Research Of Preparation Crafts And Analysis Methods Of Fenglasu

Through the experiment, preparation and purification crafts of fenglasu began with beeswax by saponification was developed. Also, a better craft was determined by comparing two kinds of crystallization. Finally, GC methods were developed for the determination of policosanol and residual solvents in fenglasu.1. By the comparing refining process of beeswax including filtering, hydrate deliming, delinking and crystallization, a conclusion was drawn that effects of refining process were not notable. The optimal condition of saponification was studied by orthogonal test and single-factor tests considering reaction time, temperature, concentration of alcohol, solid-liquid ratio, amount of Sodium hydroxide; effect of phase transfer catalyst and ultrasonic wave. The results showed that the optimal saponification condition was 80 ℃, 85% of alcohol concentration, 1:5 g·mL-1 solid-liquid ratio, 30 min for reaction, 35 g·L-1 of concentration of NaOH and poor effect of phase transfer catalyst and ultrasonic wave.2. An optimal extraction craft was developed by single-factor tests, the influence of alcohol, volume of water, pH in solution, stirring time and drying way were studied. The result turned out that the optimal condition was no treatment of alcohol, 5 mL·g-1 of water, pH=1, 45 min of strring time and air drying. To evaluate the effectiveness of the solvents, investigations were made with ethyl acetate, butyl acetate, n-heptane, acetone and mixture of ethyl acetate and n-heptane. At last, ethyl acetate was the best chosen for the recrystallization with liquid-solid ratio of 70 mL?g-1. An optimal recrystallization condition was crystallizing for 2 hours by natural cooling at the temperature of 15 ℃ was studied by orthogonal test with the factors as crystallization time, temperature and cooling way. Recrystallization with ethyl acetate and n-heptane each time, the results showed that the optimal solvent amount were 20 mL·g-1 of ethyl acetate and 45 mL·g-1 of n-heptane when studied by single-factor test with the factor of the amount of ethyl acetate and n-heptane.3. With the optimized reaction conditions determined, the content of triacontanol was 58.3 % after one recrystallization only by ethyl acetate, and also 67.4 % of octacosanol and triacontanol 31.9 % of yield was achieved also. Fenglasu, which was recrystallized by ethyl acetate and n-heptane each time, included 67.7 % of triacontanol, 78.1 % of the sum of octacosanol and triacontanol and 26.7 % of yield. These two crafts met the criterion of residual solvents. The two craft which used two times recrystallization method to purify was set down as final craft.4. GC methods were established for the determination of tetracosanol, hexacosanol, octacosanol, triacontanol and dotriacontanol in fenglasu. The established methods were easy to control with high response rate, repeatability, resolution and specifity that could meet sample analysis’ demand. Also, a method for the determination of residual solvents in fenglasu was developed which could be used for quality control.