CN1164599C - Process for preparing total alkaloid of siberian fritillary bulb with antitussive and phlegm-eliminating action - Google Patents
Process for preparing total alkaloid of siberian fritillary bulb with antitussive and phlegm-eliminating action Download PDFInfo
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Abstract
The present invention relates to an optimum extraction process of an active constituent for researching the traditional action of cough relieving and phlegm eliminating of a siberian fritillary bulb as a medicinal material, which is characterized in that the siberian fritillary bulb as a medicinal material is taken, pulverized into coarse powder with the particle diameter of 0.5 to 1.0cm, and percolated with 30 to 50% of ethanol with the weight 16 to 18 times larger than that of the medicinal material at the flow speed of 5 to 10 ml/min; the percolated liquid is concentrated until the volume ratio of the concentrated liquid to the medicinal material is 1:1 to 3, the pH value is regulated to 2 to 5 with acid, and precipitates are centrifugally removed; an acid solution is extracted with chloroform or methylene dichloride after the pH value of the acid solution is regulated to 9 to 15 with alkali; an organic solvent is recovered, and extract is dried in vacuum to obtain total alkaloids of the siberian fritillary bulb.
Description
The invention belongs to the natural drug class, specifically a kind of preparation technology with her shellfish total alkaloids of Antitussive and Expectorant Effect.
Fritillaria pallidiflora Schrenk (Fritillaria pallidiflora Schrenk) belongs to Liliaceae Fritillaria (Fritillaria) plant, and its dry bulb is traditional simply relieving cough and reducing sputum Chinese medicine [1].The composition that contains in the chemical research proof medicinal material of Fritillaria pallidiflora Schrenk in recent years is different tetrahydroisoquinoline alkaloid, as Sipeimine (imperialine) and Sipeimine glycosides (imperialine-3 β-D-glucoside) etc., and think that Sipeimine is the contained main alkaloid [2-4] of her the pears bulb of fritillary.Document extracts the tetrahydroisoquinoline alkaloid use from Fritillaria pallidiflora Schrenk extraction solvent is that 70-95% ethanol directly extracts, after the neutral extract acidifying (generally using 1-3% hydrochloric acid adjust pH 3-4), use sherwood oil, the methylene dichloride degreasing, alkalization (ammoniacal liquor or sodium hydroxide) gets total alkaloids extract with chloroform extraction again, or behind the extract recovery organic solvent, macroporous resin column in the elder generation, behind the washing desaccharification, use the methanol-eluted fractions alkaloid of different concns again, acidifying more then, degreasing, the alkalization back gets total alkaloids extract [2-6] with chloroform extraction, or earlier bulb of fritillary medicinal material is alkalized again with tetrahydroisoquinoline alkaloid [7] in other bulb of fritillary of organic solvent extraction such as benzene.These extraction work all are in order to carry out the research of individualized compound, not see relevant Fritillaria pallidiflora Schrenk cough-relieving apophlegmatic activeconstituents preparation technology's bibliographical information and patent report so far.
The objective of the invention is to study the optimum extraction process of the active constituent of medicinal material of Fritillaria pallidiflora Schrenk tradition cough-suppressing phlegm-dispelling functions.
Purpose of the present invention can reach by following measure:
Get medicinal material of Fritillaria pallidiflora Schrenk, be ground into the 0.5-1.0cm meal, adopt medicinal material weight 16-18 30-50% ethanol percolation doubly, the volume ratio that flow velocity 5-10ml/min, percolate are concentrated into concentrated solution and medicinal material is 1: 1-3, with sour adjust pH to 2-5, centrifugal removal precipitation, acidic solution with adjusting PH with base value 9-15 after, with chloroform or dichloromethane extraction, reclaim organic solvent, vacuum-drying extract De Yibei total alkali.
