加工工艺对茶油营养的影响以及脱臭馏出物中甾醇的精制
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摘要
油茶籽毛油中含有大量的活性物质如甾醇、角鲨烯等,这些活性物质对油茶籽油营养和保健作用及油茶籽油的稳定性起着重要的作用；但是油茶籽油中的活性物质在碱炼、脱色、脱臭工序中很容易损失,使油茶籽油品质下降。活性物质损失和油茶籽油酸败是加工过程中遇到的主要问题。
脱臭是油脂精炼工艺过程中的一道重要工序。脱臭馏出物主要成分为游离脂肪酸、VE、甾醇、甾醇酯等；从茶油脱臭馏出物中提取甾醇和角鲨烯等研究很少报导；因此,本课题首先对加工工艺对茶油营养成分的影响进行了研究,紧接着是甾醇和角鲨烯的纯化,尤其是甾醇的冷却结晶进行了优化,得到高纯度的甾醇；其次对角鲨烯精制做了研究,得到高纯度的角鲨烯。主要研究成果如下：
1.对油茶籽油毛油、碱炼油、脱色油、脱臭油、精炼油的理化性质及活性物质的含量进行了分析测定,研究了碱炼、脱色、脱臭三道工序对油茶籽油的酸值、过氧化值以及甾醇、α-生育酚、角鲨烯、总酚、β-胡萝卜素含量的影响。试验表明,脱色油酸值最高,为0.67(KOH)/(mg/g)；精炼油酸值最低,为0.32(KOH)/(mg/g),甾醇、α-生育酚、角鲨烯含量以毛油中最高,分别为908.75mg/kg、21.60mg、102.31mg/kg,且角鲨烯含量显著高于其他油茶籽油(P<0.05)。总酚、p-胡萝卜素含量以精炼油中最低,分别为21.750mg/kg、0.130mg/kg,脱色和脱臭两道工序是影响油茶籽油品质的重要环节。
2.以茶油皂脚、脱臭馏出物、冬化物为研究对象,结合加工工序研究茶油副产物中活性物质分布以及构成。结果表明,在四道加工工序中,脱臭对油茶籽油中α-生育酚、甾醇、角鲨烯的含量影响最大,分别损失了52.1%、34.5%、55.4%,而相应脱臭馏出物中三种活性物质含量最高,分别为750.90 mg.kg-1、2463.58mg.kg-1、8887.47 mg.kg-1。脱色对油茶籽油中α-生育酚、甾醇、角鲨烯的含量影响次之,分别损失了11.5%、9.5%、8.5%。碱炼和冬化对油茶籽油脂肪酸组成有很大的影响。
3.采用乙醇萃取VE,皂化法提取茶油脱臭馏出物中甾醇化合物,以正己烷为结晶溶剂对甾醇化合物进行重结晶。VE最佳萃取参数：液料比3：1,搅拌时间30min,萃取温度55℃,搅拌速度80r/min。甾醇最佳的提取工艺条件：碱料比1：5(KOH),醇料比15：1(乙醇),皂化时间3h,温度85℃；最佳结晶工艺条件：液料比3：1,溶剂正己烷,结晶温度-2℃,结晶时间24h,三次重结晶后精制甾醇的纯度可以达到89.3%。
The oil-tea camellia seed oil contains large amount of bioactive constituents such as phytosterol,squalene and so on, These bioactive constituents take an important role in the nutrition and health of and in the stability of oil-tea camellia seed oil.But these bioactive constituents can easily loss in the process of the alkali refining, bleaching, deodorization, effecting the quality of oil-tea camellia seed oil. The losses of bioactive constituents and rancidity of oil-tea camellia seed oil are the main problems in processing procedures.
