CN102397308B - Preparation process of hypnagogic active component of fructus cnidii - Google Patents
Preparation process of hypnagogic active component of fructus cnidii Download PDFInfo
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Abstract
The invention relates to the technical field of traditional Chinese medicine extraction and particularly relates to a preparation process of a hypnagogic active component of fructus cnidii. Through the preparation process, the problems of low efficiency of extracting the hypnagogic active component from the fructus cnidii, low yield of the hypnagogic active component and the like are solved. The preparation process of the hypnagogic active component of the fructus cnidii comprises the following steps of: extracting a crude extract from crude powder of the fructus cnidii by using a solvent through a heating reflux method; concentrating the crude extract to obtain an extractum; and performing further macroporous adsorption resin column chromatography separation on the extractum to obtain the effective extractive composition. The medicament effect is clear, the toxicity is low, and the process is simple and feasible, so the hypnagogic active component is suitable for mass industrial production and economic benefit can be improved. The preparation process has the advantages of low requirement on equipment conditions, feasible implementation, simple steps and low production cost.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of preparation technology of Fructus Cnidii hypnotic activity component.
Background technology
Fructus Cnidii (Fructus cnidii) is samphire cnidium monnieri
cnidium monnieri(L.) dry mature fruit of Cuss..Chinese medicine thinks that Fructus Cnidii is pungent, bitter, warm in nature, slightly poisonous, returns kidney channel, has warming the kidney to invigorate YANG, dampness, dispel the wind, parasite killing.For sexual impotence, cold womb, cold-damp leukorrhagia, arthralgia chiefly caused by damp pathogen lumbago; External treatment vulval eczema, married woman's pudendal pruritus, trichomonal vaginitis." medical and health " in February, 2010, disclose under Fructus Cnidii ul-trasonic irradiation in " screening of Fructus Cnidii tranquilizing soporific extraction process of effective component " literary composition, utilize the extractions such as petroleum ether, ethyl acetate, n-butyl alcohol, ethanol, water, the different extract of hypnotic effect can be obtained by different Extraction medium.Research shows, in Fructus Cnidii, the coumarinoids osthole (osthol) of extraction and isolation has certain inhibitory action to nervus centralis, 50% ~ 95% alcohol heating reflux extract has sedative-hypnotic effect, but to its be applicable to the preparation technology of industrialized great production, the safety of drug effect and and drug effect may closely-related finger printing not yet further investigate at present.
At present conventional Western medicine class tranquilizing soporific chemical medicine life-time service easily produces tolerance, and therapeutic index is low, dependency and withdrawal symptom is serious and the daytime is still drank after a night, rebound insomnia, dysmnesia, infringement etc. to cognitive and Psychomotor ability.Conventional Traditional Chinese medicine for tranquilization has Semen Ziziphi Spinosae, Cortex Albiziae, Caulis Polygoni Multiflori, Radix Polygalae, Semen Platycladi etc., and these kinds can be counted on one's fingers, and due to the restriction of resource, the increase of consumption, cause the Traditional Chinese medicine for tranquilization price of determined curative effect year after year high.
Fructus Cnidii is widely distributed, the equal suitable planting of China's most area, have cold-resistant drought-enduring, require not tight to soil, growth is fast, the feature that output is high, cheap, utilize Fructus Cnidii aboundresources, cheap advantage, so in order to increase Fructus Cnidii hypnosis effect, improve its medical value, expand the selection of clinical insomnia's medication, therefore, employing can be adapted to the simple and easy to do preparation technology of large production, extract from Fructus Cnidii and there is syngignoscism active component safely and effectively, contribute to develop and useining Fructus cnidii resource, for preparation hypnosis natural drug lays the foundation, promote Chinese Medicine Industry, significant for development Chinese traditional medicinal economy.
Summary of the invention
The present invention is low from Fructus Cnidii extraction hypnosis active component efficiency at present in order to solve, and the problems such as output is few, provide a kind of from Fructus Cnidii, extract the preparation method with the active component of hypnotic activity.
The present invention is realized by following technical scheme, a kind of preparation technology of Fructus Cnidii hypnotic activity component, utilize solvent to extract crude extract by heating reflux method from Fructus Cnidii coarse powder, concentrate and obtain extractum, further macroporous adsorbent resin column chromatography separation is carried out to extractum, obtains effective extraction components.