Advantage of the present invention:
Used extraction solvent species of technology of the present invention and concentration, extracting method, medicinal material size etc. are to form through orthogonal Design Research, guaranteed that resulting Sinkiang Fritillary Bulb total alkaloids yield is the highest, and main active ingredient also has the Sipeimine glycosides except that the Sipeimine that document is thought, and the amount of Sipeimine glycosides is than Sipeimine height, and both content sums are greater than 50%.Its research step and detailed data are as follows:
1. medicinal material
Select the dry bulb of Liliaceae Fritillaria plant Fritillaria pallidiflora Schrenk Fritillaria pallidiflora Schrenk for use, the properties and characteristics of medicinal material, powder characteristics, physico-chemical property should meet the content under 2000 editions one one " Sinkiang Fritillary Bulb " items of Chinese Pharmacopoeia.
2. the extraction process technology condition of You Huaing
2.1 extraction solvent
Study the experience of the bulb of fritillary for a long time according to this seminar, solvent species is bigger to the extraction efficiency influence, and for the factor and the level of selective extraction process optimization, we have designed the primary election experiment of extracting solvent.Get the about 50g of medicinal powder of the about 0.5cm of particle diameter, the accurate title, decide, 95% ethanol=25: 8: 2.5), 50% acetone, methylene dichloride, 30% ethanol and 50% ethanol cold soaking spend the night (ether: chloroform:, wherein, mixed solvent and dichloromethane extract directly concentrate with mixed solvent respectively, other solvent extraction liquid is condensed into 50ml, through acidifying, alkalinisation treatment, with chloroform extraction 3 times, merge No. 3 times extracting solution again, measure total alkaloid content in the extract with nonaqueous titrations, the result is as shown in table 1.
Table 1 different solvents is to the influence of total alkaloids extraction efficiency
Heavy (g) total alkali yield of solvent samples (%) carry the total alkaloids amount
(mg/50g)
50.08 0.12
Mixed solvent 50.02 0.13 0.12 ± 0.0011 62.07
50.09 0.12
50.01 0.17
50% acetone 50.04 0.16 0.16 ± 0.0025 81.53
50.02 0.16
50.00 0.09
Methylene dichloride 50.07 0.08 0.09 ± 0.0046 42.54
50.07 0.09
50.03 0.15
50% ethanol 50.03 0.15 0.15 ± 0.0015 75.03
50.00 0.15
50.00 0.18
30% ethanol 50.08 0.18 0.18 ± 0.0017 88.57
50.05 0.18
Above result shows that the dichloromethane extraction effect is the poorest, and mixed solvent takes second place.50% acetone, 30% ethanol and 50% extraction using alcohol effect are better.Though 30% extraction using alcohol effect is best in several solvents, 50% acetone extraction effect slightly is better than 50% ethanol, considers the cost of suitability for industrialized production, intends selecting ethanol as extracting solvent, carries out extraction process optimization.
2.2 the cold soaking extraction process of optimizing
In order to determine the influence to extraction efficiency of medicinal material particle diameter, alcohol concn, consumption and extraction time, we are index with orthonormal design of experiments with the total alkaloid contents, and extraction process is optimized.Experimental design is shown in table 2 and table 3.Pulverizing medicinal materials is become three grain size categories,, test by requirement in the orthogonal test table.Extract with cold-maceration, after extracting solution concentrated, through acidifying, alkalinisation treatment, chloroform extraction was measured total alkaloid content in the extract by nonaqueous titrations, the results are shown in Table shown in 3.
Table 2 level of factor table
Factor medicinal material particle diameter (A) solvent strength (B) solvent load (C) extraction time (D)
Level
50% 6 times of the about 0.5cm of 1 particle diameter 1 time (24 hours)
70% 8 times in 2 20 orders 2 times
95% 10 times in 3 40 orders 3 times
Do not consider interaction, choose L
9(3
4) the orthogonal table experiment.
