豆油脱臭馏出物酶法甲酯化纯化V_E的研究
|
摘要
本文以豆油脱臭馏出物为原料,以Novoyme 435酶为催化剂,对馏出物的间歇式和连续式酶法甲酯化工艺进行了研究,并对该反应的动力学规律进行了探索。对甲酯化产物进行了转酯化反应、甾醇分离和分子蒸馏研究,富集了高纯度的维生素E;对分离精制植物甾醇的工艺进行了摸索,同时对维生素E在鱼油中的抗氧化效果进行了考查。
首先对豆油脱臭馏出物的组成和基本性质进行了测定并对其进行了刮膜式蒸发器脱水试验。水分含量由1.3g/kg降低至0.3g/kg。在Novoyme 435酶的作用下,对影响馏出物中脂肪酸甲酯化酯化率的因素:时间、酶用量、温度和底物比进行了单因素试验,并通过正交优化试验,发现影响酯化率的主要因素是反应时间和酶用量,其次为反应温度和底物比。经极差分析并综合各因素,确定四因素的最佳组合条件为酸醇摩尔比1:1.5,酶用量60plu/g,反应温度55℃,反应时间8h,该条件下酯化率为95.86%。薄层分析证实了豆油脱臭馏出物中的游离脂肪酸酶法甲酯化后转化为脂肪酸甲酯,其中的甘油酯并未甲酯化。甲酯化产物经20℃结晶,过滤分离,得粗甾醇,其纯度质量分数为54.01%,保留率为74.32%,分离甾醇后的甲酯化产物中维生素E含量质量分数为10.07%,保留率为98.35%。经甲酯化处理并脱除甲醇、水和甾醇后,维生素E的总保留率为95.86%。
对脂肪酶催化豆油脱臭馏出物中的游离脂肪酸与甲醇的酯合成反应动力学进行了研究。从不同加酶量条件下反应初速度的变化研究,表明反应初速度随加酶量的增加而线性增加,酯化反应受动力学控制。并对反应的机理进行了初步推断,分析表明该甲酯化反应符合乒乓反应机制,并对其初速度动力学方程进行了推导,方程参数拟合表明实验值与计算值的趋势基本一致,反应机理推断和模型推导所作的假设合理。
采用填充床反应器对连续式酶法甲酯化工艺进行了研究,考察了反应温度、底物比、进料速度、酶柱高、进料速度比值和分子筛用量对甲酯化酯化率的影响,对底物比、反应温度、进料速度比值进行三因素三水平正交实验,发现影响酯化率大小的因素依次是底物比、反应温度、进料速度比值。经极差分析,确定最佳反应条件为酸醇摩尔比1:2,进料速度比值0.075ml/min·cm,反应温度55℃,该条件下酯化率可达90.87%。该反应体系下,Novoyme 435酶的半衰期为45h。
其次,对初步分离甾醇后的酶甲酯化产物利用甲醇钠催化其中甘油酯与甲醇发生转酯化反应,反应条件为0.5%(W/W油基)甲醇钠,0.7:1(V/W)甲醇,温度70℃,反应时间1h,经甘油分析表明原料体系中的甘油酯成分得到了较好的转化。此时维生素E含量质量分数10.14%,保留率96.27%。
同时对不同冷析温度分离甾醇后的转酯化产物的脂肪酸组成和运动粘度进行了测定,并对滤饼中甾醇的纯度和保留率进行了分析,确定采用5℃冷析转酯化产物分离甾醇。
对转酯化产物经分子蒸馏富集维生素E的工艺进行了研究。考察了一次蒸馏温度、二次蒸馏温度、进料速率、蒸馏压力以及刮膜器转速对产品维生素E含量和得率的影响。通过响应面分析,确定了二次蒸馏温度、进料速率、刮膜器转速对维生素E含量影响的回归方程,确定了最佳工艺:进料速度98.0～99.0ml/h,刮膜器转速156.0～157.0r/min,一次蒸馏温度110℃,二次蒸馏温度151～152℃,压力0.1Pa,维生素E含量可达质量分数50.98%,得率60.21%。对分子蒸馏的次数进行了研究,3次蒸馏后,维生素E含量质量分数为73.31%,得率为50.25%;4次蒸馏后,维生素E含量质量分数为85.35%,得率为45.62%。
对冷析分离得到的粗甾醇进行了溶剂萃取洗脱的精制工艺研究,通过甾醇纯度和得率及经济性分析,选择正己烷作为粗甾醇洗脱剂;通过单因素实验和响应面分析,建立了甾醇纯度和得率回归方程,并进行了方差分析和显著性检验,确定了最佳工艺条件:液料比16.7:1,温度30℃,时间10min;该条件下,验证试验结果:甾醇纯度质量分数为85.10%,得率77.51%。产品经三次洗涤,纯度达到质量分数95.34%,得率为49.47%。
天然维生素E为鱼油的特定抗氧化剂。以甘三酯型鱼油及乙酯型鱼油为原料,通过烘箱法耐热试验发现维生素E确实能够阻止鱼油的自动氧化。试验同时发现EPA,DHA含量质量分数30%鱼油中添加质量分数0.1%的天然V_E,比添加质量分数为0.12%V_E的抗氧化效果要好,可使鱼油的保质期延长144天。在EPA和DHA含量质量分数80%的鱼油中添加质量分数0.12%的天然V_E时,其抗氧化效果较好。
In this paper,intermittent and continuous enzymatic processes of methyl esterification on soybean oil deodorized distillate(SODD)as raw materials,using lipase Novoyme 435 as a catalyst were studied,and the mechanism of the the reaction kinetics was also investigated.After methyl esterification and molecular distillation,we enriched and refined high-purity vitamin E, and studied the process of separating and refining plants sterol from the methyl esterifing production.We also test the antioxidant effect of the vitamin E in the fish oil.
Firstly,on the composition of raw materials(SODD) were determined,and the dehydration test was done.The moisture content decreased from 1.3g/kg to 0.3g/kg.The single factors test which impact the conversion of fatty acids to methyl ester was carried out.Through orthogonal process optimization experiments,we found that the main factors affecting the conversion were the enzyme dosage and reaction time,and that temperature and substrate ratio were of secondary interest.Using the extreme analysis and comprehensive analysis,we obtained the best combination of four factors.They are the acid conditions of methanol molar ratio of 1:1.5;the enzyme dosage 60 plu/g;the reaction temperature 55℃;and the reaction time 8 hours.The conversion rate under the conditions was 95.86%.The TLC analysis verified that most of the fatty acids from the SODD converted into fatty acid methyl ester,but that triglyceride did not change.The purity of sterol which was crystallized at 20℃,from the product of methyl esterification and separated by filtration was 54.01%,the preserving rate was 74.32%.The content of V_E in SODD was 10.07%and the preserving rate of vitamin E was 98.35%after removing sterols.After the methanol,sterols and moisture were removed,the total preserving rate of vitamin E was 95.86%.
The reaction kinetics of lipase catalysis of SODD and methanol synthesis was studied.First of all,the studies of the influence of different enzyme dosage to the initial velocity showed that the initial velocity of the reaction linearly increased with the enzyme dosage increase,and esterification reaction was controlled by its kinetic.Secondly,with the inference of the reaction mechanism,the analysis showed that the reaction of methyl esterification conformed to accord with ping pong response mechanisms.Their initial velocity of the kinetic equations was derived. It was found that after fitting and of trending the parameters of the equation the calculated values were in agreement with the experimental data,reaction mechanism and model inferred is reasonable assumptions.
The continuous process of methyl esterification of SODD was investigated by using fill-bed reactor.The conversion of fatty acids to methyl esters was optimized by using a statistical design.Through the single factor experimental and the orthogonal experiment,each influence factor(under experimental condition which the influence order in this experiment applies) to the response was:the substrate ratio＞the reaction temperature＞the input speed ratio. The optimum methyl esterification response conditions were:substrate ratio:1:2,temperature: 55℃,the input speed 0.075ml/min·cm.The obtained conversion rate was 90.87%.Under the optimum condition,the half-life of the Novoyme 435 is 45 hours.
Secondly,by using sodium methoxide in the SODD that had been methyl esterficated and separated sterols,triglyceride and methanol were reacted.The reaction conditions were the 0.5% (W/W oil-based) sodium methoxide,0.7:1(V/W) methanol,temperature 70℃,the reaction time 1h.Glycerol analysis showed trilyceride components had been better conversion.The purity of vitamin E was 10.14%,the preserving rate was 96.27%.
The kinematic viscosity of esterification product which had been crystallized under different temperature and separated sterols was analysed,and the sterol purity and the recovery rate were analyzed,then 5℃was determined to be the temperature of crystallization of esterification.
Application of the molecular distillation process to enrich vitamin E of SODD was studied. It was tested that was first distillation temperature,second distillation temperature,feed rate, distillation pressure,speed scraping rate and times of distillation which impact the purity and recovery rate of the vitamin E.Through response surface analysis,the effects of second distillation temperature,feed rate,scraping speed on vitamin E content were set up in the regression equation,and the optimum experimental condition was identified:first distillation temperature of 110℃,the second distillation temperature of 151～152℃,press 0.1Pa,feed speed 98～99 ml/h,scraping speed 156.0～157.0r/min.Under the best conditions,the content of vitamin E was up to 50.98%,and the recovery rate reached to 60.21%.The times of distillation was studied,the content of vitamin E was 73.31%,and the recovery rate was 50.25%by three times distillation;the content of vitamin E was 85.35%,and the recovery rate only was 45.62%by four times distillation.
Solvent extraction method was used to refine sterols.Through sterol purity and obtaining ratio and economic analysis,hexane was chosen as a washing decolorization agent for the raw sterols;Through the single factor experiments and response surface analysis,a regression equation was set up,and a significant test was done,the optimum conditions were determined: hexane to material 16.7:1,temperature 30℃,and time 10min.The confirmation test results verified that sterol purity was up to 85.10%,the recovery rate was 77.51%under the optimum conditions.The sterol purity was 95.34%,but the obtaining ratio was only 49.47%after 3 times of hexane extractions.
Natural vitamin E is a better antioxidant in fish oil.Using glyceride fish oil and ethyl fish oil as raw materials,through heat-resistant test we found that vitamin E can indeed prevent fish oil from automatic oxidation.Compared to adding 0.12%mass fraction of the natural vitamin E, the oil containing 30%EPA and DHA which was added 0.1%mass fraction of the natural vitamin E had better antioxidant effect.The shelf-life can be extended to 144 days.For the fish oil containing 80%EPA and DHA with the addition of 0.12%natural vitamin E,its antioxidant effect was better.
