超声波辅助萃取菜籽磷脂酰胆碱的研究
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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。
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.
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。
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.
引文
[1]赵超财.卵磷脂之制造与利用.食品科学技术专题讨论汇编(10号),食品工业发展研究所编印,1984.
[2]王永庆,姜宽.简述磷脂的性质及用途[J].黑河科技,2000: 1.
[3]卢行芳,卢荣.天然磷脂产品的加工及应用[M].化学工业出版社, 2004: 2-3.
[4]曹栋,裘爱泳,王兴国.磷脂及磷脂酰胆碱生物学功能[J].粮食与油脂,2002, (11):23-24.
[5] B.Rewald, J. Soc. Chem. Ind. 56, 403T(1937).
[6]陆艳,胡健华.双低油菜籽冷榨饼脱毒工艺的初步研究[J].粮油加工, 2005, 4: 14-16.
[7]卿中全,于炎湖,齐德生,等.双低菜籽(粕)的营养成分及抗营养因子的含量分析[J].饲料工业, 2000, 21(10): 26-28.
[8] Wetestein HR,Andrea,M,Kretmer.M.Effects of raw and modified canola lecithin compared to canola oil, canola seed and soy lecithin on ruminal fermentation measured with rumen simulation technique[J]. Animal Feed Science and Technology.2000, 85(1): 153-169.
[9]孔娟,刘晓宇,周仪.菜籽油脚中磷脂的研究进展[J] .农产品加工, 2008, 3: 4-7.
[10]刘元法,王兴国.大豆磷脂组成与特性[J].粮食与油脂, 2000, (3): 11-14.
[11]王晓辉,司南,叶爱英.植物油脚的综合利用[J].现代化工, 2006, 26(11): 21-24.
[12]陈宏伟,韦会方,李世平.菜籽磷脂生产工艺及其在水产养殖上的应用[J].中国油脂, 2003, 28(12): 80-81.
[13]彭可茂,席利卿.中国油菜籽的生产函数测定启示[J].统计与决策. 2007, 1: 41-42.
[14]油菜种植面积将扩大明年国内菜籽油价偏向利空.中国证券报, 2008.
[15]白满英,张金诚.大豆磷脂的营养保健功能[J].粮油食品, 2001, 9(5): 34-37.
[16] Willem Van Nienwenhuyzen. The Industrial Uses of Special Lecithin[J]. American Oil Chemist's Society, 1981(10): 886-888.
[17]徐生庚,裘爱泳主译.贝雷油脂化学与工艺学[M].第五版,中国轻工出版社, 2001, 318-327, 358-378.
[18]凌沛学,荣晓花.磷脂在保健食品和药品中的应用[J].山东食品科技, 2004, 2: 6-7.
[19] Kung, Viola Tze, et al. Liposome composition and method. WO 86 04, 232.
[20] Lawell, George H, et al. Submicron emulsions as vaccine adjuvants. WO 95 11, 700.
[21] Chagnon, Mark S. Electromagnetic wave absorbing, surface modified magnetic particles for use in medical applications, and their method of production. U.S.Pat. No5, 441, 746.
[22] Masek, Karel, et al. Czech CS 202, 245. 1878, 4, 9.
[23]刘燕华.卵磷脂技术发展现况及应用[J].食品工业, 1995, 27(12):8-12.
[24] Johnson.M.C.R. Chemical and Physical Properties of Phospholipids[J]. chem. And physic. Lip. 1973, (10): 318-322.
[25] Yates J. Leciyhin works wonders[J. Prevention, 1980, (32): 55-59.
[26] Candy DJ. Zeisel SH. Lecithin and choline in human health and disease[J], Nutr. Rer, 1994, (52): 27-29.
[27]徐世忠.卵磷脂的工业用途[J].化工新型材料, 27 (6): 37-38.
[28]张镜澄.超临界流体萃取[M].化学工业出版社, 2001.7.
[29] Feral Temelli. Extraction of Triglycerides and Phospholipids from Canola with Supercritical Carbon Dioxide and Ethanol [J]. Journal of Food Science, 1992, 57 (2): 440-442.
[30] Luigi Montanari, Paolo Fantozzi, Janet M Snyder, et al. Selective Extraction of Phospholipids from Soybeans with Supercritical Carbon Dioxide and Ethanol[J]. Journal of Supercritical Fluids, 1999, 14: 87-93.