Table 3 extraction process orthogonal table
| Factor experiment number | A (medicinal material particle diameter) | B (alcohol concn) | C (solvent is used) | D (extracting inferior) | Total alkaloids amount (mg/50g) | Medicinal extract amount (mg/50g) | Yield of extract (%) |
| 1 2 3 4 5 6 7 8 9 | 1 1 1 2 2 2 3 3 3 | 1 2 3 1 2 3 1 2 3 | 1 2 3 2 3 1 1 3 2 | 1 2 3 3 1 2 2 3 1 | 76.71 75.33 49.71 100.61 69.84 23.09 95.82 77.75 20.73 | 100.6 96.7 72.0 166.0 99.2 63.5 169.5 108.9 5.7 | 0.20 0.19 0.14 0.33 0.20 0.13 0.34 0.23 0.19 |
K1 201.75 273.14 195.62 167.28
K2 193.54 222.92 196.67 194.24
K3 194.3 93.53 197.30 228.07
K1 67.25 91.05 65.21 55.76
K2 64.51 74.31 65.56 64.75
K3 64.77 31.18 65.77 76.03
R 2.74 59.87 0.56 20.27
In A factor three levels, K1＞K3＞K2, so when factor A gets A1, extract total alkaloid content height;
In B factor three levels, K1＞K2＞K3, so when factor B gets B1, extract total alkaloid content height;
In C factor three levels, K3＞K2＞K1, so when factor C gets C3, extract total alkaloid content height;
In D factor three levels, K3＞K2＞K1, so when factor D gets D3, extract total alkaloid content height;
So, do not consider that the optimised process of secondary factors is: A1, B1, C3, D3, promptly the medicinal material particle diameter is the 0.5cm size, 50% ethanol, 10 times of amount solvents extract 3 times.Yet from extract total alkaloids amount extreme difference as can be known, factor is followed successively by to inferior order from main: B＞D＞A＞C, and factor B (solvent strength) is a principal element, and factor C (solvent load) and factor A (medicinal material particle diameter) influence is little, is secondary cause.Because solvent load is a secondary cause, 6 times of amount solvent total alkaloidss on average must be measured and be 65.21mg, and 8 times of amount solvent total alkaloidss on average must be measured and be 65.56mg, and 10 times of amount solvent total alkaloidss on average must be measured and be 65.77mg, so actual optimal conditions can be: A1, B1, C1, D3 or A1, B1, C2, D3.Because these two conditions did not occur in done 9 times experiments, we have designed two experiments again and have been verified for this reason, see Table 4.
The checking of table 4 orthogonal experiment optimal conditions
The heavy total alkaloids of test conditions sample must be measured the heavy yield of extract of medicinal extract
(mg/50g) (mg/50g) (％)
A1B1C1D3 50.02 124.08 159.20
50.00 126.42 124.92±1.33 160.74 161.17±2.40 0.32
50.06 124.28 163.65
A1B1C2D3 50.05 128.36 171.39
50.03 131.08 129.00±1.84 174.98 172.28±1.93 0.34
50.01 127.58 171.95
According to above result, the optimised process that the Sinkiang Fritillary Bulb total alkaloids extracts is A1, B1, and C1, D3, promptly the medicinal material particle diameter is the 0.5cm size, 50% ethanol, 6 times of amount solvents extract 3 times.
2.3 extracting mode is to the influence of extraction efficiency
Get the about 20g of the medicinal powder that is ground into 0.5cm respectively, the accurate title, decide, and extracts by following method with 6 times of amount 59% ethanol:
Cold soaking: 6 times of amount solvent cold soaks spend the night, and extract 3 times.
Diacolation: 18 times of amount solvent diacolations.
Thermal backflow: 6 times of amount solvent thermal reflux, and extract 3 times.
Merge various extracting solutions respectively, measure total alkaloids amount in the extract, result such as table 5 respectively by nonaqueous titrations.
Table 5 extracting mode is to the influence of extraction efficiency
| Sample heavy (g) | Extracting mode | Total alkaloid content (%) | Total alkaloids must be measured (mg/20g) | Medicinal extract amount (mg/20g) | Yield (%) | ||
| 20.00 20.01 20.15 20.00 20.10 20.03 20.09 20.08 20.00 | The thermal backflow of cold soaking diacolation | 0.201 0.191 0.195 0.210 0.203 0.201 0.237 0.250 0.239 | 0.196±0.005 0.205±0.005 0.242±0.007 | 39.20 41.00 48.40 | 60.20 55.56 65.20 67.50 62.20 60.60 63.90 58.10 64.30 | 60.30±4.85 63.4±3.60 62.10±3.47 | 0.30 0.32 0.31 |
Above result as seen, the extraction efficiency that heat is carried is the highest, diacolation takes second place, cold soaking is relatively poor, but three's difference is not remarkable.Consider from the suitability for industrialized production angle, hot extraction cost height, cold-maceration is operated than the percolation complexity, so the first-elected percolation of suitability for industrialized production.