首先对豆油脱臭馏出物的组成和基本性质进行了测定并对其进行了刮膜式蒸发器脱水试验。水分含量由1.3g/kg降低至0.3g/kg。在Novoyme 435酶的作用下,对影响馏出物中脂肪酸甲酯化酯化率的因素:时间、酶用量、温度和底物比进行了单因素试验,并通过正交优化试验,发现影响酯化率的主要因素是反应时间和酶用量,其次为反应温度和底物比。经极差分析并综合各因素,确定四因素的最佳组合条件为酸醇摩尔比1:1.5,酶用量60plu/g,反应温度55℃,反应时间8h,该条件下酯化率为95.86%。薄层分析证实了豆油脱臭馏出物中的游离脂肪酸酶法甲酯化后转化为脂肪酸甲酯,其中的甘油酯并未甲酯化。甲酯化产物经20℃结晶,过滤分离,得粗甾醇,其纯度质量分数为54.01%,保留率为74.32%,分离甾醇后的甲酯化产物中维生素E含量质量分数为10.07%,保留率为98.35%。经甲酯化处理并脱除甲醇、水和甾醇后,维生素E的总保留率为95.86%。
对脂肪酶催化豆油脱臭馏出物中的游离脂肪酸与甲醇的酯合成反应动力学进行了研究。从不同加酶量条件下反应初速度的变化研究,表明反应初速度随加酶量的增加而线性增加,酯化反应受动力学控制。并对反应的机理进行了初步推断,分析表明该甲酯化反应符合乒乓反应机制,并对其初速度动力学方程进行了推导,方程参数拟合表明实验值与计算值的趋势基本一致,反应机理推断和模型推导所作的假设合理。
采用填充床反应器对连续式酶法甲酯化工艺进行了研究,考察了反应温度、底物比、进料速度、酶柱高、进料速度比值和分子筛用量对甲酯化酯化率的影响,对底物比、反应温度、进料速度比值进行三因素三水平正交实验,发现影响酯化率大小的因素依次是底物比、反应温度、进料速度比值。经极差分析,确定最佳反应条件为酸醇摩尔比1:2,进料速度比值0.075ml/min·cm,反应温度55℃,该条件下酯化率可达90.87%。该反应体系下,Novoyme 435酶的半衰期为45h。
其次,对初步分离甾醇后的酶甲酯化产物利用甲醇钠催化其中甘油酯与甲醇发生转酯化反应,反应条件为0.5%(W/W油基)甲醇钠,0.7:1(V/W)甲醇,温度70℃,反应时间1h,经甘油分析表明原料体系中的甘油酯成分得到了较好的转化。此时维生素E含量质量分数10.14%,保留率96.27%。
同时对不同冷析温度分离甾醇后的转酯化产物的脂肪酸组成和运动粘度进行了测定,并对滤饼中甾醇的纯度和保留率进行了分析,确定采用5℃冷析转酯化产物分离甾醇。
对转酯化产物经分子蒸馏富集维生素E的工艺进行了研究。考察了一次蒸馏温度、二次蒸馏温度、进料速率、蒸馏压力以及刮膜器转速对产品维生素E含量和得率的影响。通过响应面分析,确定了二次蒸馏温度、进料速率、刮膜器转速对维生素E含量影响的回归方程,确定了最佳工艺:进料速度98.0～99.0ml/h,刮膜器转速156.0～157.0r/min,一次蒸馏温度110℃,二次蒸馏温度151～152℃,压力0.1Pa,维生素E含量可达质量分数50.98%,得率60.21%。对分子蒸馏的次数进行了研究,3次蒸馏后,维生素E含量质量分数为73.31%,得率为50.25%;4次蒸馏后,维生素E含量质量分数为85.35%,得率为45.62%。
对冷析分离得到的粗甾醇进行了溶剂萃取洗脱的精制工艺研究,通过甾醇纯度和得率及经济性分析,选择正己烷作为粗甾醇洗脱剂;通过单因素实验和响应面分析,建立了甾醇纯度和得率回归方程,并进行了方差分析和显著性检验,确定了最佳工艺条件:液料比16.7:1,温度30℃,时间10min;该条件下,验证试验结果:甾醇纯度质量分数为85.10%,得率77.51%。产品经三次洗涤,纯度达到质量分数95.34%,得率为49.47%。
天然维生素E为鱼油的特定抗氧化剂。以甘三酯型鱼油及乙酯型鱼油为原料,通过烘箱法耐热试验发现维生素E确实能够阻止鱼油的自动氧化。试验同时发现EPA,DHA含量质量分数30%鱼油中添加质量分数0.1%的天然V_E,比添加质量分数为0.12%V_E的抗氧化效果要好,可使鱼油的保质期延长144天。在EPA和DHA含量质量分数80%的鱼油中添加质量分数0.12%的天然V_E时,其抗氧化效果较好。
In this paper,intermittent and continuous enzymatic processes of methyl esterification on soybean oil deodorized distillate(SODD)as raw materials,using lipase Novoyme 435 as a catalyst were studied,and the mechanism of the the reaction kinetics was also investigated.After methyl esterification and molecular distillation,we enriched and refined high-purity vitamin E, and studied the process of separating and refining plants sterol from the methyl esterifing production.We also test the antioxidant effect of the vitamin E in the fish oil.
Firstly,on the composition of raw materials(SODD) were determined,and the dehydration test was done.The moisture content decreased from 1.3g/kg to 0.3g/kg.The single factors test which impact the conversion of fatty acids to methyl ester was carried out.Through orthogonal process optimization experiments,we found that the main factors affecting the conversion were the enzyme dosage and reaction time,and that temperature and substrate ratio were of secondary interest.Using the extreme analysis and comprehensive analysis,we obtained the best combination of four factors.They are the acid conditions of methanol molar ratio of 1:1.5;the enzyme dosage 60 plu/g;the reaction temperature 55℃;and the reaction time 8 hours.The conversion rate under the conditions was 95.86%.The TLC analysis verified that most of the fatty acids from the SODD converted into fatty acid methyl ester,but that triglyceride did not change.The purity of sterol which was crystallized at 20℃,from the product of methyl esterification and separated by filtration was 54.01%,the preserving rate was 74.32%.The content of V_E in SODD was 10.07%and the preserving rate of vitamin E was 98.35%after removing sterols.After the methanol,sterols and moisture were removed,the total preserving rate of vitamin E was 95.86%.
The reaction kinetics of lipase catalysis of SODD and methanol synthesis was studied.First of all,the studies of the influence of different enzyme dosage to the initial velocity showed that the initial velocity of the reaction linearly increased with the enzyme dosage increase,and esterification reaction was controlled by its kinetic.Secondly,with the inference of the reaction mechanism,the analysis showed that the reaction of methyl esterification conformed to accord with ping pong response mechanisms.Their initial velocity of the kinetic equations was derived. It was found that after fitting and of trending the parameters of the equation the calculated values were in agreement with the experimental data,reaction mechanism and model inferred is reasonable assumptions.
The continuous process of methyl esterification of SODD was investigated by using fill-bed reactor.The conversion of fatty acids to methyl esters was optimized by using a statistical design.Through the single factor experimental and the orthogonal experiment,each influence factor(under experimental condition which the influence order in this experiment applies) to the response was:the substrate ratio＞the reaction temperature＞the input speed ratio. The optimum methyl esterification response conditions were:substrate ratio:1:2,temperature: 55℃,the input speed 0.075ml/min·cm.The obtained conversion rate was 90.87%.Under the optimum condition,the half-life of the Novoyme 435 is 45 hours.
Secondly,by using sodium methoxide in the SODD that had been methyl esterficated and separated sterols,triglyceride and methanol were reacted.The reaction conditions were the 0.5% (W/W oil-based) sodium methoxide,0.7:1(V/W) methanol,temperature 70℃,the reaction time 1h.Glycerol analysis showed trilyceride components had been better conversion.The purity of vitamin E was 10.14%,the preserving rate was 96.27%.
The kinematic viscosity of esterification product which had been crystallized under different temperature and separated sterols was analysed,and the sterol purity and the recovery rate were analyzed,then 5℃was determined to be the temperature of crystallization of esterification.
Application of the molecular distillation process to enrich vitamin E of SODD was studied. It was tested that was first distillation temperature,second distillation temperature,feed rate, distillation pressure,speed scraping rate and times of distillation which impact the purity and recovery rate of the vitamin E.Through response surface analysis,the effects of second distillation temperature,feed rate,scraping speed on vitamin E content were set up in the regression equation,and the optimum experimental condition was identified:first distillation temperature of 110℃,the second distillation temperature of 151～152℃,press 0.1Pa,feed speed 98～99 ml/h,scraping speed 156.0～157.0r/min.Under the best conditions,the content of vitamin E was up to 50.98%,and the recovery rate reached to 60.21%.The times of distillation was studied,the content of vitamin E was 73.31%,and the recovery rate was 50.25%by three times distillation;the content of vitamin E was 85.35%,and the recovery rate only was 45.62%by four times distillation.
Solvent extraction method was used to refine sterols.Through sterol purity and obtaining ratio and economic analysis,hexane was chosen as a washing decolorization agent for the raw sterols;Through the single factor experiments and response surface analysis,a regression equation was set up,and a significant test was done,the optimum conditions were determined: hexane to material 16.7:1,temperature 30℃,and time 10min.The confirmation test results verified that sterol purity was up to 85.10%,the recovery rate was 77.51%under the optimum conditions.The sterol purity was 95.34%,but the obtaining ratio was only 49.47%after 3 times of hexane extractions.
Natural vitamin E is a better antioxidant in fish oil.Using glyceride fish oil and ethyl fish oil as raw materials,through heat-resistant test we found that vitamin E can indeed prevent fish oil from automatic oxidation.Compared to adding 0.12%mass fraction of the natural vitamin E, the oil containing 30%EPA and DHA which was added 0.1%mass fraction of the natural vitamin E had better antioxidant effect.The shelf-life can be extended to 144 days.For the fish oil containing 80%EPA and DHA with the addition of 0.12%natural vitamin E,its antioxidant effect was better.