[31]曾虹燕,方芳,蒋丽娟.超临界CO2萃取大豆油与大豆磷脂工艺条件研究[J].生物技术, 2003, 13 (2): 37-39.
[32] Leyla Teberikler, Sefa Koseoglu, Aydin Akgerman. Selective Extraction of Phosphatidylcholine from Lecithin by Supercritical Carbon Dioxide /Ethanol Mixture [J]. J. Am. Oil. Chem. Soc., 2001, 78 (2): 115-118.
[33]汪勇,王兴国,欧仕益,等.大豆磷脂酰胆碱分离、纯化和检测方法[J].粮食与油脂, 2003, 2: 6-8.
[34]徐晨.大豆卵磷脂的提纯研究[J].天然产物研究与开发, 1998, 10( 2): 75.
[35] Renkonen O. Breakdown of lecithin on aluminum oxide columns[J]. Lipid Research, 1962, l3( 2): 181-183.
[36] Shinho Kikuo, et al. Purification of PC. Japan Kokai Tokkyo koho. JP60197696.
[37] Liu Y F, Shan L, Wang X G. Purification of soybean phosphatidylcholine using D113-III ion exchange macro porous resin packed column chromatography[J]. J. Am. Oil Chem. Soc., 2009, 86: 183-188.
[38]王凤玲,刘爱国,朱宏吉.注射用大豆卵磷脂的提取纯化与质量分析[J].食品科学, 2005, 26(4): 183-186.
[39]胡小中,温光源,龙金林.磷脂分析检测技术研究进展[J].中国油脂, 2003, 28(3): 41-44.
[40]李立.大豆磷脂开发利用[J].粮食与油脂, 2001, 2: 33-36.
[41]韩轶,周扬,赵永芳.卵磷脂的提纯、鉴定及应用[J].氨基酸与生物资源, 2001, 23(2): 28-31.
[42] J.M.Nzai, A. Proctor. Soy lecithin phospholipids’determination by fourier transforms infrared spectroscopy and the acid[J]. JAOCS, 1999, 76(1): 61-66.
[43] J.M.Nzai, A. Proctor. Phospholipids determination in vegetable oil by thin-layer chromatography and imaging densitometry[J]. Food Chemistry, 1998, 63(4): 571-576.
[44]徐学兵.油脂化学[M].北京:中国商业出版社, 1993.
[45]孙秀燕,宋爱菊,张治国.单向薄层色谱技术分离磷脂的方法研究[J].沈阳药学院学报, 1992, 9(4): 262 -265.
[46] AMERICAN OIL CHEMISTS SOCIETY. Official methods and recommended practices of the American Oil Chemists Society [M]. 5thed.Section J: Lecithin. Ja7-86 Phospholipids in lecithin concentrates by thin-layer chromatography. Champaign, JAOCS press, 1998: 1-3.
[47] Arduino Arduini, Alessandro Peschechera. High performance liquid chromatography of long-chain acylcarnitie and phospholipids in fatty acid turnover studies[J], Journal of Lipid Research, 1996, 37: 684-689.
[48]冯会迎,胡忍乐,韩牛,等. HPLC-ELSD色谱法测定氢化大豆卵磷脂含量[J].中国油脂, 2003, 28(10): 43-45.
[49]施邑屏,黎燕斌,孙玲玲. 31P核磁共振光谱及薄层色谱分析针剂大豆卵磷脂[J].分析化学, 1991, 19(7): 733-736.
[50]章建浩等.干腌火腿工艺过程蛋白质与脂质分解氧化及其对风味的贡献[J].食品工业科技, 2003, 24 (12): 103-105.
[51] Grant R.Bartlett. Phosphorus Assay in Column Chromatography[J]. J.Chromatography, Vol. 234(3): 466-468.
[52]胡小中,温光源.磷脂分析检测技术研究进展[J].中国油脂, 2003, 28 (3): 41-44.
[53] J.M.Nzai, A. Proctor. Phospholipids determination in vegetable oil by thin-layer chromatography and imaging densitometry[J]. Food Chemistry, 1998, 63(4): 571-576.
[54]杨亦文,李艳. HPLC-RI法快速准确测定大豆磷脂酰胆碱含量[J].分析测试学报, 2003, 23 (5): 118-121.