To sum up study as seen, it is as follows that the alkaloidal technology of Sinkiang Fritillary Bulb is extracted in industrialization: pulverizing medicinal materials is to 0.5cm, with 50% ethanol percolation of 18 times of amounts.
2.4 the separation of Sinkiang Fritillary Bulb total alkali, purifying, concentrated and drying process
2.4.1 isolation and purification technology
This seminar studies show that, the oil-soluble impurities that degreasing is removed after the acidifying of Fritillaria pallidiflora Schrenk bulb seldom, thereby the isolation and purification technical study is as follows: percolate thin film evaporation or rotary evaporation to volume and medicinal material weight ratio is 1: 1-3.Percolate after concentrating with the salt acid for adjusting pH value to 2-5, centrifugal, remove precipitation, aqueous acid is regulated the pH value to 8-13 with alkali, chloroform extraction 4 times, each 1/2 volume (medicinal material weight 1/2), combining extraction liquid is washed to neutrality, anhydrous Na
2SO
4Dehydration.
2.4.2 concentrate and drying process
Through anhydrous Na
2SO
4The extraction liquid of dehydration leaves standstill, filters, and decompression and solvent recovery, vacuum-drying, promptly.
3. the cough-relieving apophlegmatic activity of Sinkiang Fritillary Bulb total alkaloids
3.1 drawing, ammoniacal liquor coughs the test of method antibechic
3.1.1 test materials
3.1.1.1 be subjected to the reagent thing: her shellfish total alkali, total alkali 72.6%, lot number 990826
3.1.1.2 positive control drug: codeine phosphate
3.1.1.3 negative control medicine: 0.5%CMC-Na solution
3.1.1.4 instrument and reagent water bath, large beaker, syringe, bell glass, children's's stethoscope, strong aqua
3.1.1.5 animal subject Kunming kind small white mouse
3.1.2 method and result
3.1.2.1 operation steps
3.1.2.1.1 dosage: press table 6 dosed administration
Table 6 antibechic test mice dosage
Drug dose (mg/kg)
Her shellfish total alkali 40
Codeine phosphate 25
3.1.2.1.2 medicine preparation
Solvent:, prepare the respective concentration soup as solvent with 0.5%CMC-Na according to dosage and administration volume 0.2ml/10g mouse.
Compound method: be subjected to reagent to place mortar, add an amount of solvent and grind to form suspension, redilution becomes the desired concn soup.Positive drug directly is made into the desired concn soup with a certain amount of solvent.
3.1.2.1.3 testing sequence
Get 176 of mouse and be divided into 11 groups at random, 16 every group, male and female half and half, number consecutively is weighed, and gastric infusion is 5 days continuously, and 1h, 2h, 3h, 4h after the last administration adopt sequential method to measure EDT to each group mouse respectively
50(half mouse spraying cause the time of coughing), and calculate the R value, R＞130% has been judged to antitussive effect, and R＞150% item has obvious antitussive effect.
3.1.2.2 result
She draws the antitussive effect of coughing (n=16) by the shellfish total alkali table 7 to mouse ammoniacal liquor
Group dosage 1h 2h 3h 4h
mg·kg
-1 EDT
50 R(％) EDT
50 R(％) EDT
50 R(％) EDT
50 R(％)
Negative control 8.4 7.8 5.5 6.0
Her shellfish total alkali 40 23.7 282.1 15.8 202.6 15.0 230.8 12.6 210.0
Positive control 25 11.5 136.9 22.1 283.3 12.1 186.2 13.0 216.7
3.2 phenol red excretion method expectorant test
3.2.1 test materials
3.2.1.1 be subjected to the reagent thing: the same
3.2.1.2 positive control drug: methyl catechol
3.2.1.3 negative control medicine: 0.5%CMC-Na solution
3.2.1.4 medicine and instrument: phenol red, NaHCO
3.NaOH, physiological saline, 752 spectrophotometers, operating scissors, ophthalmology tweezer, small test tube
3.2.1.5 animal subject: Kunming kind small white mouse
3.2.2 method and result
3.2.2.1 method
3.2.2.1.1 drawing standard curve
0.25% phenol red preparation: 2.5g is phenol red with 2.5ml 1mol/lNaOH dissolving, adds physiological saline again to 100ml, shakes up promptly.Accurately draw 0.25% phenol red 20ml with suction pipe, add 0.5%NaHCO
3Get the 1mg/ml phenol red solution to 50ml, be diluted to 10,8,6,4,3,2,1.5,1,0.5,0.25 μ g/ml series solution afterwards successively.Measure absorbancy respectively at λ=558nm place.
