Study on the Effective Components of Ledum Palustre L. in Daxing’an Mountain Region
|School||Northeast Forestry University|
|Keywords||Ledum Supercritical carbon dioxide extraction High Performance Liquid Chromatography Essential oils : coumarin Ursolic acid|
Ledum volume of Heilongjiang Province rich wild plant resources, domestic and foreign research data shows that it has an important spice and medicinal values, growth in Daxinganling Ledum as the research object, the establishment of a high-performance liquid chromatography analysis Ledum active ingredient - coumarin and Ursolic chromatographic conditions to determine the best conditions for supercritical carbon dioxide extraction method to extract coumarin and essential oils, to determine the optimum conditions of ultrasonic extraction of ursolic acid and silica gel column separation of its separation and purification. The results are as follows: 1. HPLC analysis of coumarin contents chromatographic conditions: ODS column (25cm × 4.6 mm, 5 μm); mobile phase: acetonitrile: water (volume ratio 40:60); detection wavelength: 273nm; Injection volume: 10 μL; Flow rate: 1.0mL/min; column temperature: 25 ° C. Ursolic acid content of high-performance liquid chromatography analysis of chromatographic conditions: mobile phase: methanol: water (volume ratio 90:10); detection wavelength: 210 nm; the remaining conditions ibid. 2. The supercritical CO 2 extraction extract coumarin best conditions: extraction temperature 45 ° C, extraction pressure 30Mpa, separation temperature 55 ° C, extraction pressure are the main factors affecting the extraction rate. The supercritical CO 2 the extraction rate of the extraction method is 14.13μg / g, is Tifa Ti achieved rate (4.26μg / g) with ethanol and dip 3.32 times. 3. The supercritical CO 2 Extraction Du essential oils: extraction temperature 55 ° C, extraction pressure 25Mpa the first separation autoclave pressure 8Mpa, separation the cauldron temperature of 35 ℃. Which separation kettle pressure is a major factor. By gas chromatography - mass spectrometry (GC-MS) to analyze and identify the components of the extract by the standard spectrum Gallery retrieve supercritical extract containing waxy and fatty acids, such as non-volatile impurities. 4. Daxinganling region the Ledum different collection period essential oils and ursolic content are different, both the highest content in fruit ripening in August, its collection period may be relaxed in production. 5. Ursolic acid extraction method is ultrasonic extraction, ultrasonic extraction conditions of 95% ethanol concentration, the the ultrasonic temperature of 45 ° C for 30min, frequency 40KHz, in which the concentration of ethanol is the main influencing factors. 6. With silica gel column chromatography method to extract preliminary separation, eluent chloroform: methanol (volume ratio 500:1), the color-developing agent for a 5% sulfuric acid in ethanol, and evaporated extract obtained after the solvent was recovered, with 95% ethanol and recrystallized once get the ursolic acid crude purity of 85%. Further consideration Chadu the active ingredient in the incense, the establishment of comprehensive utilization of technology to improve the comprehensive utilization rate, and take full advantage of the rich plant resources to meet the current demand of the international community of natural medicine, has an extremely important significance.