Bushen Yijing extraction of particles
【Abstract】 Objective To optimize the extraction of Bushen Yijing particle preparation process. Methods icariin content as an indicator, by percolation experiments and orthogonal design to return the best extraction conditions for screening experiments. The best results of percolation process for extraction with 70% ethanol as solvent, soaking 48 h, to 1 ~ 3 ml / min speed slowly percolation. Orthogonal design experiments optimum reflow process as follows: using 8 times
the amount of 50% ethanol, extracting a sub-3 h. Conclusion
The optimized by orthogonal design experiments of Epimedium reflux reflux of the ethanol extraction conditions were stable and practical.
Key words Bushen Yijing particles icariin percolation France
orthogonal
Optimization of Extracting Process for Bushenyijing Granules by Orthogonal Test
Abstract: ObjectiveTo optimize the extracting process for Bushenyijing Granules. MethodsWith content of icariin as the
inspection indicators, percolation method and orthogonal test were designed for optimization of extracting process for Bushenyijing Granules. Orthogonal test was used to investigate the influence of four extracting factors (concentration of alcohol (A), alcohol volume (B), extracting time (C) and times of extracting (D)) on the extracting process.ResultsThe optimum percolation method was that the medicinal material was percolated at 1 to 3 ml / min after soaked for 48 hours in 70% alcohol. The optimum extracting process was A2D1C3B2, ie the
50% alcohol volume being 8 times of the weight of medicinal material, extraction for 1 times and 3 hours each
time.ConclusionOptimization of extracting process for Bushenyijing Granules by orthogonal test is a simple, quick
and accurate method.
Key words: Bushenyijing Granules; Icariin; Percolation method; Orthogonal test
Bushen Yijing granules side by epimedium, Osthol, Chinese angelica, Chuanxiong, fennel, Schisandra, psoralen, etc. composed of seven medicinal flavor, with kidney impotence,
promoting blood circulation to fill the effectiveness of precision and so on. In this study, we developed new drugs in accordance with the requirements of traditional Chinese medicine, Chinese medicine prescriptions in accordance with
the theory and analysis of prescription drugs each flavor the relationship between the dosage forms prepared in conjunction with the basis of need, respectively, using percolation method and orthogonal experimental design to return to icariin yield
as an indicator of kidney Yijing particle extraction process were optimized.
1 Equipment
1.1 Materials and reagents
Epimedium, Cnidium, Chinese angelica, Chuanxiong, fennel, Schisandra, psoralen and other medicinal herbs were purchased
from Zhejiang Huadong Medicine Co., Ltd. herbs ginseng and branch offices, and by Liu Hua, an associate research fellow identification. Icariin reference substance (Lot 0737-200111)
was purchased from Chinese medicine and biological products. The remaining reagents were analytical grade.
1.2 Instrument Agilent 1100 HPLC (Agilent Technologies Inc. USA), rotary evaporator (Re-52AA, Shanghai Yali-wing
biochemical Instrument Factory).
2 Methods and Results
2.1 Determination of icariin content
2.1.1 Chromatographic conditions icariin content using high performance liquid chromatography [1,2]. Column was Agilent ZORBAX Eclipse XDB-C18 chromatography (4.6 mm × 150
mm, 5 μm); mobile phase of acetonitrile - water (V / V =
30:70); detection wavelength was 270 nm; flow rate 1 ml / min. Icariin calculated according to peak number of theoretical plates should not be less than 1500.
2.1.2 Preparation of standard curve obtained precision that icariin reference substance, add methanol made from 40 μ
g per ml of the reference substance stock solution. When paired with different concentrations of the provisional reference substance liquid, precision drawing reference
substance solution of 10 μl, according to chromatographic
conditions set standard curve, results showed that 0.09 ~ 23 μg / ml concentration range, the absorption of icariin degree (Y) and concentration (X) showed good linear relationship, the
regression equation Y = 0.038 7 X 0.000 1 (r = 0.999 9). 5 times a day precision and between-day precisions were 1.74%
and 2.11%.
2.1.3 Preparation for the test product solution liquid extract derived from 2 ml, set in sub-funnel, extracted with
ethyl acetate four times, 10 ml / times, combined ethyl acetate layer. Evaporated, residue was dissolved in 10 ml of methanol, filtration, that is, too. Reposted elsewhere in the paper for free download http://
2.1.4 Sample test items for testing precision drawing solution of 10 μl, into the liquid chromatograph to measure. Substituting into the standard curve of peak area calculated for the test items in the content of icariin.