Getting regression equation through match is: A=0.1331C-1.9778, r=0.9997
3.2.2.1.2 soup preparation
The concentration of positive drug methyl catechol is 0.75mg/ml, and all the other soup compound methods are the same.
3.2.2.1.3 testing sequence
Get 176 of mouse, be divided into 11 groups at random, 16 every group, male and female half and half, each organizes the mouse numbering of weighing successively, and gastric infusion is 5 days continuously, and give ip in mice 5% phenol red solution 0.25ml half an hour after the last administration, after half an hour mouse taken off cervical vertebra and put to death.Cut off skin of neck, separate tracheae, thyroid cartilage is cut down to tracheae crotch tracheae section.Stringer is cut off and is soaked in 2ml 5%HCO again
3In the solution, measure absorbancy in 752 spectrophotometer 558nm places behind the shake well, write down the A value.And the substitution regression equation is asked for corresponding C value.
3.2.2.2 result
Her shellfish total alkali of table 8 to the influence of the phenol red excretion amount of mouse (x ± SD, n=14)
Group dosage mgkg
-1Phenol red excretion amount (the μ gml of A value
-1)
Negative control 0.167 ± 0.049 16.127 ± 0.368
Her shellfish total alkali 40 0.180 ± 0.089 16.222 ± 0.672
Methyl catechol 150 0.220 ± 0.062
*16.527 ± 0.465
*
Annotate: compare with negative control group,
*P＜0.05
Embodiment 1
Medicinal material of Fritillaria pallidiflora Schrenk 100kg is ground into the 0.5cm particle, with 18 times of amount 50% ethanol percolations, flow velocity 5ml/min.The volume ratio that percolate is concentrated into concentrated solution and medicinal material is 1: 1, with hydrochloric acid soln adjust pH to 2, and centrifugal removal precipitation, acidic solution is used dichloromethane extraction after using sodium hydroxide solution adjust pH 9, is washed to neutrality, anhydrous Na
2SO
4Dehydration is reclaimed methylene dichloride, vacuum-drying extract De Yibei total alkali 0.43kg.
Embodiment 2
Medicinal material of Fritillaria pallidiflora Schrenk 200kg is ground into the 0.5cm particle, with 16 times of amount 30% ethanol percolations, flow velocity 7ml/min.The volume ratio that percolate is concentrated into concentrated solution and medicinal material is 1: 2, with hydrochloric acid soln adjust pH to 3, and centrifugal removal precipitation, acidic solution is used chloroform extraction after using sodium hydroxide solution adjust pH 10, is washed to neutrality, anhydrous Na
2SO
4Dehydration is reclaimed chloroform, vacuum-drying extract De Yibei total alkali 0.8kg.
Embodiment 3
Medicinal material of Fritillaria pallidiflora Schrenk 400kg is ground into the 0.5cm particle, with 17 times of amount 40% ethanol percolations, flow velocity 10ml/min.The volume ratio that percolate is concentrated into concentrated solution and medicinal material is 1: 3, with hydrochloric acid soln adjust pH to 4, and centrifugal removal precipitation, acidic solution is used chloroform extraction after using sodium hydroxide solution adjust pH 12, is washed to neutrality, anhydrous Na
2SO
4Dehydration is reclaimed chloroform, vacuum-drying extract De Yibei total alkali 1.64kg.The quality of three batches of Sinkiang Fritillary Bulb total alkalis sees Table 9.