Concrete steps are as follows:
Step one: get Fructus Cnidii coarse powder, adds the ethanol of 95%, heating and refluxing extraction 1-5 time, each 1-2h, merging filtrate, decompression recycling ethanol, concentrates to obtain extractum,
Step 2: get macroporous adsorbent resin, soaked overnight, wet method dress post, by distilled water flushing chromatographic column to without alcohol taste, dissolves rear loading by above-mentioned extractum 95% ethanol,
Step 3: carry out eluting with 40%-95% ethanol, preferred 50-60%, not etc., eluent concentrating under reduced pressure, recycling design is not to small size, and merge fraction, reconcentration, cold drying obtains Fructus Cnidii tranquilizing soporific active component for each eluting 4 ~ 8 times of column volumes.
Carrying out hypnosis experiment by extracting the component obtained above, proving that there is certain syngignoscism at Fructus Cnidii 40% ~ 95% ethanol column chromatography position, having certain inhibitory action to central nervous system.Application Bliss method calculates LD
50be 10.32 g/kg, 95% credibility interval is 8.33 ~ 12.79 g/kg.Its hypnosis effective dose is 0.0625g/kg, illustrates that safety is larger.
Feature of the present invention is:
1. reported first of the present invention Fructus Cnidii syngignoscism ethanol column chromatography preparation technology is develop Fructus cnidii resource developing frontier.
2. disclose a kind of preparation technology of Fructus Cnidii hypnotic activity component, drug effect is clear and definite and toxicity is little, simple for process, is applicable to large-scale industrial and produces, can increase economic efficiency.The present invention requires low, easy to implement to appointed condition, and step is succinct, and production cost is low.
Accompanying drawing explanation
Fig. 1 is the standard diagram HPLC of Fructus cnidii extract
Fig. 2 is the Fructus cnidii extract collection of illustrative plates utilizing water elution to obtain
Fig. 3 is the Fructus cnidii extract collection of illustrative plates utilizing 30% ethanol elution to obtain
Fig. 4 is the Fructus cnidii extract collection of illustrative plates utilizing 40% ethanol elution to obtain
Fig. 5 is the Fructus cnidii extract collection of illustrative plates utilizing 50% ethanol elution to obtain
Fig. 6 is the Fructus cnidii extract collection of illustrative plates utilizing 60% ethanol elution to obtain
Fig. 7 is the Fructus cnidii extract collection of illustrative plates utilizing 70% ethanol elution to obtain
Fig. 8 is the Fructus cnidii extract collection of illustrative plates utilizing 80% ethanol elution to obtain
Fig. 9 is the Fructus cnidii extract collection of illustrative plates utilizing 95% ethanol elution to obtain.
Figure 10 is tester collection of illustrative plates.
Detailed description of the invention
1 instrument and reagent
Aglient1200 high performance liquid chromatograph, vacuum degassing machine, (G1322A) quaternary pump (G1311A), automatic sampler (G1329A), column oven (G1316A), diode array detector (G1315D), HP Chemstation chromatographic work station; : Agilent company limited of the U.S.;
Sartorious 100,000/analytical balance: Sartorius AG;
D101 macroporous adsorbent resin: Tianjin sea light Chemical Co., Ltd. lot number 030510(1-3);
Fructus cnidii: be purchased from institute of traditional Chinese medicine of Shanxi Province, likes professor of pharmacy's qualification through Specimen Room height sky, institute for drug control, Shanxi Province;
Osthole (lot number 0822-9802), imperatorin (lot number 11826-200308): be all purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
2 experimental techniques and result
The preparation of the different extract of 2.1 Fructus Cnidii column chromatographies
Get Fructus Cnidii coarse powder 300g, add the ethanol of 4 times amount 95%, heating and refluxing extraction 3 times, each 1.5h, merging filtrate, decompression recycling ethanol, concentrated, cold drying, obtains the heavy 22.752g of cream.
Take 500gD101 macroporous adsorbent resin, 95% soak with ethanol is spent the night, wet method dress post, by distilled water flushing chromatographic column extremely without alcohol taste, loading after above-mentioned 22.752g extractum is dissolved with 95% ethanol, add filter paper, bead lid sample, use water successively, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol carries out eluting, each eluting 4 ~ 8 times of column volumes are not etc., according to the wash water color depth, judge whether to change eluting solvent composition, eluent decompression and solvent recovery is to small size, merge stream part, be total to obtain 8 components, each flow point solvent under reduced pressure is reclaimed, concentrated, cold drying obtains each active component of Fructus Cnidii tranquilizing soporific.