[55]徐桂云,常理文.大豆磷脂组成的薄层色谱分析[J].分析化学, 1998, 26(1): 81-84.
[56] R.Przybylskl, N.A.M.Eskln. Phospholipid Composition of Canola Oils During the Early Stages of Processing as Measured by TLC with Flame Ionization Detector [J]. JAOCS, 1991, 68 (4): 241-245.
[57] Marian Sosada. Optimal Conditions for Fractionation of Rapeseed Lecithin with Alcohols[J]. JAOCS, 1993, 70(4): 405-410.
[58]李桂华,张根旺.粉末菜油磷脂饲用技术的研究[J].郑州粮食学院学报,1996, 7(3): 12-21.
[59]林光哲,李绍章,刘金银,等.从菜子油脚中直接萃取磷脂的工艺研究[J].湖北农业科学, 2003, 3: 83-86.
[60]赵海伶.菜籽油脚中磷脂的研究[D]. 2004,西南农业大学.
[61]杨兰花,钱俊青.乙醇萃取菜籽油卵磷脂的工艺研究[J].中国粮油学报, 2007, 22(4): 75-79.
[62]王丽君,王文焱,李致清. ICP-AES光谱仪的技术特点.现代仪器, 2005(3): 56-57.
[63]梁伟.电感耦合等离子体发射光谱法(ICP-AES)的分析和干扰机理研究[D]. 2007,中山大学.
[64]张经华,王辉,杨若明等.灰化ICP-AES法测定肉与肉类制品中总磷含量的研究[J].中央民族大学学报(自然科学版), 2003, 12(4): 307-310.
[65]魏丰华,牛林.全谱直读ICP光谱法测定磷酸氢钙中磷的含量[J].山东化工, 2002, 31(2): 39-40.
[66]辛仁轩.等离子体发射光谱分析[M].北京:化学工业出版社, 2005. 283-285.
[67]陈建国,江祖成,孔令英.光谱学与光谱分析[J], 1990, 10(6): 59.
[68]周毅,张福绥,杨红生,等.灰化法磷测定中不同灰化助剂的效果比较[J].分析实验室, 2001, 20(6): 58-61.
[69] Solórzano L, Sharp J H. Limaol. Oceanography., 1980, 25: 754-758.
[70]周毅,张福绥,杨红生,等.水环境中磷的灰化法提取[J].分析化学研究简报, 2002, 30(7): 86l-864.
[71]徐伯洪,闫慧芳.工作场所有害物质监测方法[M].北京:中国人民公安大学出版社, 2003: 28-29.
[72]项昭保,霍丹群.超声波在中草药化学成分提取中的应用[J].自然杂志, 2001, 23(5): 289-291.
[73]杨磊,唐晓溪,赵春建,等.响应面法优选桃儿七中的鬼臼毒素的超声提取工艺[J].化工进展, 2009, 28(2): 297-301.
[74]王昌利,杨景亮,宋小妹.超声技术在中草药提取方面的应用[J].陕西中医学院学报, 1993, 16 (3) : 33.
[75]冯若.超声手册[M].南京:南京大学出版社, 1999: 90.
[76]杜朝军,杨幼明.物理场强化萃取技术及应用[J].江西有色金属, 2003, 17(3): 34-36, 46.
[77]孙庆磊,梁月荣,陆建良.超声波在茶叶提取中的应用[J].茶叶, 2006, 32(2): 79-82.
[78] Suslick K S, Hammertion D A, Cline R E. The sonochemical hot spot [J]. J Am Chem. Soc, 1986, 108: 5641-5642.
[79]张斌,许莉勇.超声萃取技术研究与应用进展[J].浙江工业大学学报, 2008, 36(5): 558-561.
[80] MASON T J. Chemistry with ultrasound[R] Critical reports on applied chemistry, London and New York; Elsevier Science Publishers, 1990: 4-6.
[81]张健,蔡建国,杜福彦,等.山绿茶中黄酮的超声波提取研究[J].食品工业, 2006(1): 49-51.
[82]赵选民.试验设计方法[M].北京:科学出版社, 2006: 8.
[83]陈莉,屠康,王海,等.采用响应曲面法对采后红富士苹果热处理条件的优化[J].农业工程学报, 2006, 22(2): 159-163.
[84]李桂华.油料油脂检验与分析[M].化学工业出版社, 2006.
