Study On The Process Of Distillation Coupling Solvent Extraction Extract Volatile Oil Of Ligusticum Chuanxiong Hort And Quality Evaluate

Chuanxiong is the dried rhizome of Ligusticum chuanxiong Hort for umbelliferae, promoting blood and Qi circulation ang relieving pain ang Feng, modern is mainly used for the treatment of cardiovascular and cerebrovascular diseases, for the treatment of headache and irregular menstruation application are also very much. The volatile oil is one of the main active parts of Ligusticum chuanxiong Hort, can improve microcirculation, lower blood pressure, increase cerebral blood flow, regulate cardiovascular function, anti coagulation. The extraction process of volatile oil of Ligusticum chuanxiong Hort is mainly distillation method, this method is simple, safe, less environmental pollution, is suitable for industrialized production. But the proportion of volatile oil is close to 1, it is difficult to gather, resulting in distillation to extract the volatile oil extraction rate is relatively low, only about 0.4%. In order to solve the problem of this industry, we carried out the research.Objective:1 Reseach distillation coupling solvent extraction for extracting volatile oil from Ligusticum chuanxiong Hort.4 Completed the quality evaluation of distillation coupling solvent extraction for extracting volatile oil from Ligusticum chuanxiong Hort.Methods:1 Establish the determination of content of ligusticum in volatile oil of Ligusticum chuanxiong Hort by gas chromatography(GC).Carry on methodological study of ligustilide, including linear range, precision experiment, repeated experiment, stability experiment, recovery experiment.Establish the determination of content of total lactone in volatile oil of Ligusticum chuanxiong Hort by ultraviolet spectrophotometry(UV). Carry on methodological study of total lactone including linear range, precision experiment, stability experiment, recovery experiment.2 The single factor investigation: Study on effect of the soaking time, extraction time, the effect of water multiple and boiling degree(the unit of time return rate) the extraction rate of volatile oil from Ligusticum chuanxiong Hort, determine the main factors and level; Orthogonal test: with Chuanxiong volatile oil extraction rate as index,carrying on three factors and three levels orthogonal experiment, using the analysis of variance statistics for the results of orthogonal experiments, determination of the distillation extraction process of volatile oil of Ligusticum chuanxiong Hort, and process validation.3 The research of distillation coupling solvent extraction extract the volatile oil of Ligusticum chuanxiong Hort. The method is in the based on distillation extraction of volatile oil from Ligusticum chuanxiong Hort, adding a certain amount of extractant in the volatile oil extractor, realizing volatile oil enrichment and oil-water separation; Through two times of extraction, salting preparation of volatile oil of Ligusticum chuanxiong Hort.In the volatile oil volume, ligustilide and total lactone precent increase in content as the index, optimize liquid paraffin, vaseline and corn oil three extraction agent. With the recovery rate of ligustilide as the index, optimize the separation process of Ligusticum chuanxiong Hort volatile oil extraction, the effects of ethanol extraction times, the mass fraction of water solution and the amount of Na Cl.To verify this extraction process of distillation extraction coupling extraction of volatile oil of Ligusticum chuanxiong Hort.In the extraction rate of volatile oil、total lactones and ligustilide as index, comparison of two methods for volatile oil extraction effect.4 Establish Ligusticum chuanxiong Hort volatile oil fingerprints by use of GC temperature program. The use of “traditional Chinese medicine fingerprint Computer Aided Similarity Evaluation Software” evaluating the process of traditional steam distillation and distillation coupling solvent extraction of volatile oil of Ligusticum chuanxiong Hort stability and two methods of extracting volatile oil quality consistency of the proposed.Results:1 Established the determination of ligustilide content in gas chromatography. Methodological study results: The standard curve equation is: Y=1789.8X+4.6914, r=0.9999(n=6), linear range: 0.121 ~ 1.01mg/m L;precision of RSD =1.43%; stability of RSD =1.47%; repeatability of RSD =1.74%; the average recovery was 99.33%, RSD=2.8%.Established the determination of total lactone content in ultraviolet spectrophotometry. Methodological study results: The standard curve equation is: Y=70.903X+0.0073,r=0.9999(n=6),linear range: 0.001~0.010mg/m L;precision of RSD =0.14%; stability of RSD =0.82%; the average recovery was 102.37%,RSD=1.53%.2 The single factor experiment results: determined the factors and levels of orthogonal test for the extraction time(4h, 6h, 8h), soaking time(0h, 2h, 4h), the unit time return rate(4.95±0.45、6.65±0.45、8.35±0.45). The results of orthogonal experiments: 6h extraction, do not soak, the unit time return rate(8.35±0.45). Determined the optimum extraction process of distillation in the extraction of volatile oil of Ligusticum chuanxiong Hort: Take Ligusticum chuanxiong Hort coarse powder 200 g in the round bottom flask containing 3000 m L, plus 6 times the amount of water, according to the unit time return rate of 8.35±0.45 distillation extraction 6h. Three stability tests of the volatile oil of Ligusticum chuanxiong Hort average value is 0.72%, RSD<5%.3 The optimal extraction agent is liquid paraffin 1.5m L; volatile oil purification process: ethanol extraction for 6 times, the first dosage of 1m L, other each time the amount of 0.5m L; the mass fraction of Na Cl in aqueous solution was 20%, the amount is 1.5 times of volatile oil in ethanol solution. Determined the optimum extraction process of distillation coupling solvent extraction in the extraction of volatile oil of Ligusticum chuanxiong Hort: Take Ligusticum chuanxiong Hort coarse powder 200 g in the round bottom flask containing 3000 m L, plus 6 times the amount of water, shake, volatile oil extractor plus 1.5m L liquid paraffin, according to the unit time return rate of 8.35±0.45, distillation extraction 6h, the separation of essential oil and liquid paraffin solution, according to the volatile oil purification method of preparation of essential oil of Ligusticum chuanxiong hort. Three batches of process validation of Rhizoma Chuanxiong volatile oil extraction rate of the average value is 1.07%, RSD<5%; the extraction rate of total lactones of the average value is 0.50%, RSD<5%; the extraction rate of ligustilide of average value is 0.47%, RSD<5%.4 Establish the GC fingerprint of volatile oil of Ligusticum chuanxiong Hort. Fingerprint conditions : AT-5 fused silica capillary column(30m×0.32 mm × 0.25μm); FID detector; carrier gas : N2; inlet and detector temperature: 250℃;the use of fourth-order temperature program: initial temperature of 90℃, in order to 1.5℃/min temperature programmed to 100℃; 15 ℃ /min temperature programmed to 159 ℃, holding 1min; 0.5 ℃ /min temperature programmed to 165℃, holding 1 min; 30℃/min temperature programmed to 250℃, holding 3 min. Both the proposed extraction method volatile oil fingerprint similarity are above 0.998, indicating that the two extraction method is stable and repeatable. The volatile oil of Ligusticum chuanxiong Hort extracted by distillation coupling solvent extraction with traditional steam distillation fingerprint identified 19 common peaks, accounting for the traditional steam distillation method proposed Ligusticum chuanxiong Hort volatile oil of 98%, accounting for distillation coupling solvent extraction method proposed Ligusticum chuanxiong Hort volatile oil 99%. The common pattern of fingerprint of volatile oil of Ligusticum chuanxiong Hort extracted by two methods conduct similarity evaluation, the similarity is 0.998.Conclution:Distillation coupling solvent extraction to extract volatile oil of Ligusticum chuanxiong Hort, the volatile oil extraction rate, ligustilide extraction rate, total lactone extraction rate compared to the existing distillation to extract the volatile oil were greatly improved, the process and the product quality is stable. Two extraction methods of Ligusticum chuanxiong Hort fingerprint of volatile oil of high similarity between the proposed. The composition is basically the same. Can think of distillation coupling solvent extraction of volatile oil of Ligusticum chuanxiong Hort is superior to the existing distillation process.