2.2 set up Fructus Cnidii column chromatography different component finger printing
2.2.1 chromatographic condition and system suitability:
With Elite SinoChrom ODS-BP 5 μm, (4.6mm × 250mm) chromatographic column, with acetonitrile-0.1% aqueous acetic acid gradient elution, elution program is: 0 ~ l5min, and acetonitrile is increased to 45% by 23%, and 15 ~ 30min acetonitrile is increased to l00% by 45%, 30 ~ 40min, acetonitrile is l00%; Determined wavelength: 245nm (0 ~ 26 min), 322nm (26 ~ 30 min), 245nm (30 ~ 40 min); Column temperature: 40 DEG C.
2.2.2 the preparation of reference substance solution
Precision takes osthole and imperatorin is appropriate, adds methanol and makes every 1ml respectively containing the mixed solution of 50 μ g and 45 μ g, product solution in contrast.
2.2.3 the preparation of need testing solution
Get each extract of Fructus Cnidii appropriate (being equivalent to 1g crude drug), put in 10ml measuring bottle, add 70% ethanol to scale, shake up, filter, as need testing solution.
2.2.4 the preparation of control medicinal material solution
Get Fructus Cnidii control medicinal material appropriate, put in 25ml measuring bottle, add ethanol 15ml, supersound extraction 30 minutes, lets cool and adds ethanol to scale, shake up, and filters, medical material Solutions Solution in contrast.
2.2.5 algoscopy
Draw Fructus Cnidii control medicinal material solution 20 μ L, inject high performance liquid chromatograph.Measure 3 batches of Fructus cnidii samples under these conditions, the results are shown in Figure 1.In chromatographic fingerprinting, 8 peaks are that each test sample is common, therefore determine that these 8 peaks are for total peak.Do Peak homogeneity by diode array detector, these 8 peaks are pure chromatographic peak, and wherein 6# peak is imperatorin, and 7# peak is osthole.
Finally adopt high performance liquid chromatograph to establish column chromatography eight component efficient liquid-phase chromatograph finger print atlas, see Fig. 2-9.
2.2.6 methodological study
1. precision test gets control medicinal material solution, continuous sample introduction 5 times, and the RSD recording test sample each total peak relative retention time (taking osthole as contrast) is all less than 3%, shows that the precision of sample introduction and instrument is good, in table 1.
Table 1 Precision test result
| Sequence number | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# |
| 1 | 0.362 | 0.434 | 0.613 | 0.689 | 0.765 | 0.959 | 1.000 | 1.148 |
| 2 | 0.355 | 0.431 | 0.607 | 0.686 | 0.766 | 0.962 | 1.000 | 1.149 |
| 3 | 0.355 | 0.427 | 0.608 | 0.682 | 0.758 | 0.957 | 1.000 | 1.146 |
| 4 | 0.361 | 0.434 | 0.613 | 0.686 | 0.766 | 0.960 | 1.000 | 1.147 |
| 5 | 0.356 | 0.430 | 0.612 | 0.688 | 0.765 | 0.959 | 1.000 | 1.147 |
| RSD（%） | 1.01 | 0.65 | 0.44 | 0.36 | 0.42 | 0.18 | 0.00 | 0.11 |
2. replica test gets control medicinal material 6 parts, prepares solution according to 2.2.4 method, and the RSD that sample introduction records each total peak relative retention time (be with osthole contrast) respectively is all less than 3%, shows method repeatability better, in table 2.
Table 2 replica test result
| Sequence number | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# |
| 1 | 0.363 | 0.435 | 0.623 | 0.685 | 0.764 | 0.956 | 1.000 | 1.146 |
| 2 | 0.356 | 0.424 | 0.617 | 0.687 | 0.763 | 0.961 | 1.000 | 1.148 |
| 3 | 0.353 | 0.425 | 0.610 | 0.683 | 0.756 | 0.956 | 1.000 | 1.148 |
| 4 | 0.357 | 0.437 | 0.612 | 0.687 | 0.761 | 0.959 | 1.000 | 1.147 |
| 5 | 0.359 | 0.432 | 0.610 | 0.689 | 0.764 | 0.955 | 1.000 | 1.145 |
| 6 | 0.354 | 0.435 | 0.603 | 0.682 | 0.761 | 0.958 | 1.000 | 1.146 |
| RSD（%） | 1.11 | 1.31 | 1.14 | 0.36 | 0.37 | 0.22 | 0.00 | 0.11 |
3. stability test gets control medicinal material solution, respectively 0, and 2,4,6,8,12 h sample introductions, the RSD recording each total peak relative retention time (taking osthole as contrast) is all less than 3%, shows that sample is stable in 12h, in table 3.
