质,在食品、保健品、医药、化妆品等行业得到广泛应用。目前出售的磷脂酰胆碱主要来源于大豆磷脂和蛋黄磷脂,菜籽磷脂与大豆磷脂的化学组成相似,但菜籽磷脂中硫甙、植酸等限制了菜籽磷脂的开发利用。随着双低油菜的广泛种植,菜籽磷脂可作为商品食用磷脂重要来源之一。我国菜籽油脚资源丰富,以菜籽油脚为原料萃取磷脂酰胆碱,具有成本低廉,菜籽油脚附加值高等优点。以菜籽油脚为原料,用超声辅助丙酮萃取粉末磷脂,在单因素实验的基础上,响应面法考察了液料(丙酮与粗磷脂)比、萃取时间、萃取温度及超声功率对磷脂含量的影响,建立超声辅助萃取粉末磷脂的二次多项数学模型。结果表明,最优的萃取条件为:液料比6.4mL/g、萃取时间9 min、萃取温度32℃、超声功率86 W。此条件下实验测得的磷脂含量91.06%,与拟合条件下模型得到的理论值91.74%较为吻合。同非超声条件下溶剂萃取法相比,超声萃取磷脂含量提高了3.82%,同时也缩短萃取时间。以粉末磷脂为原料,用超声辅助乙醇萃取磷脂酰胆碱,通过单因素实验得出的最佳萃取条件为:液料(乙醇与粉末磷脂)比6 mL/g,乙醇浓度95%,超声波功率200 W,萃取温度30℃,萃取时间30 min,萃取次数2次。以纯度和得率为双响应值,利用响应面法确定主要影响因素之间最佳比例关系为:萃取时间29 min、萃取温度30℃、乙醇浓度97%、液料比6.2 mL/g。据此测得磷脂酰胆碱纯度和得率的实际值分别为45.13%和50.67%。优化了电感耦合等离子体原子发射光谱法(ICP-AES)在不同消化条件(干法灰化和湿法消化)下测定菜籽粉末磷脂中磷含量的条件,并将优化后的ICP-AES法与钼蓝比色法在线性关系、精密度(RSD)、准确度方面进行了比较。在0~100 mg/L的范围内,ICP-AES法R~2=0.9999较钼蓝比色法R~2=0.997线性关系良好;钼蓝比色法、干法灰化和湿法消化处理样品的RSD分别为2.56%、1.47%和1.31%;其加样回收率分别在94.96%~100.22%、96.76%~101.73%和98.87%~102.36%之间,ICP-AES法磷的检出限为20.37μg/L。与钼蓝比色法相比较,ICP-AES法测磷含量结果无显著差异,回收率、精密度均达检测要求,操作简便、快速,检出限低。更多还原

【Abstract】 Phosphatidylcholine (PC) is an important physiological active substance, has been widely used in food, health products, pharmaceuticals, cosmetics and other industries. PC originates from the soybean and the yolk at present. The phospholipid of rape oil and the soybean phospholipid has the similar chemical composition, but the sulfuric glucoside and phytic acid in the phospholipid of rape oil has limited its development and utilization. With the double low rapeseed is widely planted, the rapeseed oil lecithin is one of the important resources of the edible commodity of lecithin. Our country is abundant in rapeseed oil sediment resources. Hence it is a direction of rapeseed to make use of rapeseed oil lecithin to prepare PC, which is cheap and valuable.In this research, using ultrasonic extraction method of extracting lecithin powder with the special resource of rape oil residue being raw material was proposed. On the basis of single factor experiments, the response surface method (RSM) was adopted to build a second order quadratic equation for ultrasonic-assisted extraction of lecithin powder. With the lecithin yield as the response index, the result showed that the optimum extraction condition was obtained as follows: ratio of liquid to solid of 6.4mL/g, extraction time of 9 minutes, extraction temperature of 32℃and ultrasonic power of 86 W. Under the optimum condition, the phospholipid yield was 91.06%. The optimized model by the RSM agreed well with practice. The ultrasonic-assisted extraction was more effective with lower extraction time than conventional extraction techniques.Using ultrasonic-assisted, powder lecithin was extracted with ethanol. The best conditions for the ultrasonic-assisted extraction techniques of PC in single factor experiments were: ratio of liquid to solid of 6 mL/g, ethanol concentration 95%, ultrasonic power 200 W, extraction temperature of 30℃, extraction time of 30 minutes, and times of extraction is twice. With the purity and rate as the response value, the functional relationship between main factors and response value were established, and the regression equation was obtained. The extraction parameters were optimized by the RSM as follows: extraction time of 29 minutes, extraction temperature of 30℃, and ethanol concentration of 97% and solid-liquid ratio of 6.2. The optimized extraction rate could reach 50.67% and the purity was 45.13%.To optimize an inductively coupled plasma atomic emission spectrometry (ICP-AES) of the different digestion methods (dry ashing and wet digestion) on the determination of the phosphorus content of phospholipid powder and then to determine the best measurement.The effects of different detection method (ICP-AES and Molybdenum blue spectrophotometry) were compared in the aspect of linear relationship, precision and accuracy. The linear range of phosphorous was 0~100mg/L (R~2= 0.9999); the precision (RSD) of Molybdenum blue spectrophotometry, dry ashing and wet digestion were2.56%, 1.47% and 1.31%; the recovery of Molybdenum blue spectrophotometry, dry ashing and wet digestion were in the range of 94.96%~100.22%, 96.76%~101.73% and 98.87%~102.36%; the detection limit of phosphorous was 20.37μg/L. There is no clear effect to use ICP-AES method and Molybdenum blue spectrophotometry to measure the content of phosphorous. The recovery and precision of ICP-AES are both up to the requirement. The method is simple, rapid and reliable with low direction limit.更多还原