Star anise oil extraction experiment
Illicium verum HooK.F. is an evergreen tree, an aromatic plant of China's specialties. It is mainly distributed in Guangxi, Guangdong, Guizhou and Yunnan provinces. Guangxi is the main producing area of ​​China's star anise, which accounts for 85% of the country's total and accounts for 70% of the world's total. The star anise has become one of the most important economic tree species in the country. Star anise and star anise oil is an excellent food seasoning that people like to use. Star anise oil has an aroma of anise. Star anise oil is widely used in food industry, brewing industry, beverage industry, daily cosmetics and pharmaceutical industry in addition to flavoring spices. At present, the production of star anise oil at home and abroad uses steam distillation, traditional organic solvent extraction, and supercritical CO2 fluid extraction. Different processes, star anise oil production and quality are different. In this paper, the trace method was used to compare the effects of 95% ethanol and acetone on the extraction rate of Anise oil.
1 Experimental section
1.1 Instruments and Drugs
A set of miniature chemical experiment equipment (developed by Yunnan University) and JD300-3 multi-functional electronic balance.
Octagonal (purchased in Guilin), 95% ethanol (CP), acetone (CP), petroleum ether (AR).
1.2 Experimental Principle
The main component of star anise is anise brain, namely, star anise brain, accounting for about 80% - 90%, as well as anisal ketone, anisaldehyde, methyl black pepper phenol, dipentene, etc. [1]. The molecular formula of star anise is C10H12O, its molecular weight is 148.20, and its structural formula is:
Star anise oil has a clear, spicy aroma and is sweet. The anise brain is a colorless to pale yellow liquid that freezes at low temperatures and is white crystalline. It is a liquid at room temperature and has a special aroma. It can be dissolved in 2-3 times 95% ethanol and acetone, and is almost insoluble with water.
1.3 Experimental Procedure
1.3.1 Method One [2]:
Weighed 2.000 grams of star anise powder with an electronic balance, packed in a filter paper into a cylindrical shape, placed in a Soxhlet extractor, added 20 ml of 95% ethanol to the flask, heated to reflux in a water bath, and returned to the Soxhlet extractor extract. Almost no color, stop heating, naturally cool, transfer the extract from the flask to a beaker by pouring down, wash the flask with a small amount of ethanol 2 to 3 times, and combine the extracts to concentrate, when the concentrate surface appears more dark green Distilled water is added to the mixture while hot, and the filtrate is further concentrated. When dark green is present on the liquid surface, an equal amount of distilled water is added and the mixture is filtered. This operation is repeated until no dark green is present. (The purpose is to remove the concentrate. The chlorophyll in the water) was then evaporated on a water bath to give a yellow-brown paste, star anise oil, with a yield of 0.1472 g and an extraction rate of 7.36%.
1.3.2, Method Two:
Weighed 2.000 grams of crushed star anise powder with an electronic balance, wrapped in filter paper into a cylindrical shape, placed in the Soxhlet extractor, added 20 ml of acetone to the flask, heated to reflux in a water bath, and returned to the Soxhlet extractor for extraction. The liquid is almost colorless. Stop the heating. Transfer the flask's extract to a beaker using a dumping method. Wash the flask with a small amount of acetone 2 or 3 times. Combine the extracts to concentrate. When more concentrated dark-colored material appears on the concentrate surface Add the same amount of distilled water and heat the filter, continue to concentrate the filtrate, add dark green water when the liquid surface appears, add the same amount of distilled water while hot filter, repeat this operation until no dark green appears (the purpose is to remove the concentrate Chlorophyll), and then placed in a water bath and evaporated to give a yellow-brown paste - star anise oil, yield 0.1142 g, the extraction rate of 5.62%.
2 Experimental results and discussion:
2.1 The effect of 95% ethanol and acetone on the extraction rate of star anise oil:
In this paper, 95% ethanol and acetone two different solvents were used to test the effect of their extraction rate of star anise oil. The results are shown in Table 1.
As can be seen from Table 1, 95% ethanol and acetone reagents are used in 20 ml, 95% ethanol siphon 8-15 times, using time 80-100min, the resulting star anise oil extraction rate than acetone siphon 10-15 times, with time 100-120min, the resulting star anise oil extraction rate is high, so the effect of refluxing star anise oil with 95% ethanol is better.
2.2 Anise oil physical and chemical properties &
Star anise oil: yellow-brown paste, insoluble in water, miscible with ether, chloroform, benzene, ethyl acetate, acetone, carbon disulfide, petroleum ether.
2.3 Experimental Features
Compared with the conventional experiment, using a small amount of micro-reagents, effectively saving the test funding. It has greatly improved the efficiency of running schools. At the same time, it has put forward higher requirements for students to conduct normative exercises and is conducive to fostering students to develop rigorous scientific attitudes.
3, the conclusion:
In this experiment, the trace method was used to compare the effects of 95% ethanol and acetone on the extraction rate of star anise oil. The results showed that the extraction of star anise oil with 95% ethanol was better.
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