Deodorizing is the most important process in the Oil refining process. Main componential contents of deodorizer distillates in oil-tea camellia seed oil are free fatty acids, VE, phytosterol, sterol esters and so on. There are few reports on phytosterol and squalene abstraction from deodorizer distillates of oil-tea camellia seed oil. Therefore, this paper firstly studied the effects of processing operations on the contents of bioactive constituents and physical-chemical properties of oil-tea camellia seed oil. Then we studied the technological condition of the abstraction of phytosterol, especially optimizing the recrystallization conditions, and getting pure phytostero. Then, we purified the crude squalene, getting pure squalene. The main resμLts of research in this dissertation are as follows:
1. The changes of bioactive constituents and physical-chemical properties of the oil-tea camellia seed oil in different processing procedures, such as crude oil、alkalized oil、bleached oil、deodorized oil and refined oil were investigated. Acid value, peroxide value and the content of total sterol, a-tocopherol, squalene,polyphenols andβ-carotene in variety of samples were determined by means of wet chemical and instrμment methods.The resμLts showed that the bleached oil has the highest acid value, which was 0.67(KOH)/(mg/g). The refined oil has the lowest acid value, which was 0.32(KOH)/(mg/g); Compared with others, crude oil contained more total sterol(908.75mg/kg),a-tocopherol(21.60mg/kg),squalene(102.31mg/kg);what's more, the content of squalene in crude oil was significantly higher than that in other oil(P<0.05).For the total content of polyphenols andβ-carotene,the refined oil is the lowest, which was 21.75mg/kg,0.006mg/kg, respectively. The way of bleaching and deodorizing is important processing technology to the oil-tea camellia seed oil qualities.
2. The experimental investigation of soapstock、deodorization distillate、winterization property, Combined with machining operations research Oil-tea camellia seed oil by-products of bioactive constituents distribution and composition.The resμLts showed that of the four processing procedures, the deodorization effected on the content of a-tocopherol, sterol, squalene in the oil-tea camellia seed oil was the greatest, content losing 52.1%、34.5%、55.4%, respectively.While the content of a-tocopherol, sterol, squalene of the corresponding deodorizer distillate was the highest,750.90 mg.kg-1、2463.58 mg.kg-1、8887.47mg.kg-1, respectively. The influence of decoloration was greater, content losing 11.5%、9.5%、8.5%, respectively. The way of decoloration and deodorization was important processing technology to the content of bioactive constituents in oil-tea camellia seed oil.The alkali refining and dewaxing effected the component of fatty acid was very great.
3. The study extracts VE from oil-tea camellia seed oil deodorization distillate by alcohol and gains phytosterols by saponification, the phytosterols were dissolved in n-hexane to recrystallize. The optimal conditions extraction of VE are liquor-raw material ratio 3:1, back flow extract 30min, extraction temperature 55℃, rate 80r/min.The optimal conditions extraction of phytosterol are as following:potassium hydroxide-raw material ratiol:5,ethanol-raw material ratio 15:1, and back flow saponified 3h under 85℃; The optimal crystallization conditions are as following: n-hexane-raw material ratio 3:1, temperature-2℃,time 24h,the refined phytosterols with 89.3% purity were obtained by three recrystallizations.
脱臭是油脂精炼工艺过程中的一道重要工序。脱臭馏出物主要成分为游离脂肪酸、VE、甾醇、甾醇酯等；从茶油脱臭馏出物中提取甾醇和角鲨烯等研究很少报导；因此,本课题首先对加工工艺对茶油营养成分的影响进行了研究,紧接着是甾醇和角鲨烯的纯化,尤其是甾醇的冷却结晶进行了优化,得到高纯度的甾醇；其次对角鲨烯精制做了研究,得到高纯度的角鲨烯。主要研究成果如下：
1.对油茶籽油毛油、碱炼油、脱色油、脱臭油、精炼油的理化性质及活性物质的含量进行了分析测定,研究了碱炼、脱色、脱臭三道工序对油茶籽油的酸值、过氧化值以及甾醇、α-生育酚、角鲨烯、总酚、β-胡萝卜素含量的影响。试验表明,脱色油酸值最高,为0.67(KOH)/(mg/g)；精炼油酸值最低,为0.32(KOH)/(mg/g),甾醇、α-生育酚、角鲨烯含量以毛油中最高,分别为908.75mg/kg、21.60mg、102.31mg/kg,且角鲨烯含量显著高于其他油茶籽油(P<0.05)。总酚、p-胡萝卜素含量以精炼油中最低,分别为21.750mg/kg、0.130mg/kg,脱色和脱臭两道工序是影响油茶籽油品质的重要环节。
2.以茶油皂脚、脱臭馏出物、冬化物为研究对象,结合加工工序研究茶油副产物中活性物质分布以及构成。结果表明,在四道加工工序中,脱臭对油茶籽油中α-生育酚、甾醇、角鲨烯的含量影响最大,分别损失了52.1%、34.5%、55.4%,而相应脱臭馏出物中三种活性物质含量最高,分别为750.90 mg.kg-1、2463.58mg.kg-1、8887.47 mg.kg-1。脱色对油茶籽油中α-生育酚、甾醇、角鲨烯的含量影响次之,分别损失了11.5%、9.5%、8.5%。碱炼和冬化对油茶籽油脂肪酸组成有很大的影响。
3.采用乙醇萃取VE,皂化法提取茶油脱臭馏出物中甾醇化合物,以正己烷为结晶溶剂对甾醇化合物进行重结晶。VE最佳萃取参数：液料比3：1,搅拌时间30min,萃取温度55℃,搅拌速度80r/min。甾醇最佳的提取工艺条件：碱料比1：5(KOH),醇料比15：1(乙醇),皂化时间3h,温度85℃；最佳结晶工艺条件：液料比3：1,溶剂正己烷,结晶温度-2℃,结晶时间24h,三次重结晶后精制甾醇的纯度可以达到89.3%。
The oil-tea camellia seed oil contains large amount of bioactive constituents such as phytosterol,squalene and so on, These bioactive constituents take an important role in the nutrition and health of and in the stability of oil-tea camellia seed oil.But these bioactive constituents can easily loss in the process of the alkali refining, bleaching, deodorization, effecting the quality of oil-tea camellia seed oil. The losses of bioactive constituents and rancidity of oil-tea camellia seed oil are the main problems in processing procedures.
