Optimization Of The Purification Process Of Natural Borneol

Borneol (d-Borneol), also known as the D-borneol, plum slices, is commonly called camphane alcohol. It has the medicinal functions such as improving eyesight, reducing swelling, killing the pain, clearing away heat and toxic materials, preventing cancer and curing cancer. It widely used in medicine and daily necessities. This paper takes natural borneol crude (Borneol Cinnamomum camphora leaves of extract using Steam distillation extract) in Xinhuang County of Hunan provinceand and borneol fragments (borneol fragments from crystallization of crude borneol mother liquor) as raw material. Research high purity, high yield purification process and the suitable process conditions. To provide a theoretical basis and data support for further industrialized purification of natural borneol. In recent years, the demand for natural borneol is increasing in China. But the market is almost entirely occupated by synthetic borneol (Mechanisms of Borneol). However, the overall level of China’s natural borneol processing industry is not high. As few enterprises specialized in natural borneol processing, small-scale and scattered layout, it’s difficult to form group advantage. And the solvent crystallization method is mostly used in the traditional separation and purification, the yield is not high enough to achieve efficient use of natural borneol resource.In this paper, with natural bomeol taken as the object of research, authors use three method:the solvent crystallization method, method-supercritical CO2 extraction method and column chromatography purification method separate and purified borneol crude and borneol fragments. The specific findings are as follows:1.With the traditional solvent crystallization method adopted to separate and purify the crude borneol, the regular influence pattern of factors such as different solvents, crystallization time, crystallization temperature, liquid-solid ratio on product purity and yield were investigated. The result showed that under the conditions of a solvent of 120# gasoline, a crystallization time of 6d, a crystallization temperature of 8 ℃ and liquid-solid ratio of 1:1.4, the purity of natural borneol in crystalline product was 97.06%(GC method). And the crystalline product yield was 56.23%. The sequence of the each factor’s influence on the purity of natural borneol in crystalline products was liquid-solid ratio> crystallization temperature> crystallization time. And the sequence of the each factor’s influence on the yield of the crystalline product was:liquid-solid ratio> crystallization time> crystallization temperature.2.With Borneol fragments as raw material, using the solvent crystallization resep-aration and purification. And the result shows that under the conditions of a solvent of 120# gasoline, a crystallization time of 6 d, a crystallization temperature of 8 ℃ and a liquid-solid ratio of 1:1.4, with the borneol fragments of the mother liquid twice recrystallized, the purity of natural borneol was more than 96%, meeting the requirement of’Pharmacopoeia of the People’s Republic of China’. And the yield of crystalline product was 32.81%.3.With the supercritical CO2 extraction method first adopted to separate and purify the borneol fragments of mother liquid, the regular influence pattern of factors such as extraction pressure, extraction temperature, CO2 flow rate, extraction time on product purity and yield were investigated. The result showed that under the conditions of an extraction pressure of 10 MPa, a crystallization temperature of 38 ℃, a CO2 flow rate of 10 L·h-1 and a crystallization time of 20 min, the purity of natural borneol in crystalline product increased from 65.17% to 98.18%. And the crystalline product yield reached 56.23%, far more beyond the 32.81%, the product yield when solvent crystallization method was adopted. The sequence of the each factor’s influence on the purity of natural borneol was crystallization time> CO2 flow rate> extraction pressure> crystallization temperature. And the sequence of the each factor’s influence on the yield was:extraction pressure> CO2 flow rate> crystallization temperature> crystallization time.4.With the column chromatography purification method adopted to separate and purify borneol fragments, static and dynamic separation research were respectively done. The optimization process using silica gel 200-300 mesh to separate and purify borneol fragments is adsorption liquid of about pH= 6, an adsorption temperature of 30 ℃, an adsorption liquid flow rate of 2 BV/h, an adsorption liquid volume(?)5 BV, an eluent of 20 %(V/V), ethyl acetate (30%)-petroleum ether (70%), a desorption temperature of 40 ℃, a desorption dosage of 3.5 BV. The purity of natural borneol in the product increased from 65.17% to 99.26%. It can be completely isolated fragments of natural borneol and camphor these two substances, far more beyond the standard required in’Pharmacopoeia of the People’s Republic of China’.