棉籽油脱臭馏出物中甾醇的提取及纯化研究
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摘要
本文系统地研究了棉籽油脱臭馏出物中甾醇提取方法,甾醇的结晶纯化及稳定性和抗氧化研究,同时制备了甾醇包合物,主要得出以下结论：
采用SCF-CO2法和转酯化-结晶法对棉籽油脱臭馏出物中甾醇进行萃取,SCF-CO2法最佳萃取条件为：萃取压力为20Mpa,萃取温度为45℃,CO2流量为25L/h,萃取时间为3.0h,甾醇萃取率为81.3%,甾醇纯度达到83.24%。转酯化-结晶法最佳萃取条件为：料液比为1/5Wt/V,酯化温度为60℃,催化剂使用量为35%,酯化时间为4h,甾醇提取率为54.8%,甾醇纯度达到49.1%。所以选择超临界CO2萃取法比较合理。
甾醇纯化工艺中,以甾醇得率为指标,最佳纯化条件为：结晶终止温度为-10℃,养晶时间为20h,料液比为1/20Wt/V,得出甾醇纯度为93.6%。
甾醇稳定性研究表明：贮藏时间越长,甾醇稳定性越差,时随着温度的升高,甾醇稳定性下降,自然光下保存的甾醇的稳定性下降, ph值4～6之间甾醇相对比较稳定,各金属离子影响甾醇稳定的先后次序为：Cu2+>Ca2+>Fe3+>Na+>Zn2+。甾醇对油脂都有较好的抗氧化效果,在油脂的抗氧化过程中,不同的抗氧化剂对油脂抗氧化效果从强到弱依次为：EDTA>甾醇>维生素E>维生素C>柠檬酸,抗氧化剂之间有较好的协同作用,其中较佳的抗氧化剂组合为甾醇+EDTA,对油脂抗氧化效果最理想的剂量比为1/3(甾醇/EDTA)。
甾醇包合物的最佳工艺条件为：包合比为1/8,包合温度为50℃,搅拌时间为1.5h,得出包合率为93.9%。甾醇包合物即解决了甾醇稳定性的问题而且在抗氧化应用中有重要的意义。
A proeess for extracting plant sterol from cotton oil deodorizer distillate and the crystal purification, stability, antioxidantive of the sterol was systematically studied in this paper. Meanwhile, the sterol composites were prepared. The following is the mainly study results:
Study on extraction of plant sterol from cotton oil with SCF-CO2 and transesterifieation. The optimal synthetic conditions for SCF-CO2 were obtained as follwos:extraction pressure 20 Mpa; extraction temperature 45℃; CO2 flow rate 25L/h; extraction time 3.0 hour. Under this optimum technology condition, the recovery rate is 81.3% and purity of rough sterol is 83.24%. The optimal condition for transesterification of sterol ester has been obtained as followed:the rate of blend composition:1/5Wt/V; temperature:60℃; the dosage of catalyst:35%; time:4.0 hour. The recovery rate is 54.8% and purity of rough sterol is 49.1%. So we choosed SCF-CO2 to extraction of plant sterol.
We used yield rate of sterol as index to obtain the optimal condition of purification. The optimum technical conditions were obtained as follwos:recrystallization temperature-10℃; recrystallization time 20 hour; the rate of blend composition:1/20Wt/V.The purity of refining sterols is 93.6%.
The anti-oxidation of the sterols is preferable to lipid. The diffirent antioxidants'anti-oxidation effects in lipid as follow:EDTA>sterols>vitamin E>vitamin C>critic acid. Various antioxidants used in together can enhance the effects of anti-oxidation. The optimal in lipid is concluded to mix the sterols with EDTA to a content of 1/3.
The study of sterol stability showed:the sterol stability degraded with storage and with the temperature step up. The stability of sterol under natural light decreased. It was stable in the pH range from 4 to 6. The stability was affected to different metal ion:Cu2+>Ca2+>Fe3+>Na+>Zn2+.