[85]杨磊,唐晓溪,赵春建,等.响应面法优选桃儿七中的鬼臼毒素的超声提取工艺[J].化工进展, 2009, 28(2): 297-301.
[2]王永庆,姜宽.简述磷脂的性质及用途[J].黑河科技,2000: 1.
[3]卢行芳,卢荣.天然磷脂产品的加工及应用[M].化学工业出版社, 2004: 2-3.
[4]曹栋,裘爱泳,王兴国.磷脂及磷脂酰胆碱生物学功能[J].粮食与油脂,2002, (11):23-24.
[5] B.Rewald, J. Soc. Chem. Ind. 56, 403T(1937).
[6]陆艳,胡健华.双低油菜籽冷榨饼脱毒工艺的初步研究[J].粮油加工, 2005, 4: 14-16.
[7]卿中全,于炎湖,齐德生,等.双低菜籽(粕)的营养成分及抗营养因子的含量分析[J].饲料工业, 2000, 21(10): 26-28.
[8] Wetestein HR,Andrea,M,Kretmer.M.Effects of raw and modified canola lecithin compared to canola oil, canola seed and soy lecithin on ruminal fermentation measured with rumen simulation technique[J]. Animal Feed Science and Technology.2000, 85(1): 153-169.
[9]孔娟,刘晓宇,周仪.菜籽油脚中磷脂的研究进展[J] .农产品加工, 2008, 3: 4-7.
[10]刘元法,王兴国.大豆磷脂组成与特性[J].粮食与油脂, 2000, (3): 11-14.
[11]王晓辉,司南,叶爱英.植物油脚的综合利用[J].现代化工, 2006, 26(11): 21-24.
[12]陈宏伟,韦会方,李世平.菜籽磷脂生产工艺及其在水产养殖上的应用[J].中国油脂, 2003, 28(12): 80-81.
[13]彭可茂,席利卿.中国油菜籽的生产函数测定启示[J].统计与决策. 2007, 1: 41-42.
[14]油菜种植面积将扩大明年国内菜籽油价偏向利空.中国证券报, 2008.
[15]白满英,张金诚.大豆磷脂的营养保健功能[J].粮油食品, 2001, 9(5): 34-37.
[16] Willem Van Nienwenhuyzen. The Industrial Uses of Special Lecithin[J]. American Oil Chemist's Society, 1981(10): 886-888.
[17]徐生庚,裘爱泳主译.贝雷油脂化学与工艺学[M].第五版,中国轻工出版社, 2001, 318-327, 358-378.
[18]凌沛学,荣晓花.磷脂在保健食品和药品中的应用[J].山东食品科技, 2004, 2: 6-7.
[19] Kung, Viola Tze, et al. Liposome composition and method. WO 86 04, 232.
[20] Lawell, George H, et al. Submicron emulsions as vaccine adjuvants. WO 95 11, 700.
[21] Chagnon, Mark S. Electromagnetic wave absorbing, surface modified magnetic particles for use in medical applications, and their method of production. U.S.Pat. No5, 441, 746.
[22] Masek, Karel, et al. Czech CS 202, 245. 1878, 4, 9.
[23]刘燕华.卵磷脂技术发展现况及应用[J].食品工业, 1995, 27(12):8-12.
[24] Johnson.M.C.R. Chemical and Physical Properties of Phospholipids[J]. chem. And physic. Lip. 1973, (10): 318-322.
[25] Yates J. Leciyhin works wonders[J. Prevention, 1980, (32): 55-59.
[26] Candy DJ. Zeisel SH. Lecithin and choline in human health and disease[J], Nutr. Rer, 1994, (52): 27-29.
[27]徐世忠.卵磷脂的工业用途[J].化工新型材料, 27 (6): 37-38.
[28]张镜澄.超临界流体萃取[M].化学工业出版社, 2001.7.
[29] Feral Temelli. Extraction of Triglycerides and Phospholipids from Canola with Supercritical Carbon Dioxide and Ethanol [J]. Journal of Food Science, 1992, 57 (2): 440-442.
[30] Luigi Montanari, Paolo Fantozzi, Janet M Snyder, et al. Selective Extraction of Phospholipids from Soybeans with Supercritical Carbon Dioxide and Ethanol[J]. Journal of Supercritical Fluids, 1999, 14: 87-93.
[31]曾虹燕,方芳,蒋丽娟.超临界CO2萃取大豆油与大豆磷脂工艺条件研究[J].生物技术, 2003, 13 (2): 37-39.