Table 3 stability test result
| Time (h) | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# |
| 0 | 0.365 | 0.426 | 0.615 | 0.681 | 0.766 | 0.961 | 1.000 | 1.150 |
| 2 | 0.363 | 0.426 | 0.618 | 0.683 | 0.770 | 0.963 | 1.000 | 1.149 |
| 4 | 0.362 | 0.428 | 0.614 | 0.679 | 0.758 | 0.960 | 1.000 | 1.147 |
| 6 | 0.357 | 0.432 | 0.608 | 0.682 | 0.764 | 0.951 | 1.000 | 1.142 |
| 8 | 0.360 | 0.429 | 0.614 | 0.689 | 0.766 | 0.953 | 1.000 | 1.141 |
| 12 | 0.358 | 0.437 | 0.610 | 0.690 | 0.764 | 0.952 | 1.000 | 1.148 |
| RSD（%） | 0.87 | 0.97 | 0.58 | 0.65 | 0.49 | 0.55 | 0.00 | 0.35 |
2.2.7 each component sample of column chromatography measures and measures Fructus Cnidii variable concentrations column chromatography sample under these conditions, the results are shown in Figure 2.The peak retained near 25min, 26min is respectively imperatorin and osthole.
Two, Fructus Cnidii hypnotic activity component pharmacodynamic experiment research
(1) Fructus Cnidii active component hypnosis experiment screening
1 material
1.1 medicines and reagent
Fructus Cnidii: take from Shanxi Institute of Traditional Chinese Medicine's medical herbs room, through Specimen Room height sky, institute for drug control, Shanxi Province like professor of pharmacy qualification, be defined as Cnidium Cusson plant cnidium monnieri [
cnidium monnieri(L.) Cuss.] dry mature fruit, the used time is ground into coarse powder;
Diazepam tablets: Shanghai Pharmaceutical's letter friendship pharmacy head factory, lot number 090101;
Pentobarbital sodium: Chemical Reagent Co., Ltd., Sinopharm Group, lot number WS20050411; All the other reagent are commercially available analytical pure;
Ethanol: medical alcohol; Tween 80: be analytical pure.
1.2 animal
Mice, Kunming kind, cleaning grade, body weight (20 ± 2) g, by Institute of Experimental Animals, Chinese Academy of Medical Sciences's breeding field
There is provided, licence is numbered SCXK(capital) 2004-0001,0089322.
2 methods
2.1 Fructus Cnidii column chromatography water extracts, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction preparation (the same)
2.2 animal grouping and administration
Get little 100, male and female half and half, be divided at random blank, diazepam positive control (3mg/kg), water extract, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction totally 10 groups, Fructus cnidii extract dosage is 62.5mg/kg, gavage volume 20ml/kg, is all made into suspension with 10% alcoholic solution, every day 1 time, continuous 3 days, blank group was filled with 10% alcoholic solution.
2.3 sleep Indexs measure
After last administration 60min, each group of mice equal lumbar injection pentobarbital sodium 50mg/kg, sleep is index with righting reflex loss, more than 30s person is kept with the downward posture of animal back, be judged as righting reflex loss, record injection pentobarbital sodium after to mice sleeping duration as dropping asleep latency, and observed and recorded righting reflex loss to awakening time as the prolonged sleep time.
3 results
Result shows, Fructus Cnidii column chromatography water extract, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction group dropping asleep latency and blank group difference of respectively organizing that there are no significant; Fructus Cnidii column chromatography water extract, 30% ethanol extraction group prolonged sleep time compare there was no significant difference with blank group; Fructus Cnidii column chromatography 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction compare with blank group can the significant prolongation pentobarbital sodium HD mice prolonged sleep time (
p<0.01,
p<0.001,
p<0.001,
p<0.05,
p<0.05,
p<0.01); Show that the active component playing Fructus Cnidii syngignoscism is 40%, 50%, 60%, 70%, 80%, 95% ethanol column chromatography position, have certain inhibitory action to central nervous system.The results are shown in Table 4.