2.2 The percolation experiment design based on "The
People's Republic of China Pharmacopoeia" 2005 edition, which was recorded according to the Department ? fluidextract agent
with the extract under the percolation method [3]. To take medicines on prescription, said the proportion of 184.4 g, with 30%, 50%, 70% ethanol as solvent, soaking 48 h, to 1 ~ 3 ml / min speed of slow percolation, collecting percolation fluid. The total yield of icariin, as the indexes showed that three kinds of conditions, icariin were 46.57,58.46 and 64.32 mg. According to the experimental results suggest Bushen Yijing particle percolation process of extracting the best with 70% ethanol as solvent, soaking 48 h, to 1 ~ 3 ml / min speed slowly percolation.
2.3 The orthogonal experimental design reflux reflux extraction process, comprehensive consideration of various factors affecting extraction, using ethanol concentration (A), solvent dosage (B), extraction time (C) and extraction times (D) and other factors (see Table 1) to inspect, according to L9 (34) orthogonal design experiment [4,5] to yield, as the indexes of icariin on the optimization of extraction process of returning the best selection. The results in Table 2. Table 1 reflux orthogonal factor level (slightly) Table 2 reflux orthogonal (omitted)
Ethanol reflux icariin the experimental results and analysis of variance (Table 2) we can see that the impact of primary and secondary factors extracted icariin for A> D> C> B, ie alcohol concentration "extract the number of" extraction time "Solvent dosage. Optimum reflow process as: A2D1C3B2. 2.4 verification experiment under the optimum filter to be extracted five batches of samples, 184. 4 g Radix icariin content in average 103.16 mg. These results indicate that using the best extraction process extract Bushen Yijing
particles in a higher rate of extraction of icariin.
3 Discussion
The main active ingredient of Epimedium is icariin, flavonoids and other such ingredients soluble in water, methanol, ethanol and other solvents, it can use ethanol,
reflux, alkaline extraction, water extraction and alcohol precipitation method and other methods extraction, water extraction and alcohol precipitation concentrated for too long, the active ingredient wreck, and the invalid impurity more. Alkaline extraction method for extraction or
concentration process in the alkaline hydrolysis will occur, causing hydrolysis of glycosides to the active ingredients extracted reduced, while the concentration of ethanol shorter refluxing method, pH, moderate, less loss of glycosides. Thus,
according to the relevant information and pre-experiment, we
use percolation extraction method and ethanol reflux Epimedium active ingredients, and adopted the orthogonal design experiments, the main factors were studied, the optimized
extraction conditions. From the experimental results analysis shows that percolation extraction consume a large amount of alcohol, time-consuming, should choose ethanol reflux
extraction method, affecting primary and secondary factors
extracted icariin is A> D> C> B, ie alcohol concentration
"extraction times" extraction time "solvent usage. Optimum reflow process as: A2D1C3B2, verification experiment is further evidence that the process is stable, so selection on the best extraction conditions were: The 8-fold the amount of
50% ethanol, extracting a sub-3 h.
【References】
[1] Chen Po, Li Cai-rong, YANG Qing-sheng, et al. High-
performance liquid chromatography Yuanhuzhitong Tetrahydropalmatine content of the film [J]. Shizhen State Medical Sinopharm, 2006, 17 (9): 1701.
[2] Jiang Yong Nam, Yaocai Xia, Huang Bi fun. Epimedium Astragali Oral Liquid Process [J]. Guangdong Pharmaceutical, 2000, 10 (4): 27.
[3] National Pharmacopoeia Committee. Chinese Pharmacopoeia, ? Department of [S]. Beijing: Chemical
Industry Press, 2005:101.
[4] Zhang Xueqiong, Shi Zhao-hua, Xiong Fu-liang. Danshu
optimized by orthogonal test the extraction process [J]. Shizhen State Medical Sinopharm, 2006, 17 (4): 591.
[5] Cheng Kin-ming, well mountains. Dl in
tetrahydropalmatine comparative study of different extraction methods [J]. Shizhen State Medical Sinopharm, 2006, 17 (7): 1236. Reposted elsewhere in the paper for free download http://www . hi138.com