引文
[1]杨世安.维生素E[M].中国化工百科全书(第16卷).北京;化学工业出版社,1997
[2]梁诚.天然维生素E生产现状与应用前景[J].化工技术经济,2002(8)4:29-31
[3]王瑞元.中国油脂工业的现状与发展趋势[J].中国油脂,2006(31)11:7-11
[4]刘玉兰.植物油脂生产与综合利用[M].北京:中国轻工业出版社,1999
[5]雷炳福.油脂脱臭馏出物的组成与市场前景[J].中国油脂,2002,27(1):75-78
[6]吴时敏.功能性油脂[M].北京:中国轻工业出版社,2001
[7]樊明涛、吴守一、马海乐.从油脂脱臭馏出物中提取生育酚的研究概况[J].西北农林科技大学学报(自然科学版),2002,30(增刊):73-77,
[8]Kirk-Othmer.Encyclopedia of Chemical Technology,Third Edition,Vol 24[M].New Yord:John Wiely,1984
[9]IUPAC-IUB Joint Commission on Biochemical Nomenclature.Nomenclature of Tocopherols and Related Compounds:Recommendations 1981[J].Eur.J.Biochem,1982(123):473-475
[10]国家药典委员会.中华人民共和国药典2000年版2部[M].北京:化学工业出版社,2000.
[11]全国食品添加剂标准化技术委员会.GB19191-2003食品添加剂-天然维生素E[S].北京:中国标准出版社,2003.
[12]尤新.天然维生素E的生理功能和开发前景分析[J].中国食品添加剂,2000,4:30-33
[13]Fernholz,E.On the constitution of a-Tocopherol[J],J.Am.Chen.Soc,1938(60),700-705.
[14]Nelan,D.R,C.D.Robseson,The oxidation product from a-tcopherol and potassium ferricyanide and its reaction with ascorbic and hydrochloric acids[J],
[15]FDA.the united states pharmacopeia ⅩⅩⅣ[M].USA:2000
[16]Institute of Medicine of the National Academy of Sciences.Food chemicals codex,4th ed.,[M]USA.1996
[17]中华人民共和国卫生部药典委员会.中华人民共和国药典 二部[M].北京:化学工业出版社,1980
[18]邵斌.天然d-a-维生素[J].中国食品添加剂,2000(20)4:78-83
[19]梁诚.天然维生素E生产现状与应用前景[J].化工技术经济,2002(20)4:29-31
[20]朱圣东、吴迎.我国天然维生素E工业所面临的挑战[J].中国油脂,2001(26)2:14-16
[21]孙登文、先雪峰等.硅胶吸附法精制天然维生素E的工艺研究[J],中国油脂,2002(27)5:68-70
[22]雷炳福、孙登文.a-生育酚生产技术的研究进展[J],现代化工,1997(7):13-14
[23]Dutta-roy.Molecular mechanism of cellular uptake and intracellular translocation of a-tocopherol:role of tocopherol-binding proteins[J],food and chemical toxicology,1999(37):967-971
[24]尤新.天然维生素E的生理功能和开发前景分析[J].中国食品添加剂,2000(4):30-33
[25]Hickman,K.C.D.(to distillation products,ins),Improvements in and relating to the preparation of tocopherols[P].GB548,731,1942-10-20
[26]Hickman,K.C.D.(to distillation products,ins),purification of sludges,scums and the like to prepare relatively purified tocopherol[P].US2.349,270,1944-05-23
[27]Brokaw,G.Y.(to eastman kodak company),Improvements in or relating to the recovery of tocopherols from deodorizer sludges[P].GB774,855,1957-05-15
[28]Smith,F.E.(to eastman kodak company).Improvements in or relating to sterols and tocopherols[P].GB 1,008,767,1965-11-03
[29]Smith,F.E.(to eastman kodak company) Separation of tocopherols and sterols from deodorizer sludge and the like[P].US3,335,154,1967-08-08
[30]Rinbone,R.R,D.S.Huang(to aerojet genera corporation).Recovery of tocopherols from plant and animal oils[P].US5,317,245,1994-12-06
[31]Rohr,R,J.A.Trujillo-quijano(to resitee industria qimica LTDA),Process for Extraction and concentration of liposoluble vitamins and provitamins,Growth factors and animal and vegetable hormones from residues and byproducts of industrialized animal and vegetable products[P].US6,344,573B1,2002-02-05
[32]Hickman,K.C.D.and N.H.Kuhrt(to distillation products,ins),tocopherol preparation[P].US2.349,272,1944-05-23
[33]Brown,W.,K.H.meng(to eastman kokak company),process for recovery oftocopherols and sterols[P].GB1,011,923,1965-12-01
[34]Brown,W.,K.H.meng(to eastman kokak company),improvement for recovery of tocopherols and sterols[P].GB1,011,923,1965-12-01
[35]Fizet,C.(to Hoffmann-la Roche Inc.),Concentration of Natural Ingredients from Natural Materials[P].US4,939,276,1990-07-03
[36]Mattokow,M.,D.Perlman(to Benjamin Clayton),Treatment of Fatty materials[P].US2,704,764,1955-03-22
[37]樊明涛.豆油脱臭馏出物甲酯化处理的试验研究[J],西北农业学报,2002(11)4:42-45
[38]鲁志成.浓硫酸催化脱臭馏出物脂肪酸甲酯化工艺研究[J].粮食与油脂,2005,3,21-23
[39]Baxter,J.G(to Distillation Products,Inc.),Production of tocopherol or vitamin E[P]US2,349,271,1944-05-23
[40]Summer,C.E.,Jr.S.D.Barnicki,M.D.Dolfi(to Eastman Chemical Company),Process for the production of steroi and tocopherois concentraters[P].US5,424,457,1995-06-13
[41]Barnicki,S.D.,C.E.Summer(to Easterman Chemical Company),Process for the Production of tocotrienol/tocopherol blend concentrates[P].US5,660,691,1997-08-26
[42]Barnicki,S.D.,C.E.Summer(to Easterman Chemical Company),Process for the Production of tocopherol concentrates[P].US5,512,691,1997-04-30
[43]Hunt,T.K,Recovery of tocopherols[P]US5,703,252,1997-12-30
[44]Hunt,T.K,Recovery of tocopherols[P]US5,670,669,1997-09-23
[45]Hunt,T.K,Recovery of tocopherols[P]US5,616,735,1997-08-19
[46]刘青松,丁霄霖.强酸性树脂催化脂肪酸的甲酯化反应研究[J].食品工业科技 2004(25)3:73-75
[47]奚力民.棕榈油脱臭馏出物的阳离子交换树脂催化酯化反应研究[J].中国粮油学报2006(21)3:170-174
[48]杨亦文.高含量天然生育酚提取新工艺研究[D]:博士学位论文.浙江:浙江大学,2004
[49]#12
[50]Willgling,S.M.(to Henkel Corporation),Purification of tocopherols[P].US4,617,406,1986-10-14
[51]Fizet,C.(to Hoffmann-la Roche Inc.),Process for tocopherol and sterols from natural sources [P].US5,487,817,1996-01-30
[52]Mccurry P.M,Jr.S.W.Turner(to Cognis Corporation),Processes for the purification of tocopherol and/ or sterol compounds and compositions containing orthoborate ester mixture[P].US6,429,320B1,2002-08-06
[53]Mccurry P.M,Jr.S.W.Turner(to Cognis Corporation),Processes for the purification of tocopherol and/or sterol compounds and compositions containing orthoborate ester mixture[P].US2002/0072620A1,2002-01-13
[54]Sumner,C.E,Jr(to Archer-Daniels-Midland Company),Methods for Separating a tocopherol from a tocopherol-containing mixture and compositions thereof[P].WO00/43095,2000-07-27
[55]Baxzer,J.G.(to Distillation Products Inc.),Improvements in the preparation of tocopherol concentrates[P].GB546,865,1942-08-04
[56]Baxzer,J.G.(to Distillation Products Inc.),Purification or concentration of tocopherol[P].GB2,317,353,1943-04-27
[57]Hickman,K.C.D.(to distillation products,Ins),Improvements in and relating to the preparation of tocopherol[P].GB548,731,1942-10-22
[58]Hickman,K.C.D.(to distillation products,Ins),Recovery of tocopherol[P].US2,349,269,1944-05-23
[59]Hickman,K.C.D.(to distillation products,Ins),Antioxidant[P].US2,349,24,1944-05-23
[60]Baird,J.L.(to Artisan Industrise Inc.),Method for the purification of vitamin E[P].US5,582,692,1996-12-10
[61]Baird,J.L.(to Artisan Industrise Inc.),System for the purification of vitamin E[P].US5,658,433,1997-08-19
[62]#12
[63]王璋.食品酶学[M].北京:中国轻工业出版社,1992
[64]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[65]刘毅.脂肪酶催化酯合成[J].食品科学,2001(22)7:87-90
[66]周秋香,陈乐陪.脱臭馏出物中提取天然维生素E的工艺研究[J].粮食与食品工业,2003(2):25-27
[67]Alan Fersht.Enzyme Structure and Mechanism[M].W.H.Freeman and company 1985
[68]Philip L.Hall.The Quarterly Review of Biology[J]1979(54)1:73-74
[69]Wescott CR,Klibanov AM.The solvent dependence of enzyme specificity[J].Biochim biophys,1994(12)6:1-9
[70]高修功,俞耀庭.非水相酶学的原理与应用[J].国外医学生物医学工程分册.1994(17)5:268-273
[71]Klibanov AM.Improving enzymes by using them in organic solvents[J].Nature 2001.409:241-246
[72]许建和,胡英.生物转化中的有机介质系统[J].化学世界.1991(32)7:290-293
[73]Welton T.Solvents for synthesis and catalysis[J].Chem.Rev.1999(99):2071-2083
[74]姚鹏.菲水相中固定化脂肪酶催化酯合成反应的研究[D].博士学位论文,北京:北京化工大学,2000
[75]Lanne C,Boeren S.Rules for optimization of biocatalysis in organic solvents[J],biotechnol bioeng1987(30):81-87
[76]杨红、高修功、曹淑桂、章克昌.用傅立叶变换红外光谱研究有机溶剂对脂肪酶构象的影响[J].无锡轻工大学学报,1997(16)2:42-46
[77]Zaks A,Klibanov AM.Enzymatic catalysis in organic media at 100℃[J].science,1984,224:12-49
[78]Tawaki S,Klibanov AM.Chemoselectivity of enzymes in anhydrous media is strongly solvent-dependent[J].Biocatalysis,1993,8:3-19
[79]Rubio E,Fernandez-Mayorales A.Effect of the sovlent on enzyme regioselectivity[J].J am chem soc,1991,113:695-696