The mass parameter of table 9 Sinkiang Fritillary Bulb total alkali
Sinkiang Fritillary Bulb total alkali lot number assay (%)
Total alkaloids Sipeimine glucoside Sipeimine
990716 71.8 29.7 20.4
990718 72.5 30.2 20.3
990826 72.6 33.1 23.6
Reference
1. the Pharmacopoeia of People's Republic of China council. Pharmacopoeia of People's Republic of China (an one, 2000 editions),
2. Xu Dong inscription, Huang Enxi, Wang Shuqin hears twilight, Wu Xiuying. the alkaloidal research of Sinkiang Fritillary Bulb. Botany Gazette 1990; 32 (10): 789-793
3. Xu Dong inscription, in original weight doubly, village's liter, Yang Xiuwei, Huang Enxi, Li Chaosheng.Separation and the evaluation of she shellfish alkali glucoside A.Acta Pharmaceutica Sinica 1990; 25 (10): 795-797
4. yellow grace happiness, Li Chaosheng, Xu Dongming.The research of Sinkiang Fritillary Bulb alkaloid component.CHINA JOURNAL OF CHINESE MATERIA MEDICA 1990; 15 (9): 39-40
5. Xu Ya is beautiful, Xu Dongming, Huang Enxi, Wu Xiuying, Jin Xiangqun, Cui Dongbin, Liu Shiyue.Separation of Sinkiang Fritillary Bulb and evaluation.Acta Pharmaceutica Sinica 1992; 27 (2): 121-124
6. Xu Ya is beautiful, Xu Dongming, Cui Dongbin, Gao Jishan, Huang Enxi, Liu Shiyue, Yu Dequan.The separation of she shellfish alkali glucoside C and structure are identified in the Sinkiang Fritillary Bulb.Acta Pharmaceutica Sinica 1994; 29 (3); 200-203
7. the retinue becomes great, Shang Erning, Lin Wenhan, Cai Mengshen.Ningxia bulb of fritillary The Chemical Constituents.Acta Pharmaceutica Sinica 1993; 28 (7): 516-521
Claims (1)
1, a kind of preparation technology with her shellfish total alkaloids of Antitussive and Expectorant Effect, it is characterized in that: get medicinal material of Fritillaria pallidiflora Schrenk, be ground into the 0.5-1.0cm meal, adopt medicinal material weight 16-18 30-50% ethanol percolation doubly, flow velocity 5-10ml/min, the volume ratio that percolate is concentrated into concentrated solution and medicinal material is 1: 1-3, with sour adjust pH to 2-5, centrifugal removal precipitation, acidic solution with adjusting PH with base value 9-15 after, with chloroform or dichloromethane extraction, reclaim organic solvent, vacuum-drying extract De Yibei total alkali.
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1796402B (en) * | 2004-12-30 | 2010-06-30 | 华中科技大学 | Technique for preparing general alkaloid of Hubei fritillary bulb |
| CN100336821C (en) * | 2005-11-09 | 2007-09-12 | 天津大学 | Method for extracting simultaneously general alkaloid and starch from fritillary |
| CN102210803B (en) * | 2011-05-18 | 2012-09-19 | 北京中医药大学 | Extraction and enrichment method of fritillaria total alkaloids |
| CN102283851B (en) * | 2011-07-08 | 2016-08-31 | 四川大学 | Imperialine-BETA-N-oxide and the new application of isoverticine-BETA-N-oxide |
| CN102908381B (en) * | 2011-08-04 | 2015-12-09 | 北京中医药大学 | A kind of fresh Rhizoma Bolbostematis extract and preparation method thereof |
| CN102631536B (en) * | 2012-05-14 | 2014-03-12 | 天津药业集团新郑股份有限公司 | Extraction process of alkaloid in thunberg fritillary bulb |
| CN103251790A (en) * | 2013-05-06 | 2013-08-21 | 乌鲁木齐欧易生物医学科技有限公司 | Method for extracting total alkaloids from fritillaria pallidiflora |
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