[32] Leyla Teberikler, Sefa Koseoglu, Aydin Akgerman. Selective Extraction of Phosphatidylcholine from Lecithin by Supercritical Carbon Dioxide /Ethanol Mixture [J]. J. Am. Oil. Chem. Soc., 2001, 78 (2): 115-118.
[33]汪勇,王兴国,欧仕益,等.大豆磷脂酰胆碱分离、纯化和检测方法[J].粮食与油脂, 2003, 2: 6-8.
[34]徐晨.大豆卵磷脂的提纯研究[J].天然产物研究与开发, 1998, 10( 2): 75.
[35] Renkonen O. Breakdown of lecithin on aluminum oxide columns[J]. Lipid Research, 1962, l3( 2): 181-183.
[36] Shinho Kikuo, et al. Purification of PC. Japan Kokai Tokkyo koho. JP60197696.
[37] Liu Y F, Shan L, Wang X G. Purification of soybean phosphatidylcholine using D113-III ion exchange macro porous resin packed column chromatography[J]. J. Am. Oil Chem. Soc., 2009, 86: 183-188.
[38]王凤玲,刘爱国,朱宏吉.注射用大豆卵磷脂的提取纯化与质量分析[J].食品科学, 2005, 26(4): 183-186.
[39]胡小中,温光源,龙金林.磷脂分析检测技术研究进展[J].中国油脂, 2003, 28(3): 41-44.
[40]李立.大豆磷脂开发利用[J].粮食与油脂, 2001, 2: 33-36.
[41]韩轶,周扬,赵永芳.卵磷脂的提纯、鉴定及应用[J].氨基酸与生物资源, 2001, 23(2): 28-31.
[42] J.M.Nzai, A. Proctor. Soy lecithin phospholipids’determination by fourier transforms infrared spectroscopy and the acid[J]. JAOCS, 1999, 76(1): 61-66.
[43] J.M.Nzai, A. Proctor. Phospholipids determination in vegetable oil by thin-layer chromatography and imaging densitometry[J]. Food Chemistry, 1998, 63(4): 571-576.
[44]徐学兵.油脂化学[M].北京:中国商业出版社, 1993.
[45]孙秀燕,宋爱菊,张治国.单向薄层色谱技术分离磷脂的方法研究[J].沈阳药学院学报, 1992, 9(4): 262 -265.
[46] AMERICAN OIL CHEMISTS SOCIETY. Official methods and recommended practices of the American Oil Chemists Society [M]. 5thed.Section J: Lecithin. Ja7-86 Phospholipids in lecithin concentrates by thin-layer chromatography. Champaign, JAOCS press, 1998: 1-3.
[47] Arduino Arduini, Alessandro Peschechera. High performance liquid chromatography of long-chain acylcarnitie and phospholipids in fatty acid turnover studies[J], Journal of Lipid Research, 1996, 37: 684-689.
[48]冯会迎,胡忍乐,韩牛,等. HPLC-ELSD色谱法测定氢化大豆卵磷脂含量[J].中国油脂, 2003, 28(10): 43-45.
[49]施邑屏,黎燕斌,孙玲玲. 31P核磁共振光谱及薄层色谱分析针剂大豆卵磷脂[J].分析化学, 1991, 19(7): 733-736.
[50]章建浩等.干腌火腿工艺过程蛋白质与脂质分解氧化及其对风味的贡献[J].食品工业科技, 2003, 24 (12): 103-105.
[51] Grant R.Bartlett. Phosphorus Assay in Column Chromatography[J]. J.Chromatography, Vol. 234(3): 466-468.
[52]胡小中,温光源.磷脂分析检测技术研究进展[J].中国油脂, 2003, 28 (3): 41-44.
[53] J.M.Nzai, A. Proctor. Phospholipids determination in vegetable oil by thin-layer chromatography and imaging densitometry[J]. Food Chemistry, 1998, 63(4): 571-576.
[54]杨亦文,李艳. HPLC-RI法快速准确测定大豆磷脂酰胆碱含量[J].分析测试学报, 2003, 23 (5): 118-121.
[55]徐桂云,常理文.大豆磷脂组成的薄层色谱分析[J].分析化学, 1998, 26(1): 81-84.