The optimal condition for inclusion of sterol has been obtained as followed:inclusion ratio:1/8, inclusion temperature:50℃, inclusion time:1.5h. The inclusion rate is 93.9%. The sterol composites not only increase the stability of the sterols,but also are significance in applying to antioxidation.
采用SCF-CO2法和转酯化-结晶法对棉籽油脱臭馏出物中甾醇进行萃取,SCF-CO2法最佳萃取条件为：萃取压力为20Mpa,萃取温度为45℃,CO2流量为25L/h,萃取时间为3.0h,甾醇萃取率为81.3%,甾醇纯度达到83.24%。转酯化-结晶法最佳萃取条件为：料液比为1/5Wt/V,酯化温度为60℃,催化剂使用量为35%,酯化时间为4h,甾醇提取率为54.8%,甾醇纯度达到49.1%。所以选择超临界CO2萃取法比较合理。
甾醇纯化工艺中,以甾醇得率为指标,最佳纯化条件为：结晶终止温度为-10℃,养晶时间为20h,料液比为1/20Wt/V,得出甾醇纯度为93.6%。
甾醇稳定性研究表明：贮藏时间越长,甾醇稳定性越差,时随着温度的升高,甾醇稳定性下降,自然光下保存的甾醇的稳定性下降, ph值4～6之间甾醇相对比较稳定,各金属离子影响甾醇稳定的先后次序为：Cu2+>Ca2+>Fe3+>Na+>Zn2+。甾醇对油脂都有较好的抗氧化效果,在油脂的抗氧化过程中,不同的抗氧化剂对油脂抗氧化效果从强到弱依次为：EDTA>甾醇>维生素E>维生素C>柠檬酸,抗氧化剂之间有较好的协同作用,其中较佳的抗氧化剂组合为甾醇+EDTA,对油脂抗氧化效果最理想的剂量比为1/3(甾醇/EDTA)。
甾醇包合物的最佳工艺条件为：包合比为1/8,包合温度为50℃,搅拌时间为1.5h,得出包合率为93.9%。甾醇包合物即解决了甾醇稳定性的问题而且在抗氧化应用中有重要的意义。
A proeess for extracting plant sterol from cotton oil deodorizer distillate and the crystal purification, stability, antioxidantive of the sterol was systematically studied in this paper. Meanwhile, the sterol composites were prepared. The following is the mainly study results:
Study on extraction of plant sterol from cotton oil with SCF-CO2 and transesterifieation. The optimal synthetic conditions for SCF-CO2 were obtained as follwos:extraction pressure 20 Mpa; extraction temperature 45℃; CO2 flow rate 25L/h; extraction time 3.0 hour. Under this optimum technology condition, the recovery rate is 81.3% and purity of rough sterol is 83.24%. The optimal condition for transesterification of sterol ester has been obtained as followed:the rate of blend composition:1/5Wt/V; temperature:60℃; the dosage of catalyst:35%; time:4.0 hour. The recovery rate is 54.8% and purity of rough sterol is 49.1%. So we choosed SCF-CO2 to extraction of plant sterol.
We used yield rate of sterol as index to obtain the optimal condition of purification. The optimum technical conditions were obtained as follwos:recrystallization temperature-10℃; recrystallization time 20 hour; the rate of blend composition:1/20Wt/V.The purity of refining sterols is 93.6%.
The anti-oxidation of the sterols is preferable to lipid. The diffirent antioxidants'anti-oxidation effects in lipid as follow:EDTA>sterols>vitamin E>vitamin C>critic acid. Various antioxidants used in together can enhance the effects of anti-oxidation. The optimal in lipid is concluded to mix the sterols with EDTA to a content of 1/3.
The study of sterol stability showed:the sterol stability degraded with storage and with the temperature step up. The stability of sterol under natural light decreased. It was stable in the pH range from 4 to 6. The stability was affected to different metal ion:Cu2+>Ca2+>Fe3+>Na+>Zn2+.
The optimal condition for inclusion of sterol has been obtained as followed:inclusion ratio:1/8, inclusion temperature:50℃, inclusion time:1.5h. The inclusion rate is 93.9%. The sterol composites not only increase the stability of the sterols,but also are significance in applying to antioxidation.
引文
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