| In this paper, the deodorizer distillate was extracted from Xinjiang cottonseed oil. The different methods of deodorization distillate esterification and the conditions of extraction vitamin E process from the esterification were investigated. The fatty acid in deodorizer distillate was esterified under the condition of intermittent and continuous esterification. The vitamin E was extracted by molecular distillation, and the extracted material was detected and analyzed by infrared spectroscopy and high performance liquid chromatography. The results of the studies are listed as follows:1. Optimization of esterification conditionsThe fatty acid in deodorizer distillate were esterified by intermittent enzymatic esterification method. Based on the single factor experiments, Design-Expert date analysis software was used to select the reaction temperature, enzyme concentration, reaction time and ratio of acid as four parameters of response surface design to optimize extraction process. In addition, Quadratic model fitting which showed a significant influence was carried out with the help of response surface method(RSM) module. The results revealed that the ratio of acid to alcohol and the amount of enzyme was significantly effected the rate of esterification. The results showed: reaction temperature of 60℃, enzyme concentration of 62.86plu/g, reaction time of 9h and ratio of acid to alcohol of 1.00:1.65(g:m L). With the optimization conditions, the RSM model predicted the esterification rate was 97.27%, while the actual experimental values was(97.09 + 0.09)%, and the actual value was basically consistent with the predicted value.2. Continuous enzymatic esterification of cotton-seed oil deodorizer distillateThe deodorizer distillate was treated by continuous enzymatic esterification method.Firstly.Based on the single factor experiments, Design-Expert date analysis software was used to select the ratio of acid to alcohol,feed rate, enzyme concentration, reaction temperature as four parameters of response surface design to optimize extraction process. In addition, Quadratic model fitting which showed a significant influence was carried out with the help of response surface method(RSM) module. The results revealed that the ratio of acid to alcohol, the amount of enzyme and the reaction temperature was significantly effected the rate of esterification. The results showed: ratio of acid to alcohol of 1.00:1.65(g:m L),the feed rate 2.05 m L/min, reaction temperature of 56.28℃, the amount of enzyme 5.65 g. With the optimization conditions, the RSM model predicted the esterification rate was 94.21%, while the actual experimental values was(93.56±0.06)%, and the actual value was basically consistent with the predicted value.3 Enrichment vitamin E by molecular distillationThe vitamin E was extracted by molecular distillation method. The effect of feed rate,vacuum distillation, scraper speed and temperature on the content of vitamin E were studied. In addition, Quadratic model fitting which showed a significant influence was carried out with thehelp of response surface method(RSM) module. The results revealed that the ratio of acid to alcohol, the vacuum degree was significantly effected the rate of esterification. The results showed: feed rate 1m L/min, distillation temperature 203 ℃, scraper speed 580r/min, vacuum degree 0.5mbar. With the optimization conditions, the RSM model predicted the the optimum extraction conditions of vitamin E was 95.86%, while the actual experimental values was(93.29±0.03)%, and the actual value was basically consistent with the predicted value.4. Detection and analysis of vitamin EFirstly, the extracted material was analyzed by infrared spectrometer. The results were compared and analyzed by IR spectra of standard vitamin E, which speculated that the extracted for vitamin E. And the HPl C was applied on the extracted sample, blank solution and standard vitamin E. The results indicated that the objective is the vitamin E. |
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