[80]Arnold FH.Protein design for non-aqueous solvents[J].protein engineering,1988,2:21-25
[81]Rupley M.Effect of small carbohydrates on the catalytic ativity of a protesase and two glycohydrolases[J].Carbohydrate polymers,2001,45:161-167
[82]Bonscherer UT.Methods to increase enantioselectivity of lipases and esterases[J].Curropin biotechnol,2002,13:543-547
[83]Hirose Y,Kariya K.Drastic solvent effect on lipase-catalyzed enantioselvectiv hydrolysis of prochiral[J].Tetrahedron lett,1992,33:7157-7160
[84]Mejri M,Mathlouthi M.Effect of small carbohydrates ont the catalytic acitvity of a protease and two glycohydrolases[J].Carbohydrate polymers,2001,45:161-167
[85]Faber K.Biotransformation in organic chemistry[M].Germany:springer,2000
[86]Carres G.properties and synthetic applications of enzymes in organic solvents[J].Angew chem int ed,2000,39:2226-2254
[87]Fitzpatrick PA,Klibanov AM.How can the solvent affect enzyme enantioselctivity?[J].J Am chem soc,1991(113):3166-3171
[88]Zaks A,Klibanov AM.Substrate specificity of enzymes in organic solvents vs.water is reversed[J].J Am chem soc,1986(108):2767-2768
[89]Alan Fersht.Enzyme Structure and Mechanism[M].W.H.Freeman and company 1985
[90]程玉华.酶在化学合成中的应用[J].生物工程进展.1992(12)4:11-18
[91]郭诤.非水相系统中脂肪酶催化酯化反应的研究[D].博士学位论文.天津:天津大学,2003
[92]Malcata F.X.,Hector R.Complete nucleotide sequence of the lipase gene from staphylococcus hyicus cloned instaphylococcus hyicus[J]Enzyme microb technol,1992(14):426-446
[93]Margolin Al.Enzymes in the synthesis of chiral drugs[J].Enzyme microb technol,1993(15):266-280
[94]Wescott CR,Klibanov AM.the solvent dependence of enzyme specificity[J].Biochim biophys Acta,1994,(120):1-9
[95]Ke Y,Wescotta CR.Predicition of the solvent dependence of enzymatic prochiral selectivity by means of structure-based thermodynamic claculations[J].J.Am.Chem.Soc,1996(118):3366-3374
[96]罗贵民.酶工程[M].北京:化学工业出版社,2002
[97]Dartois V,Baulard A.Nucleotid and expression of a lipase gene from bacillus subtillis 168[J].Biochem biophys acta,1992,132:253-260
[98]Jaeger K-E,Ransac S,Bacterial lipases[J].FEMS microb reviews,1994(15):29-63
[99]熊力.大豆油脱臭馏出物中维生素E的浓缩和提取[D].无锡:江南大学,1997年
[100]谷克仁.脱臭馏出物提取V_E的酶预处理[J].中国油脂,2006(31)2:41-43
[101]李志学.天然维生素E得酶法萃取工艺[J].江西食品工业,2000(3):36
[102]Suresh Ramamurthl et al.Enzymatic Pretreatment of Deodorizer Distillate for Concentration of Sterols and Tocopherols[J].JAOCS,1993(70) 3:287-295
[103]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77) 10:1009-1013
[104]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81) 10:339-345
[105]Nara Lucia Facioli.Optimisation of enzymatic esterification of soybean oil deodorizer distillate[J],Journal of the Science Food and Agriculture,2001(81):1193-1198
[106]施伟,章克昌.庚烷中微生物脂肪酶催化酯化反应动力学的研究[J].无锡轻工大学学报,1998(17)3:50-52
[107]吴华昌,宗敏华,邓静,王菊芳.无溶剂系统脂肪酶促POMF酯交换生产CBE的动力学研究[J].中国油脂,2003(28)8:50-53
[108]杨文伟、潘文群.正己烷中固定化脂肪酶催化酯化反应的动力学研究[J].常州师专学 报,2002(20)6:4-6
[109]ChulalaK.Kinetic study of esterification by immobilized lipase in hexane[J].FEBS Lett,1990(276):181-184
[110]狄济乐.从油脂加工副产物中提取天然维生素E[J].粮食与饲料工业,1998(3):38-39
[111]Brown,W.(to eastman Kodak company),Process for Separating Tocopherols and sterols from Deodorizer Sludge and the like[P]US 3,153,054,1964-10-13
[112]Brown,W.(to eastman Kodak company),Improvements in or relating to tocopherols and sterols[P]GB 1,030,792,1966-05-25
[113]Brown,W.F.E.Smith(to eastman Kodak company),Process for Separating Tocopherols and sterols from Deodorizer Sludge and the like[P]US 3,153,055,1964-10-13
[114]Brown,W.F.E.Smith(to eastman Kodak company),Improvements in or relating to tocopherols and sterols[P]GB 1,030,514,1966-05-25
[115]#12
[116]#12
[117]Takagi,Y.,Y.Kai(to the Nisshin Oil Mills,Ltd.),Process for preparation of tocopherol concentrates[P].US4,454,329,1984-06-12
[118]Willging,S.M.(to Henkel Corporation),Purification of tocopherols[P].US4,550,183,1985-10-29
[119]Summer,C.E.,Jr(to Sterne,Kessler,Goldstein & Fox P.L.L.C),Methods for separating a tocopherol from a tocopherol-containing mixture[P].US2002/OO42527A1,2002-04-11
[120]Embree,N.D.,and N.H.Kuhrt(to Distillation products,Ins.),Preparation of tocopherol concentrates[P].US2,454,692,1948-11-23
[121]Embree,N.D.,and N.H.Kuhrt(to Distillation products,Ins.),Improvements in the preparation of tocopherol concentrates[P].GB616,142,1949-01-17
[122]#12
[123]#12
[124]孙云鹏、孙明华、孙传经(申请人 孙传经),超临界CO_2从大豆脱臭物中萃取分离天然维生素 E的方法[P].CN1228427,1999-09-150
[125]赵亚平、王大璞(申请人 上海交通大学),超临界流体提取浓缩天然维生素E的新工艺[P].CN1253951,2000-05-24
[126]曹国锋、龚任、刘红天,脱臭馏出物中天然维生素E提取[J],粮食与油脂,2001,(5),42-30
[127]Hickman,K.C.D.,(to Distillation Products,Inc.),Preparation of Tocopherol Products[P].US 2,349,276,1944-05-23
[128]Baxter,J.G.,C.D.Robeson(to Distillation Products,Inc.),Preparation of Tocopherols[P].US 2,379,420,1945-07-03
[129]Baxter,J.G.,and C.D.Robeson(to Distillation Products,Inc.),Improvements in the Preparation of Tocopherols[P].GB 616,939,1949-01-28
[130]#12
[131]孙登文、曲德林、刘福祯、陆振民(申请人 清华大学),从植物油精炼副产物中提取维生素E 和甾醇的新工艺[P]。CN1074217,1993-07-14
[132]Kijima,S,K.Naito,T.Mori(to Eisai Co.,Ltd.),Purification Process of Tocopherol Containing Materials[P].US3,122,565,1964-02-25
[133]Kijima,S.,T.Nakamura(to Eisai Co.,Ltd),Method of Isolating and Refining Tocopherol Homologues[P].US3,402,182,1968-09-17
[134]#12
[135]#12
[136]曲德林、陈培榕、苏健民(申请人 清华大学),从精炼植物油油渣中分离维生素E的工艺[P].CN1034367,1989-08-020
[137]Green,J.S.Z.Marcinkiewicz(to Vitamins Limited),Improvements in or relating to the Concentration of Tocopherols[P].GB832,572,1960-04-13
[138]Sampathkumar(to UC Unitas Corporation),Process for Recovering Tocopherols from Deodorizer Sludge[P].US4,594,437,1986-06-10
[139]Woziwodzki,H.E.(to Lever Brothers Company),Separation of the Isomers of Tocopherol by Liquid/Solid Chromatography[P].US4,122,094,1978-10-24
[140]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues[P].US4,480,108,1984-10-30
[141]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues(Ⅰ)[P].US4,602,098,1986-07-22
[142]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues(Ⅱ)[P].US4,607,111,19 86-08-19
[143]#12
[144]#12
[145]孙伯鲁(申请人孙伯鲁),工业化天然维生素E提取新工艺[P].CN1099754,1995-03-080
[146]May,C.Y,M.A.Ngan,Y.Basiron(to Pennie & Edmonds LLP),Method for the Chromatographic Isolation of Vitamin E Isomers[P].US2001/0044548A1,2001-11-22
[147]Bellafiore,L.,K.Henreta(to Technikrom,Inc.),Method for Producing Purified Tocotrienols and Tocopherols Using Liquid Chromatography[P].US6,395,915B1,2002-05-8
[148]彭莺、刘福祯.天然植物甾醇的应用与提取工艺[J].化工进展,2002(21)1:49-53
[149]赵国志.植物甾醇及其产品开发利用[J].粮食与油脂,2006,2:3-6
[150]吴时敏.功能性油脂[M].北京:中国轻工业出版社,2001
[151]裘爱泳,吴时敏.脱臭馏出物中植物甾醇的回收[J].中国油脂,1997,22(3):49-50
[152]Yoshinori Hirota.Purification of Steryl Esters from Soybean Oil Deodorizer Distillate[J].JAOCS,2003(80)4:341-346
[153]曹莹,谷克仁.植物甾醇提取方法研究进展[J].粮油食品科技,2006,14(5):25-28
[154]万建春,张维农.天然植物甾醇的分离纯化[J].武汉工业学院学报.2006(14)4:12-17
[1]雷炳福.油脂脱臭馏出物的组成与市场前景[J],中国油脂,2002(27)1:75-78
[2]梁诚.天然维生素E生产现状与应用前景[J],化工技术经济,2002(20)4:29-31
[3]毕艳兰.油脂化学[M].北京:化学工业出版社,2005
[4]Y.H.Hui主编,徐生庚,裘爱泳主译.贝雷:油脂化学与工艺学[M].北京:中国轻工业出版社,2001
[5]施学东、陈黎.植物油精炼副产物的综合利用及深加工[J].福建化工,2001(2),3-9
[6]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[7]何东平.油脂工厂设计手册[M].湖北:湖北科学技术出版社,1990
[8]杨波涛.植物甾醇的提取与精制[D].硕士学位论文,无锡:无锡轻工大学,2000
[9]P.F.Martins,V.M.Ito,C.B.Batistella and M.R.W.Maciel.Free fatty acid separation from vegetable oil deodorizer distillate using molecular distillation process[J].Separation and Purification Technology.2006(48) 1:78-84.