Deodorizing is the most important process in the Oil refining process. Main componential contents of deodorizer distillates in oil-tea camellia seed oil are free fatty acids, VE, phytosterol, sterol esters and so on. There are few reports on phytosterol and squalene abstraction from deodorizer distillates of oil-tea camellia seed oil. Therefore, this paper firstly studied the effects of processing operations on the contents of bioactive constituents and physical-chemical properties of oil-tea camellia seed oil. Then we studied the technological condition of the abstraction of phytosterol, especially optimizing the recrystallization conditions, and getting pure phytostero. Then, we purified the crude squalene, getting pure squalene. The main resμLts of research in this dissertation are as follows:
1. The changes of bioactive constituents and physical-chemical properties of the oil-tea camellia seed oil in different processing procedures, such as crude oil、alkalized oil、bleached oil、deodorized oil and refined oil were investigated. Acid value, peroxide value and the content of total sterol, a-tocopherol, squalene,polyphenols andβ-carotene in variety of samples were determined by means of wet chemical and instrμment methods.The resμLts showed that the bleached oil has the highest acid value, which was 0.67(KOH)/(mg/g). The refined oil has the lowest acid value, which was 0.32(KOH)/(mg/g); Compared with others, crude oil contained more total sterol(908.75mg/kg),a-tocopherol(21.60mg/kg),squalene(102.31mg/kg);what's more, the content of squalene in crude oil was significantly higher than that in other oil(P<0.05).For the total content of polyphenols andβ-carotene,the refined oil is the lowest, which was 21.75mg/kg,0.006mg/kg, respectively. The way of bleaching and deodorizing is important processing technology to the oil-tea camellia seed oil qualities.
2. The experimental investigation of soapstock、deodorization distillate、winterization property, Combined with machining operations research Oil-tea camellia seed oil by-products of bioactive constituents distribution and composition.The resμLts showed that of the four processing procedures, the deodorization effected on the content of a-tocopherol, sterol, squalene in the oil-tea camellia seed oil was the greatest, content losing 52.1%、34.5%、55.4%, respectively.While the content of a-tocopherol, sterol, squalene of the corresponding deodorizer distillate was the highest,750.90 mg.kg-1、2463.58 mg.kg-1、8887.47mg.kg-1, respectively. The influence of decoloration was greater, content losing 11.5%、9.5%、8.5%, respectively. The way of decoloration and deodorization was important processing technology to the content of bioactive constituents in oil-tea camellia seed oil.The alkali refining and dewaxing effected the component of fatty acid was very great.
3. The study extracts VE from oil-tea camellia seed oil deodorization distillate by alcohol and gains phytosterols by saponification, the phytosterols were dissolved in n-hexane to recrystallize. The optimal conditions extraction of VE are liquor-raw material ratio 3:1, back flow extract 30min, extraction temperature 55℃, rate 80r/min.The optimal conditions extraction of phytosterol are as following:potassium hydroxide-raw material ratiol:5,ethanol-raw material ratio 15:1, and back flow saponified 3h under 85℃; The optimal crystallization conditions are as following: n-hexane-raw material ratio 3:1, temperature-2℃,time 24h,the refined phytosterols with 89.3% purity were obtained by three recrystallizations.
引文
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