Table 4 Fructus Cnidii column chromatography different component on the impact of pentobarbital sodium HD mouse sleep time (
±
s, n=10)
| Group | Dosage (mg/kg) | Dropping asleep latency (min) | The length of one's sleep (min) |
| Blank | - | 3.65±1.73 | 84.1±20.1 |
| Positive control | 3.0 | 3.48±1.80 | 191.3±43.4*** |
| Water extraction | 62.5 | 4.21±1.73 | 85.9±28.4 |
| 30% alcohol extraction | 62.5 | 2.93±0.25 | 81.8±17.4 |
| 40% alcohol extraction | 62.5 | 4.38±1.18 | 103.8±16.1* |
| 50% alcohol extraction | 62.5 | 3.01±0.42 | 148.5±39.7*** |
| 60% alcohol extraction | 62.5 | 3.47±1.25 | 133.5±29.1*** |
| 70% alcohol extraction | 62.5 | 3.33±0.83 | 100.7±13.6* |
| 80% alcohol extraction | 62.5 | 3.38±0.50 | 102.6±13.0* |
| 95% alcohol extraction | 62.5 | 3.28±0.47 | 125.5±37.2** |
Compare with blank group: *
p<0.05 * *
p<0.01 * * *
p<0.001
Can learn according to upper table data analysis, the extract obtained with the alcohol extraction of 50-60% has good hypnotic effect.
(2) Fructus Cnidii ethanol extract LD
50mensuration research
Learning through preliminary experiment causes the dead dosage of mice 0% and 100% to be respectively 5g/kg and 30g/kg.
Getting body weight and get mice 60, male and female half and half, be divided into 6 groups at random, take 30g/kg as maximum dose level, and each dosage group is in 1:0.75 ratio, and concrete dosage is in table 9.Gavage proxima luce (prox. luc), each group mice fasting 12 hours, freely drinks water, test the same day, each group mice gavage gives Fructus Cnidii 95% ethanol extract, is made into variable concentrations for reagent liquid with 2% Tween 80, slight fever makes dissolving, the reaction of observed and recorded mouse toxicity and death condition after administration.Fructus Cnidii ethanol extract LD is calculated by Bliss method
50and 95% credibility interval.The results are shown in Table 5.
Table 5 Fructus Cnidii ethanol extract LD
50measurement result
| Group | Dosage (g/kg) | Log10 dose | Mus number | Death toll | Mortality rate P | P 2 |
| 1 | 7.12 | 0.853 | 10 | 2 | 0.2 | 0.04 |
| 2 | 9.49 | 0.977 | 10 | 4 | 0.4 | 0.16 |
| 3 | 12.66 | 1.102 | 10 | 8 | 0.8 | 0.64 |
| 4 | 16.88 | 1.227 | 10 | 8 | 0.8 | 0.64 |
| 5 | 22.50 | 1.352 | 10 | 9 | 0.9 | 0.81 |
| 6 | 30.00 | 1.477 | 10 | 10 | 1 | 1 |
Result shows, and after gastric infusion 30min, toxic reaction in various degree all appears in each group mice, severe poisoning, occur that lethargy is depressed, movable minimizing, tired contracting, hogback, feed stops, and occurs dead in different time, as died non-in 24h, recovers normal all gradually.Application Bliss method calculates LD
50be 10.32 g/kg, 95% credibility interval is 8.33 ~ 12.79 g/kg.Its hypnosis effective dose is 0.0625g/kg, can prove that the safety of Fructus Cnidii ethanol extract is larger.
Claims (1)
1. a Fructus Cnidii hypnotic activity component is preparing the application in hypnotic drug, the preparation technology of described Fructus Cnidii hypnotic activity component, step is as follows: step one, get Fructus Cnidii coarse powder, add the ethanol of 95%, heating and refluxing extraction 1-5 time, each 1-2h, merging filtrate, decompression recycling ethanol, concentrate to obtain extractum, step 2, get macroporous adsorbent resin, soaked overnight, wet method dress post, by distilled water flushing chromatographic column extremely without alcohol taste, loading after above-mentioned extractum is dissolved with 95% ethanol, step 3, eluting is carried out with 50-60% ethanol, each eluting 4 ~ 8 times of column volumes are not etc., eluent concentrating under reduced pressure, recycling design is to small size, merge fraction, reconcentration, cold drying obtains Fructus Cnidii tranquilizing soporific active component.
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| CN115813986B (en) * | 2022-11-07 | 2023-08-15 | 山西省中医药研究院（山西省中医院） | A safe and effective Chinese medicinal composition for treating insomnia without toxic and side effects, and its preparation method |
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| Title |
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| 蛇床子的药理作用研究进展;朱艳杰,周洪智;《黑龙江医药》;20100430;第23卷(第4期);618－619 * |
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