[10]袁勤生.现代酶学[M].上海:华东理工大学出版社:2001
[11](美)茨拉脱坎斯(A.Zlmkis),(联邦德国)卡爱塞(R.E.Kaiser)著;林珍安译.高效薄层色谱[M].上海:上海科学技术出版社,2002
[12]北京市粮食科学研究所.GB/T 5528-1995植物油脂水分及挥发物含量测定法[S].北京:中国标准出版社,1995
[13]商业部粮食储运局.GB/T 5529-85植物油脂检验 杂质测定法[S].北京:中国标准出版社,1985
[14]国内贸易部谷物油脂化学研究所.GB/T 5530-1998动植物油脂 酸价和酸度测定[S].北京:中国标准出版社,1998
[15]方涛.超临界二氧化碳萃馏浓缩天然生育酚的研究[D].博士学位论文,无锡:江南大学,2001
[16]李桂华.油料油脂检验与分析[M].北京:化学工业出版社,2006
[17]:浙江医药股份有限公司新昌制药厂、浙江海正药业股份有限公司.GB 19191—2003食品添加剂天然维生素E[S].北京:中国标准出版社,2003
[18]高瑜莹,裘爱泳.植物甾醇的分析方法[J],中国油脂,2001(26)1:25-28
[19]Nara Lucia Facioli.Optimisation of enzymatic esterification of soybean oil deodorizer distillate[J],Journal of the Science Food and Agriculture,2001(81):1193-1198
[20]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81) 10:339-345
[21]肖旭霖.食品加工机械与设备[M].北京:中国轻工业出版社,2000
[22]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77)10:1009-1013
[23]贺尊诗 李青山 聂铁铮.无机色谱分析法[M].北京:中国环境科学出版社,1990
[1]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[2]王璋.食品酶学[M].北京:中国轻工业出版社,1992
[3]颜思旭,蔡红玉.酶催化动力学原理与方法[M],厦门:厦门大学出版社,1987
[4]Cleland,W.W.The Kinetics of Enzyme-Catalyzed Reactions with Two or More Substrates or Products[J].Biochimica ET Biophsica Acta,1963(67):104-137
[5]陈石根.酶学[M].上海:复旦大学出版社,2001
[6]赵赣、杨礼锐.关于酶促反应速度与酶促反应的初速度的教学[J].植物生理学通讯,2001(37)1:50-51
[7]吴华昌,宗敏华.无溶剂系统脂肪酶促POMF酯交换生产CBE的动力学研究[J].中国油脂,2003(28)8:50-53
[8]国内贸易部谷物油脂化学研究所.GB/T 5530-1998动植物油脂 酸价和酸度测定[S].北京:中国标准出版社,1998
[9]Lortie R.Kinetic Study of the Lipase-catalyzed Synthesis ofTriolein[J].Biotechnol Bioeng,1993,41:1021-1026
[10]King,EL.;Altman,C.A Schematic Method of Deriving the Rate Laws for Enzyme-Catalyzed Reactions[J].Journal of Physical Chemistry,1956(1) 1375-1388
[11]吴有炜.试验设计与数据处理[M].苏州大学出版社,2002
[1]陈石根.酶学[M].上海:复旦大学出版社,2001
[2]陈陶声,居乃玻,陈石根.固定化酶理论与应用[M].北京:轻工出版社:1987
[3]李彦峰、李军荣、伏莲娣.固定化酶的制备及应用[J].高分子通报,2001:13-23
[4]罗贵民,曹淑桂、张今.酶工程[M].北京:化学工业出版社,2002
[5]Manuel Ferrer,M Angeles Cruces,Francisco J Plou,et al.A simple procedure for the regioselective synthesis of fatty acid esters of maltose leucrose,maltot riose and n2dodecyl maltosides[J].Tetrahedron,2000,56:4053-4061
[6]杨守志.生物化学反应工程第三讲:生化反应器的性能[J].化工进展,1991,(2):44-47
[7]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81)10:339-345
[8]徐兆瑜.略析分子筛的发展和应用[J].化工技术与开发,2007(36)7:31-36
[9]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[10]姚鹏.非水相中固定化脂肪酶催化酯合成反应的研究[D].博士学位论文,北京:北京化工大学,2000
[11]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77)10:1009-1013
[12]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[1]毕艳兰.油脂化学[M].北京:化学工业出版社,2005
[2]邢其毅、徐瑞秋、周政、裴伟伟.基础有机化学[M].北京:高等教育出版社,2002
[3]刘汝宽.制备生物柴油的催化剂研究进展[J].中国粮油学报,2006(21)3:273-276
[4]DAVID BGA.The theoretical and experimental study of the centrifugal molecular still[J].Aiche J,1972,18(2):269-276
[5]杨村、于宏奇.分子蒸馏技术[M].北京:化学工业出版社,2003
[6]乔国平,王兴国.分子蒸馏技术及其在油脂工业中的应用[J].粮食与油脂,2002,(5):25-27
[7]王军武,许松林,徐世民.分子蒸馏技术的应用现状[J].化工进展,2002,21(7):499-501
[8]Nguyen Anh Dung,Le Goffic Francois.Limits of wiped film short-path distilled[J].Chemical Engineering Scisence,1997,52(16):2661-2666
[9]Cvengros J,Pollak S,MicovM.Film wiping in the molecular evaporator[J].Chemical Engineering Journal,2001,81(1):9-14
[10]鲁志成,谷克仁,冶保献.浓硫酸催化脱臭馏出物脂肪酸甲酯化工艺研究[J].中国油脂,2005,30(3):21-24
[11]杨百勤.物理化学实验[M].北京:化学工业工业出版社,2001
[12]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[13]Schafer A.Vegetable Oil fatty acid methyl esters alternative dieselfuelsfor commercial vehicles engines[A].Plant O.Fuel Proc.Syrup[C].1997:29-46
[14]全国食品添加剂标准化技术委员会.GB19191-2003食品添加剂-天然维生素E[S].北京:中国标准出版社,2003.
[15]吴有炜.试验设计与数据处理[M].苏州:苏州大学出版社,2002
[1]国家药典委员会.中华人民共和国药典2000年版2部[M].北京:化学工业出版社,2000
[2]赵国志.植物甾醇及其产品开发利用[J].粮食与油脂,2006,2:3-6
[3]梁艳,张英.植物甾醇的提取分离和分析检测方法研究进展[J].中国粮油学报,2006,(21)3:1-7
[4]管伟举,谷克仁.植物甾醇研究紧张[J].粮食与油脂,2006,3:5-9
[5]吴素萍,章中.植物甾醇的研究现状[J].中国食物与营养,2007,9:20-21
[6]高瑜莹,裘爱泳.植物甾醇的分析方法[J].中国油脂,2001(26)1:25-29
[7]杨波涛.植物甾醇的提取与精制[D].无锡:江南大学硕士学位论文,2001
[8]许文林,王雅琼,黄一波等.重结晶法精制植物甾醇的溶剂选择[J].扬州大学学报(自然科学版),2002,(2):58-62
[9]韦继慷.植物甾醇提取工艺研究[D]硕士学位论文.浙江:浙江大学,2002
[10]Q/321283GEB07-2006,植物甾醇[S].江苏春之谷生物制品有限公司,2006
[1]Daeseok Han.Solubilization of Vitamin C in Fish Oil and Synergistic Effect with Vitamin E in Retarding
[2]高蓝、李浩明.几种抗氧化剂对鲲鱼油的抗氧化作用的研究[J].中国食品添加剂,1999,2:22-25
[3]Namiki M.Antiox idants/antimutagens in food,in CRC Crit[M].Rev Food Sci Nutr,CRC Press BocaRaton.1990,256
[4]吴克刚.大蒜提取物对鱼油抗氧化作用的研究及其机理的探讨[J].中国调味品2000,11:11-14
[5]Bran A L.Toxicology and biochemistry of BHA and BHT[J].JAOCS,1975,52(2):372-375
[6]潘蓄林.维生素E类化合物抗氧化活性的理论分析[J].化学研究与应用,2004(16)1:27-29
[7]凌关庭.食品抗氧化剂及其进展(Ⅱ)[J].粮食与油脂,2000(7):47-48
[8]赵贵兴.维生素E抗油脂氧化的功能[J].黑龙江农业科学,2003(1):45-48
[9]韩国麒.用于食用油脂的抗氧化剂[J].郑州粮食学院学报,1981,2:24-43
[10]宋国安.天然维生素的应用及开发前景[J].武汉工业学院学报,2000,20(4):29-32
[11]梁诚.天然VE生产现状与应用前景[J].化工技术经济,2002,20(4):29-32
[12]赵贵兴,陈霞维.维生素E抗油脂氧化效果的研究[J].中国油料作物学报,2002,24(3):58-59
[13]David DK.An evaluation of the mutiple effects of the antioxidant vitamins[J].Trend in food science technology,1997,8(6):198-203
[14]GB/T5538-1995,油脂过氧化值测定[S].北京:中国标准出版社,1995
[15]ENISO 6885:1998,Animal and vegetable fats and oils-Demination ofanisidine value[S].CEN,2000
[16]王璋,许时婴,汤坚.食品化学[M].北京:中国轻工业出版社,2002,110
[17]李彦萍、高荫榆.微量金属元素对乌桕类可可脂氧化稳定性研究[J].食品科学,2002(23)1:23-26
[18]W.G.Mentens,C.E.Swindells and B.F.Teasdale[J].JAOCS,1971,48:544-546
[19]M.H.Gordon,X.C.Weng.Antioxidant properties of Extracts from Tanshen[J].Food Chem,1992,44:119-122
[2]梁诚.天然维生素E生产现状与应用前景[J].化工技术经济,2002(8)4:29-31
[3]王瑞元.中国油脂工业的现状与发展趋势[J].中国油脂,2006(31)11:7-11
[4]刘玉兰.植物油脂生产与综合利用[M].北京:中国轻工业出版社,1999
[5]雷炳福.油脂脱臭馏出物的组成与市场前景[J].中国油脂,2002,27(1):75-78
[6]吴时敏.功能性油脂[M].北京:中国轻工业出版社,2001
[7]樊明涛、吴守一、马海乐.从油脂脱臭馏出物中提取生育酚的研究概况[J].西北农林科技大学学报(自然科学版),2002,30(增刊):73-77,
[8]Kirk-Othmer.Encyclopedia of Chemical Technology,Third Edition,Vol 24[M].New Yord:John Wiely,1984
[9]IUPAC-IUB Joint Commission on Biochemical Nomenclature.Nomenclature of Tocopherols and Related Compounds:Recommendations 1981[J].Eur.J.Biochem,1982(123):473-475
[10]国家药典委员会.中华人民共和国药典2000年版2部[M].北京:化学工业出版社,2000.
