The Extraction Of Effective Components From Star Anise With Hydro-Diffusion Distillation

Hydro-diffusion distillation technology was a new technology firstly appeared in foreign countries, compared with the traditional steam distillation, the steam would pass through the material from top to bottom, owing to the positive effect of gravity, water dispersion was strengthened, that was more conducive to the extraction of active ingredients. In the present work, star anise were the raw materials to extract star anise oil and shikimic acid at the same time via the hydro-diffusion distillation and determined their optimal extraction process, then the activated carbon decolorization process of extracting solution were carried out, and finally purified shikimic acid used the way of wine yeast and recrystallization. All the results were showed below:1. The Hydro-diffusion distillation method was studied to extract star anise oil and shikimic acid, according to the single factor experiment and orthogonal experiments to determined the optimal extraction process:(1). The extraction conditions of star oil from star anise via hydro-diffusion distillation were:the steam consumption was 3500mL, raw material particle size was 0.32cm, extraction time was 3h. In optimal conditions, the extraction rate of star anise oil was 7.16%. The research was studied in a 5L stainless still, raw material was 1200g, the oil extraction rate in three hours was 6.92%.(2). While in the extraction of essential oil,it could get water-soluble extract, the main components were shikimic acid and polysaccharides. The extraction process of star anise shikimic acid and polysaccharides were optimized, under the conditions of the steam consumption was 3000mL、raw material particle size was 0.32cm、extraction time was 5h, the extraction rate of star anise shikimic acid was 6.26%, while the extraction rate of star anise polysaccharide was 10.18%. The research was studied in a 5L stainless still, raw material was 1200g, the extraction rate of shikimic acid in five hours was 6.92%, the extraction rate of polysaccharide was 6.92%.(3). Integrated weighted scoring method was used to obtain simultaneous extraction process of star anise oil and shikimic acid, under the conditions of the steam consumption was 3000mL、raw material particle size was 0.32cm、 extraction time was 5h, the extraction rate of star anise shikimic acid was 6.26%, while the extraction rate of star anise oil was 6.20%.2. Compared the difference of essential oil rate with the way between hydro-diffusion distillation and the traditional steam distillation, and analyzed essential oils by GC-MS and GC:(1). The essential oil rate with the way of hydro-diffusion distillation in three hours was 7.16%, using the traditional water distillation in three hours was 5.08%、in seven hours was 7.43%, the oil extraction rate with hydro-diffusion distillation was faster than the traditional water distillation.(2). Analyzed by GC-MS:the major components characterized in the oil extracted from hydro-diffusion distillation were trans-anethole (90.38%)、 limonene (2.9%)、 cumin(1.97%)、 diisobutyl phthalate (0.42%). In terms of the oil from the traditional steam distillation, the main ingredients were similar to the hydro-diffusion distillation, but the content was different:trans-anethole (86.34%), limonene (5.73%)、 cumin (2.32%)、 caryophyllene(0.66%). The major constituent trans-anethole was higher in the oil extracted from hydro-diffusion distillation.3. Compared the difference between hydro-diffusion distillation water distillation and hot water extraction method in the extraction rate of star anise shikimic acid, and used UV to quantitative analysis. Under the conditions of the steam consumption 3500mL、raw material particle size 0.32cm、 extraction time、 3h, the extraction rate with hydro-diffusion distillation in five hours was 6.20%、 with the way of hot water extraction method in three hours and three extraction times, the extraction rate was 6.58%; The extraction rate with water distillation in seven hours was 5.21%. The extraction efficacy with the hydro-diffusion distillation was higher than the traditional water extraction method.4. The decolorization process with activated carbon was researched, decolorization rate and shikimic acid retention as index. Under the conditions of activated carbon dosage was 1.5%、decolorization temperature was 80℃、 decolorization time was 50 min, the decolorization effect was best, the decolorization rate was 91.7%, the retention rate of shikimic acid and polysaccharide were 56.76% and 61.34%. After purification, the shikimic acid crystals were obtained, which the color was yellow, the purity was 12.17%, the yield was 3.98%. The shikimic acid crystals contained some polysaccharides, polysaccharide and shikimic acid was difficult to separate.5. Using wine yeast fermentation to remove polysaccharide amd purified shikimate. The yeast removed polysaccharides by anaerobic respiration, after 14 days of fermentation, the removal rate of polysaccharides were more than 90%, shikimic acid remain the same. Using solvent extraction crystallized three times could get shikimic acid, the purity was 90.24%, the yield was 3.36%. In combination with potassium dichromate method and gas chromatography to analysis fermentation products, the results showed that:the content of the fermentation product was ethanol, the extracting solution from the 180g raw materials during yeast fermentation were available to get 15.18g ethanol.