[56] R.Przybylskl, N.A.M.Eskln. Phospholipid Composition of Canola Oils During the Early Stages of Processing as Measured by TLC with Flame Ionization Detector [J]. JAOCS, 1991, 68 (4): 241-245.
[57] Marian Sosada. Optimal Conditions for Fractionation of Rapeseed Lecithin with Alcohols[J]. JAOCS, 1993, 70(4): 405-410.
[58]李桂华,张根旺.粉末菜油磷脂饲用技术的研究[J].郑州粮食学院学报,1996, 7(3): 12-21.
[59]林光哲,李绍章,刘金银,等.从菜子油脚中直接萃取磷脂的工艺研究[J].湖北农业科学, 2003, 3: 83-86.
[60]赵海伶.菜籽油脚中磷脂的研究[D]. 2004,西南农业大学.
[61]杨兰花,钱俊青.乙醇萃取菜籽油卵磷脂的工艺研究[J].中国粮油学报, 2007, 22(4): 75-79.
[62]王丽君,王文焱,李致清. ICP-AES光谱仪的技术特点.现代仪器, 2005(3): 56-57.
[63]梁伟.电感耦合等离子体发射光谱法(ICP-AES)的分析和干扰机理研究[D]. 2007,中山大学.
[64]张经华,王辉,杨若明等.灰化ICP-AES法测定肉与肉类制品中总磷含量的研究[J].中央民族大学学报(自然科学版), 2003, 12(4): 307-310.
[65]魏丰华,牛林.全谱直读ICP光谱法测定磷酸氢钙中磷的含量[J].山东化工, 2002, 31(2): 39-40.
[66]辛仁轩.等离子体发射光谱分析[M].北京:化学工业出版社, 2005. 283-285.
[67]陈建国,江祖成,孔令英.光谱学与光谱分析[J], 1990, 10(6): 59.
[68]周毅,张福绥,杨红生,等.灰化法磷测定中不同灰化助剂的效果比较[J].分析实验室, 2001, 20(6): 58-61.
[69] Solórzano L, Sharp J H. Limaol. Oceanography., 1980, 25: 754-758.
[70]周毅,张福绥,杨红生,等.水环境中磷的灰化法提取[J].分析化学研究简报, 2002, 30(7): 86l-864.
[71]徐伯洪,闫慧芳.工作场所有害物质监测方法[M].北京:中国人民公安大学出版社, 2003: 28-29.
[72]项昭保,霍丹群.超声波在中草药化学成分提取中的应用[J].自然杂志, 2001, 23(5): 289-291.
[73]杨磊,唐晓溪,赵春建,等.响应面法优选桃儿七中的鬼臼毒素的超声提取工艺[J].化工进展, 2009, 28(2): 297-301.
[74]王昌利,杨景亮,宋小妹.超声技术在中草药提取方面的应用[J].陕西中医学院学报, 1993, 16 (3) : 33.
[75]冯若.超声手册[M].南京:南京大学出版社, 1999: 90.
[76]杜朝军,杨幼明.物理场强化萃取技术及应用[J].江西有色金属, 2003, 17(3): 34-36, 46.
[77]孙庆磊,梁月荣,陆建良.超声波在茶叶提取中的应用[J].茶叶, 2006, 32(2): 79-82.
[78] Suslick K S, Hammertion D A, Cline R E. The sonochemical hot spot [J]. J Am Chem. Soc, 1986, 108: 5641-5642.
[79]张斌,许莉勇.超声萃取技术研究与应用进展[J].浙江工业大学学报, 2008, 36(5): 558-561.
[80] MASON T J. Chemistry with ultrasound[R] Critical reports on applied chemistry, London and New York; Elsevier Science Publishers, 1990: 4-6.
[81]张健,蔡建国,杜福彦,等.山绿茶中黄酮的超声波提取研究[J].食品工业, 2006(1): 49-51.
[82]赵选民.试验设计方法[M].北京:科学出版社, 2006: 8.
[83]陈莉,屠康,王海,等.采用响应曲面法对采后红富士苹果热处理条件的优化[J].农业工程学报, 2006, 22(2): 159-163.
[84]李桂华.油料油脂检验与分析[M].化学工业出版社, 2006.
[85]杨磊,唐晓溪,赵春建,等.响应面法优选桃儿七中的鬼臼毒素的超声提取工艺[J].化工进展, 2009, 28(2): 297-301.