[11]全国食品添加剂标准化技术委员会.GB19191-2003食品添加剂-天然维生素E[S].北京:中国标准出版社,2003.
[12]尤新.天然维生素E的生理功能和开发前景分析[J].中国食品添加剂,2000,4:30-33
[13]Fernholz,E.On the constitution of a-Tocopherol[J],J.Am.Chen.Soc,1938(60),700-705.
[14]Nelan,D.R,C.D.Robseson,The oxidation product from a-tcopherol and potassium ferricyanide and its reaction with ascorbic and hydrochloric acids[J],
[15]FDA.the united states pharmacopeia ⅩⅩⅣ[M].USA:2000
[16]Institute of Medicine of the National Academy of Sciences.Food chemicals codex,4th ed.,[M]USA.1996
[17]中华人民共和国卫生部药典委员会.中华人民共和国药典 二部[M].北京:化学工业出版社,1980
[18]邵斌.天然d-a-维生素[J].中国食品添加剂,2000(20)4:78-83
[19]梁诚.天然维生素E生产现状与应用前景[J].化工技术经济,2002(20)4:29-31
[20]朱圣东、吴迎.我国天然维生素E工业所面临的挑战[J].中国油脂,2001(26)2:14-16
[21]孙登文、先雪峰等.硅胶吸附法精制天然维生素E的工艺研究[J],中国油脂,2002(27)5:68-70
[22]雷炳福、孙登文.a-生育酚生产技术的研究进展[J],现代化工,1997(7):13-14
[23]Dutta-roy.Molecular mechanism of cellular uptake and intracellular translocation of a-tocopherol:role of tocopherol-binding proteins[J],food and chemical toxicology,1999(37):967-971
[24]尤新.天然维生素E的生理功能和开发前景分析[J].中国食品添加剂,2000(4):30-33
[25]Hickman,K.C.D.(to distillation products,ins),Improvements in and relating to the preparation of tocopherols[P].GB548,731,1942-10-20
[26]Hickman,K.C.D.(to distillation products,ins),purification of sludges,scums and the like to prepare relatively purified tocopherol[P].US2.349,270,1944-05-23
[27]Brokaw,G.Y.(to eastman kodak company),Improvements in or relating to the recovery of tocopherols from deodorizer sludges[P].GB774,855,1957-05-15
[28]Smith,F.E.(to eastman kodak company).Improvements in or relating to sterols and tocopherols[P].GB 1,008,767,1965-11-03
[29]Smith,F.E.(to eastman kodak company) Separation of tocopherols and sterols from deodorizer sludge and the like[P].US3,335,154,1967-08-08
[30]Rinbone,R.R,D.S.Huang(to aerojet genera corporation).Recovery of tocopherols from plant and animal oils[P].US5,317,245,1994-12-06
[31]Rohr,R,J.A.Trujillo-quijano(to resitee industria qimica LTDA),Process for Extraction and concentration of liposoluble vitamins and provitamins,Growth factors and animal and vegetable hormones from residues and byproducts of industrialized animal and vegetable products[P].US6,344,573B1,2002-02-05
[32]Hickman,K.C.D.and N.H.Kuhrt(to distillation products,ins),tocopherol preparation[P].US2.349,272,1944-05-23
[33]Brown,W.,K.H.meng(to eastman kokak company),process for recovery oftocopherols and sterols[P].GB1,011,923,1965-12-01
[34]Brown,W.,K.H.meng(to eastman kokak company),improvement for recovery of tocopherols and sterols[P].GB1,011,923,1965-12-01
[35]Fizet,C.(to Hoffmann-la Roche Inc.),Concentration of Natural Ingredients from Natural Materials[P].US4,939,276,1990-07-03
[36]Mattokow,M.,D.Perlman(to Benjamin Clayton),Treatment of Fatty materials[P].US2,704,764,1955-03-22
[37]樊明涛.豆油脱臭馏出物甲酯化处理的试验研究[J],西北农业学报,2002(11)4:42-45
[38]鲁志成.浓硫酸催化脱臭馏出物脂肪酸甲酯化工艺研究[J].粮食与油脂,2005,3,21-23
[39]Baxter,J.G(to Distillation Products,Inc.),Production of tocopherol or vitamin E[P]US2,349,271,1944-05-23
[40]Summer,C.E.,Jr.S.D.Barnicki,M.D.Dolfi(to Eastman Chemical Company),Process for the production of steroi and tocopherois concentraters[P].US5,424,457,1995-06-13
[41]Barnicki,S.D.,C.E.Summer(to Easterman Chemical Company),Process for the Production of tocotrienol/tocopherol blend concentrates[P].US5,660,691,1997-08-26
[42]Barnicki,S.D.,C.E.Summer(to Easterman Chemical Company),Process for the Production of tocopherol concentrates[P].US5,512,691,1997-04-30
[43]Hunt,T.K,Recovery of tocopherols[P]US5,703,252,1997-12-30
[44]Hunt,T.K,Recovery of tocopherols[P]US5,670,669,1997-09-23
[45]Hunt,T.K,Recovery of tocopherols[P]US5,616,735,1997-08-19
[46]刘青松,丁霄霖.强酸性树脂催化脂肪酸的甲酯化反应研究[J].食品工业科技 2004(25)3:73-75
[47]奚力民.棕榈油脱臭馏出物的阳离子交换树脂催化酯化反应研究[J].中国粮油学报2006(21)3:170-174
[48]杨亦文.高含量天然生育酚提取新工艺研究[D]:博士学位论文.浙江:浙江大学,2004
[49]#12
[50]Willgling,S.M.(to Henkel Corporation),Purification of tocopherols[P].US4,617,406,1986-10-14
[51]Fizet,C.(to Hoffmann-la Roche Inc.),Process for tocopherol and sterols from natural sources [P].US5,487,817,1996-01-30
[52]Mccurry P.M,Jr.S.W.Turner(to Cognis Corporation),Processes for the purification of tocopherol and/ or sterol compounds and compositions containing orthoborate ester mixture[P].US6,429,320B1,2002-08-06
[53]Mccurry P.M,Jr.S.W.Turner(to Cognis Corporation),Processes for the purification of tocopherol and/or sterol compounds and compositions containing orthoborate ester mixture[P].US2002/0072620A1,2002-01-13
[54]Sumner,C.E,Jr(to Archer-Daniels-Midland Company),Methods for Separating a tocopherol from a tocopherol-containing mixture and compositions thereof[P].WO00/43095,2000-07-27
[55]Baxzer,J.G.(to Distillation Products Inc.),Improvements in the preparation of tocopherol concentrates[P].GB546,865,1942-08-04
[56]Baxzer,J.G.(to Distillation Products Inc.),Purification or concentration of tocopherol[P].GB2,317,353,1943-04-27
[57]Hickman,K.C.D.(to distillation products,Ins),Improvements in and relating to the preparation of tocopherol[P].GB548,731,1942-10-22
[58]Hickman,K.C.D.(to distillation products,Ins),Recovery of tocopherol[P].US2,349,269,1944-05-23
[59]Hickman,K.C.D.(to distillation products,Ins),Antioxidant[P].US2,349,24,1944-05-23
[60]Baird,J.L.(to Artisan Industrise Inc.),Method for the purification of vitamin E[P].US5,582,692,1996-12-10
[61]Baird,J.L.(to Artisan Industrise Inc.),System for the purification of vitamin E[P].US5,658,433,1997-08-19
[62]#12
[63]王璋.食品酶学[M].北京:中国轻工业出版社,1992
[64]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[65]刘毅.脂肪酶催化酯合成[J].食品科学,2001(22)7:87-90
[66]周秋香,陈乐陪.脱臭馏出物中提取天然维生素E的工艺研究[J].粮食与食品工业,2003(2):25-27
[67]Alan Fersht.Enzyme Structure and Mechanism[M].W.H.Freeman and company 1985
[68]Philip L.Hall.The Quarterly Review of Biology[J]1979(54)1:73-74
[69]Wescott CR,Klibanov AM.The solvent dependence of enzyme specificity[J].Biochim biophys,1994(12)6:1-9
[70]高修功,俞耀庭.非水相酶学的原理与应用[J].国外医学生物医学工程分册.1994(17)5:268-273
[71]Klibanov AM.Improving enzymes by using them in organic solvents[J].Nature 2001.409:241-246
[72]许建和,胡英.生物转化中的有机介质系统[J].化学世界.1991(32)7:290-293
[73]Welton T.Solvents for synthesis and catalysis[J].Chem.Rev.1999(99):2071-2083
[74]姚鹏.菲水相中固定化脂肪酶催化酯合成反应的研究[D].博士学位论文,北京:北京化工大学,2000
[75]Lanne C,Boeren S.Rules for optimization of biocatalysis in organic solvents[J],biotechnol bioeng1987(30):81-87
[76]杨红、高修功、曹淑桂、章克昌.用傅立叶变换红外光谱研究有机溶剂对脂肪酶构象的影响[J].无锡轻工大学学报,1997(16)2:42-46
[77]Zaks A,Klibanov AM.Enzymatic catalysis in organic media at 100℃[J].science,1984,224:12-49
[78]Tawaki S,Klibanov AM.Chemoselectivity of enzymes in anhydrous media is strongly solvent-dependent[J].Biocatalysis,1993,8:3-19
[79]Rubio E,Fernandez-Mayorales A.Effect of the sovlent on enzyme regioselectivity[J].J am chem soc,1991,113:695-696
[80]Arnold FH.Protein design for non-aqueous solvents[J].protein engineering,1988,2:21-25
[81]Rupley M.Effect of small carbohydrates on the catalytic ativity of a protesase and two glycohydrolases[J].Carbohydrate polymers,2001,45:161-167
[82]Bonscherer UT.Methods to increase enantioselectivity of lipases and esterases[J].Curropin biotechnol,2002,13:543-547
[83]Hirose Y,Kariya K.Drastic solvent effect on lipase-catalyzed enantioselvectiv hydrolysis of prochiral[J].Tetrahedron lett,1992,33:7157-7160
[84]Mejri M,Mathlouthi M.Effect of small carbohydrates ont the catalytic acitvity of a protease and two glycohydrolases[J].Carbohydrate polymers,2001,45:161-167
[85]Faber K.Biotransformation in organic chemistry[M].Germany:springer,2000
[86]Carres G.properties and synthetic applications of enzymes in organic solvents[J].Angew chem int ed,2000,39:2226-2254
[87]Fitzpatrick PA,Klibanov AM.How can the solvent affect enzyme enantioselctivity?[J].J Am chem soc,1991(113):3166-3171
[88]Zaks A,Klibanov AM.Substrate specificity of enzymes in organic solvents vs.water is reversed[J].J Am chem soc,1986(108):2767-2768
[89]Alan Fersht.Enzyme Structure and Mechanism[M].W.H.Freeman and company 1985
[90]程玉华.酶在化学合成中的应用[J].生物工程进展.1992(12)4:11-18
[91]郭诤.非水相系统中脂肪酶催化酯化反应的研究[D].博士学位论文.天津:天津大学,2003
[92]Malcata F.X.,Hector R.Complete nucleotide sequence of the lipase gene from staphylococcus hyicus cloned instaphylococcus hyicus[J]Enzyme microb technol,1992(14):426-446
[93]Margolin Al.Enzymes in the synthesis of chiral drugs[J].Enzyme microb technol,1993(15):266-280
[94]Wescott CR,Klibanov AM.the solvent dependence of enzyme specificity[J].Biochim biophys Acta,1994,(120):1-9
[95]Ke Y,Wescotta CR.Predicition of the solvent dependence of enzymatic prochiral selectivity by means of structure-based thermodynamic claculations[J].J.Am.Chem.Soc,1996(118):3366-3374
[96]罗贵民.酶工程[M].北京:化学工业出版社,2002
[97]Dartois V,Baulard A.Nucleotid and expression of a lipase gene from bacillus subtillis 168[J].Biochem biophys acta,1992,132:253-260
[98]Jaeger K-E,Ransac S,Bacterial lipases[J].FEMS microb reviews,1994(15):29-63
[99]熊力.大豆油脱臭馏出物中维生素E的浓缩和提取[D].无锡:江南大学,1997年
[100]谷克仁.脱臭馏出物提取V_E的酶预处理[J].中国油脂,2006(31)2:41-43
[101]李志学.天然维生素E得酶法萃取工艺[J].江西食品工业,2000(3):36
[102]Suresh Ramamurthl et al.Enzymatic Pretreatment of Deodorizer Distillate for Concentration of Sterols and Tocopherols[J].JAOCS,1993(70) 3:287-295
[103]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77) 10:1009-1013
[104]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81) 10:339-345
[105]Nara Lucia Facioli.Optimisation of enzymatic esterification of soybean oil deodorizer distillate[J],Journal of the Science Food and Agriculture,2001(81):1193-1198
[106]施伟,章克昌.庚烷中微生物脂肪酶催化酯化反应动力学的研究[J].无锡轻工大学学报,1998(17)3:50-52
[107]吴华昌,宗敏华,邓静,王菊芳.无溶剂系统脂肪酶促POMF酯交换生产CBE的动力学研究[J].中国油脂,2003(28)8:50-53
[108]杨文伟、潘文群.正己烷中固定化脂肪酶催化酯化反应的动力学研究[J].常州师专学 报,2002(20)6:4-6
[109]ChulalaK.Kinetic study of esterification by immobilized lipase in hexane[J].FEBS Lett,1990(276):181-184
[110]狄济乐.从油脂加工副产物中提取天然维生素E[J].粮食与饲料工业,1998(3):38-39
[111]Brown,W.(to eastman Kodak company),Process for Separating Tocopherols and sterols from Deodorizer Sludge and the like[P]US 3,153,054,1964-10-13
[112]Brown,W.(to eastman Kodak company),Improvements in or relating to tocopherols and sterols[P]GB 1,030,792,1966-05-25
[113]Brown,W.F.E.Smith(to eastman Kodak company),Process for Separating Tocopherols and sterols from Deodorizer Sludge and the like[P]US 3,153,055,1964-10-13
[114]Brown,W.F.E.Smith(to eastman Kodak company),Improvements in or relating to tocopherols and sterols[P]GB 1,030,514,1966-05-25
[115]#12
[116]#12
[117]Takagi,Y.,Y.Kai(to the Nisshin Oil Mills,Ltd.),Process for preparation of tocopherol concentrates[P].US4,454,329,1984-06-12
[118]Willging,S.M.(to Henkel Corporation),Purification of tocopherols[P].US4,550,183,1985-10-29
[119]Summer,C.E.,Jr(to Sterne,Kessler,Goldstein & Fox P.L.L.C),Methods for separating a tocopherol from a tocopherol-containing mixture[P].US2002/OO42527A1,2002-04-11
[120]Embree,N.D.,and N.H.Kuhrt(to Distillation products,Ins.),Preparation of tocopherol concentrates[P].US2,454,692,1948-11-23
[121]Embree,N.D.,and N.H.Kuhrt(to Distillation products,Ins.),Improvements in the preparation of tocopherol concentrates[P].GB616,142,1949-01-17
[122]#12
[123]#12
[124]孙云鹏、孙明华、孙传经(申请人 孙传经),超临界CO_2从大豆脱臭物中萃取分离天然维生素 E的方法[P].CN1228427,1999-09-150
[125]赵亚平、王大璞(申请人 上海交通大学),超临界流体提取浓缩天然维生素E的新工艺[P].CN1253951,2000-05-24
[126]曹国锋、龚任、刘红天,脱臭馏出物中天然维生素E提取[J],粮食与油脂,2001,(5),42-30
[127]Hickman,K.C.D.,(to Distillation Products,Inc.),Preparation of Tocopherol Products[P].US 2,349,276,1944-05-23
[128]Baxter,J.G.,C.D.Robeson(to Distillation Products,Inc.),Preparation of Tocopherols[P].US 2,379,420,1945-07-03
[129]Baxter,J.G.,and C.D.Robeson(to Distillation Products,Inc.),Improvements in the Preparation of Tocopherols[P].GB 616,939,1949-01-28
[130]#12
[131]孙登文、曲德林、刘福祯、陆振民(申请人 清华大学),从植物油精炼副产物中提取维生素E 和甾醇的新工艺[P]。CN1074217,1993-07-14
[132]Kijima,S,K.Naito,T.Mori(to Eisai Co.,Ltd.),Purification Process of Tocopherol Containing Materials[P].US3,122,565,1964-02-25
[133]Kijima,S.,T.Nakamura(to Eisai Co.,Ltd),Method of Isolating and Refining Tocopherol Homologues[P].US3,402,182,1968-09-17
[134]#12
[135]#12
[136]曲德林、陈培榕、苏健民(申请人 清华大学),从精炼植物油油渣中分离维生素E的工艺[P].CN1034367,1989-08-020
[137]Green,J.S.Z.Marcinkiewicz(to Vitamins Limited),Improvements in or relating to the Concentration of Tocopherols[P].GB832,572,1960-04-13
[138]Sampathkumar(to UC Unitas Corporation),Process for Recovering Tocopherols from Deodorizer Sludge[P].US4,594,437,1986-06-10
[139]Woziwodzki,H.E.(to Lever Brothers Company),Separation of the Isomers of Tocopherol by Liquid/Solid Chromatography[P].US4,122,094,1978-10-24
[140]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues[P].US4,480,108,1984-10-30
[141]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues(Ⅰ)[P].US4,602,098,1986-07-22
[142]Foster,C.H.(to Eastman Kodak Company),Process for Separation of Tocopherol Homologues(Ⅱ)[P].US4,607,111,19 86-08-19
[143]#12
[144]#12
[145]孙伯鲁(申请人孙伯鲁),工业化天然维生素E提取新工艺[P].CN1099754,1995-03-080
[146]May,C.Y,M.A.Ngan,Y.Basiron(to Pennie & Edmonds LLP),Method for the Chromatographic Isolation of Vitamin E Isomers[P].US2001/0044548A1,2001-11-22
[147]Bellafiore,L.,K.Henreta(to Technikrom,Inc.),Method for Producing Purified Tocotrienols and Tocopherols Using Liquid Chromatography[P].US6,395,915B1,2002-05-8
[148]彭莺、刘福祯.天然植物甾醇的应用与提取工艺[J].化工进展,2002(21)1:49-53
[149]赵国志.植物甾醇及其产品开发利用[J].粮食与油脂,2006,2:3-6
[150]吴时敏.功能性油脂[M].北京:中国轻工业出版社,2001
[151]裘爱泳,吴时敏.脱臭馏出物中植物甾醇的回收[J].中国油脂,1997,22(3):49-50
[152]Yoshinori Hirota.Purification of Steryl Esters from Soybean Oil Deodorizer Distillate[J].JAOCS,2003(80)4:341-346
[153]曹莹,谷克仁.植物甾醇提取方法研究进展[J].粮油食品科技,2006,14(5):25-28
[154]万建春,张维农.天然植物甾醇的分离纯化[J].武汉工业学院学报.2006(14)4:12-17
[1]雷炳福.油脂脱臭馏出物的组成与市场前景[J],中国油脂,2002(27)1:75-78
[2]梁诚.天然维生素E生产现状与应用前景[J],化工技术经济,2002(20)4:29-31
[3]毕艳兰.油脂化学[M].北京:化学工业出版社,2005
[4]Y.H.Hui主编,徐生庚,裘爱泳主译.贝雷:油脂化学与工艺学[M].北京:中国轻工业出版社,2001
[5]施学东、陈黎.植物油精炼副产物的综合利用及深加工[J].福建化工,2001(2),3-9
[6]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[7]何东平.油脂工厂设计手册[M].湖北:湖北科学技术出版社,1990
[8]杨波涛.植物甾醇的提取与精制[D].硕士学位论文,无锡:无锡轻工大学,2000
[9]P.F.Martins,V.M.Ito,C.B.Batistella and M.R.W.Maciel.Free fatty acid separation from vegetable oil deodorizer distillate using molecular distillation process[J].Separation and Purification Technology.2006(48) 1:78-84.
[10]袁勤生.现代酶学[M].上海:华东理工大学出版社:2001
[11](美)茨拉脱坎斯(A.Zlmkis),(联邦德国)卡爱塞(R.E.Kaiser)著;林珍安译.高效薄层色谱[M].上海:上海科学技术出版社,2002
[12]北京市粮食科学研究所.GB/T 5528-1995植物油脂水分及挥发物含量测定法[S].北京:中国标准出版社,1995
[13]商业部粮食储运局.GB/T 5529-85植物油脂检验 杂质测定法[S].北京:中国标准出版社,1985
[14]国内贸易部谷物油脂化学研究所.GB/T 5530-1998动植物油脂 酸价和酸度测定[S].北京:中国标准出版社,1998
[15]方涛.超临界二氧化碳萃馏浓缩天然生育酚的研究[D].博士学位论文,无锡:江南大学,2001
[16]李桂华.油料油脂检验与分析[M].北京:化学工业出版社,2006
[17]:浙江医药股份有限公司新昌制药厂、浙江海正药业股份有限公司.GB 19191—2003食品添加剂天然维生素E[S].北京:中国标准出版社,2003
[18]高瑜莹,裘爱泳.植物甾醇的分析方法[J],中国油脂,2001(26)1:25-28
[19]Nara Lucia Facioli.Optimisation of enzymatic esterification of soybean oil deodorizer distillate[J],Journal of the Science Food and Agriculture,2001(81):1193-1198
[20]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81) 10:339-345
[21]肖旭霖.食品加工机械与设备[M].北京:中国轻工业出版社,2000
[22]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77)10:1009-1013
[23]贺尊诗 李青山 聂铁铮.无机色谱分析法[M].北京:中国环境科学出版社,1990
[1]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[2]王璋.食品酶学[M].北京:中国轻工业出版社,1992
[3]颜思旭,蔡红玉.酶催化动力学原理与方法[M],厦门:厦门大学出版社,1987
[4]Cleland,W.W.The Kinetics of Enzyme-Catalyzed Reactions with Two or More Substrates or Products[J].Biochimica ET Biophsica Acta,1963(67):104-137
[5]陈石根.酶学[M].上海:复旦大学出版社,2001
[6]赵赣、杨礼锐.关于酶促反应速度与酶促反应的初速度的教学[J].植物生理学通讯,2001(37)1:50-51
[7]吴华昌,宗敏华.无溶剂系统脂肪酶促POMF酯交换生产CBE的动力学研究[J].中国油脂,2003(28)8:50-53
[8]国内贸易部谷物油脂化学研究所.GB/T 5530-1998动植物油脂 酸价和酸度测定[S].北京:中国标准出版社,1998
[9]Lortie R.Kinetic Study of the Lipase-catalyzed Synthesis ofTriolein[J].Biotechnol Bioeng,1993,41:1021-1026
[10]King,EL.;Altman,C.A Schematic Method of Deriving the Rate Laws for Enzyme-Catalyzed Reactions[J].Journal of Physical Chemistry,1956(1) 1375-1388
[11]吴有炜.试验设计与数据处理[M].苏州大学出版社,2002
[1]陈石根.酶学[M].上海:复旦大学出版社,2001
[2]陈陶声,居乃玻,陈石根.固定化酶理论与应用[M].北京:轻工出版社:1987
[3]李彦峰、李军荣、伏莲娣.固定化酶的制备及应用[J].高分子通报,2001:13-23
[4]罗贵民,曹淑桂、张今.酶工程[M].北京:化学工业出版社,2002
[5]Manuel Ferrer,M Angeles Cruces,Francisco J Plou,et al.A simple procedure for the regioselective synthesis of fatty acid esters of maltose leucrose,maltot riose and n2dodecyl maltosides[J].Tetrahedron,2000,56:4053-4061
[6]杨守志.生物化学反应工程第三讲:生化反应器的性能[J].化工进展,1991,(2):44-47
[7]Yomi Watanabe.Purification of Tocopherols and Phytosterols by a Two-step in situ Enzymatic Reaction[J],JAOCS,2004(81)10:339-345
[8]徐兆瑜.略析分子筛的发展和应用[J].化工技术与开发,2007(36)7:31-36
[9]孙志浩.生物催化工艺学[M].北京:化学工业出版社,2004
[10]姚鹏.非水相中固定化脂肪酶催化酯合成反应的研究[D].博士学位论文,北京:北京化工大学,2000
[11]Yuji Shimada.Facile Purification of Tocopherols from Soybean Oil Deodorizer Distillate in High Yield Using Lipase[J],JAOCS,2000(77)10:1009-1013
[12]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[1]毕艳兰.油脂化学[M].北京:化学工业出版社,2005
[2]邢其毅、徐瑞秋、周政、裴伟伟.基础有机化学[M].北京:高等教育出版社,2002
[3]刘汝宽.制备生物柴油的催化剂研究进展[J].中国粮油学报,2006(21)3:273-276
[4]DAVID BGA.The theoretical and experimental study of the centrifugal molecular still[J].Aiche J,1972,18(2):269-276
[5]杨村、于宏奇.分子蒸馏技术[M].北京:化学工业出版社,2003
[6]乔国平,王兴国.分子蒸馏技术及其在油脂工业中的应用[J].粮食与油脂,2002,(5):25-27
[7]王军武,许松林,徐世民.分子蒸馏技术的应用现状[J].化工进展,2002,21(7):499-501
[8]Nguyen Anh Dung,Le Goffic Francois.Limits of wiped film short-path distilled[J].Chemical Engineering Scisence,1997,52(16):2661-2666
[9]Cvengros J,Pollak S,MicovM.Film wiping in the molecular evaporator[J].Chemical Engineering Journal,2001,81(1):9-14
[10]鲁志成,谷克仁,冶保献.浓硫酸催化脱臭馏出物脂肪酸甲酯化工艺研究[J].中国油脂,2005,30(3):21-24
[11]杨百勤.物理化学实验[M].北京:化学工业工业出版社,2001
[12]国家医药管理局上海医药设计院.化工工艺设计手册[M].北京:化学工业出版社,1989
[13]Schafer A.Vegetable Oil fatty acid methyl esters alternative dieselfuelsfor commercial vehicles engines[A].Plant O.Fuel Proc.Syrup[C].1997:29-46
[14]全国食品添加剂标准化技术委员会.GB19191-2003食品添加剂-天然维生素E[S].北京:中国标准出版社,2003.
[15]吴有炜.试验设计与数据处理[M].苏州:苏州大学出版社,2002
[1]国家药典委员会.中华人民共和国药典2000年版2部[M].北京:化学工业出版社,2000
[2]赵国志.植物甾醇及其产品开发利用[J].粮食与油脂,2006,2:3-6
[3]梁艳,张英.植物甾醇的提取分离和分析检测方法研究进展[J].中国粮油学报,2006,(21)3:1-7
[4]管伟举,谷克仁.植物甾醇研究紧张[J].粮食与油脂,2006,3:5-9
[5]吴素萍,章中.植物甾醇的研究现状[J].中国食物与营养,2007,9:20-21
[6]高瑜莹,裘爱泳.植物甾醇的分析方法[J].中国油脂,2001(26)1:25-29
[7]杨波涛.植物甾醇的提取与精制[D].无锡:江南大学硕士学位论文,2001
[8]许文林,王雅琼,黄一波等.重结晶法精制植物甾醇的溶剂选择[J].扬州大学学报(自然科学版),2002,(2):58-62
[9]韦继慷.植物甾醇提取工艺研究[D]硕士学位论文.浙江:浙江大学,2002
[10]Q/321283GEB07-2006,植物甾醇[S].江苏春之谷生物制品有限公司,2006
[1]Daeseok Han.Solubilization of Vitamin C in Fish Oil and Synergistic Effect with Vitamin E in Retarding
[2]高蓝、李浩明.几种抗氧化剂对鲲鱼油的抗氧化作用的研究[J].中国食品添加剂,1999,2:22-25
[3]Namiki M.Antiox idants/antimutagens in food,in CRC Crit[M].Rev Food Sci Nutr,CRC Press BocaRaton.1990,256
[4]吴克刚.大蒜提取物对鱼油抗氧化作用的研究及其机理的探讨[J].中国调味品2000,11:11-14
[5]Bran A L.Toxicology and biochemistry of BHA and BHT[J].JAOCS,1975,52(2):372-375
[6]潘蓄林.维生素E类化合物抗氧化活性的理论分析[J].化学研究与应用,2004(16)1:27-29
[7]凌关庭.食品抗氧化剂及其进展(Ⅱ)[J].粮食与油脂,2000(7):47-48
[8]赵贵兴.维生素E抗油脂氧化的功能[J].黑龙江农业科学,2003(1):45-48
[9]韩国麒.用于食用油脂的抗氧化剂[J].郑州粮食学院学报,1981,2:24-43
[10]宋国安.天然维生素的应用及开发前景[J].武汉工业学院学报,2000,20(4):29-32
[11]梁诚.天然VE生产现状与应用前景[J].化工技术经济,2002,20(4):29-32
[12]赵贵兴,陈霞维.维生素E抗油脂氧化效果的研究[J].中国油料作物学报,2002,24(3):58-59
[13]David DK.An evaluation of the mutiple effects of the antioxidant vitamins[J].Trend in food science technology,1997,8(6):198-203
[14]GB/T5538-1995,油脂过氧化值测定[S].北京:中国标准出版社,1995
[15]ENISO 6885:1998,Animal and vegetable fats and oils-Demination ofanisidine value[S].CEN,2000
[16]王璋,许时婴,汤坚.食品化学[M].北京:中国轻工业出版社,2002,110
[17]李彦萍、高荫榆.微量金属元素对乌桕类可可脂氧化稳定性研究[J].食品科学,2002(23)1:23-26
[18]W.G.Mentens,C.E.Swindells and B.F.Teasdale[J].JAOCS,1971,48:544-546
[19]M.H.Gordon,X.C.Weng.Antioxidant properties of Extracts from Tanshen[J].Food Chem,1992,44:119-122