CN102397308A - 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 the Chinese medicine extraction technical field, be specifically related to a kind of preparation technology of Fructus Cnidii hypnotic activity component.
Background technology
Fructus Cnidii (Fructus cnidii) is the samphire cnidium monnieri
Cnidium monnieri(L.) dry mature fruit of Cuss..Chinese medicine is learned and is thought that Fructus Cnidii is hot, bitter, warm in nature, slightly poisonous, returns kidney channel, and warming the kidney to invigorate YANG is arranged, and dampness is dispeled the wind, parasite killing.Be used for sexual impotence, cold womb, cold-damp leukorrhagia, arthralgia chiefly caused by damp pathogen lumbago; The external treatment vulval eczema, married woman's pudendal pruritus, trichomonal vaginitis." medical and health " in February, 2010; Disclose under the effect of Fructus Cnidii ultrasound wave in " screening of Fructus Cnidii tranquilizing soporific extraction process of effective component " literary composition; Utilize extractions such as petroleum ether, ethyl acetate, n-butyl alcohol, ethanol, water, can obtain the different extract of hypnotic effect through different extraction media.Research shows; The coumarin composition osthole (osthol) of extraction separation has certain inhibitory action to nervus centralis in the Fructus Cnidii; 50%～95% alcohol heating reflux extract has sedative-hypnotic effect, but to its be applicable to industrialized great production preparation technology, drug effect safety and with drug effect maybe the further investigation as yet at present of closely-related finger printing.
Western medicine class tranquilizing soporific chemical medicine life-time service at present commonly used is prone to produce tolerance, and therapeutic index is low, dependency and withdrawal symptom seriously and the daytime be still drank after a night, bounce aypnia, dysmnesia, to the infringement of cognition and psychomotor function etc.Traditional Chinese medicine for tranquilization commonly used has Semen Ziziphi Spinosae, Cortex Albiziae, Caulis Polygoni Multiflori, Radix Polygalae, Semen Platycladi etc., and these kinds are very few, and owing to the restriction of resource, the increase of consumption, causes the Traditional Chinese medicine for tranquilization price of determined curative effect high year after year.
Fructus Cnidii distributes extensively, and the equal suitable planting of China's most of areas has cold-resistant drought-enduringly, requires not tight to soil; The characteristics that growth is fast, output is high, cheap, utilize Fructus Cnidii aboundresources, cheap advantage, so in order to increase Fructus Cnidii hypnosis effect; Improve its medical value, enlarge the selection of clinical insomnia's medication, therefore; Employing can be adapted to the big simple and easy to do preparation technology that produces, and from Fructus Cnidii, extracts to have syngignoscism active component safely and effectively, helps to develop and use the Fructus Cnidii herb resource; For preparation hypnosis natural drug lays the foundation, promote the Chinese crude drug industrialization, significant for the development Chinese traditional medicinal economy.
Summary of the invention
Problems such as the present invention is low from Fructus Cnidii extraction hypnosis active component efficient at present in order to solve, and output is few provide a kind of method for preparing of from Fructus Cnidii, extracting the active component with hypnotic activity.
The present invention is realized by following technical scheme; A kind of preparation technology of Fructus Cnidii hypnotic activity component; Be to utilize solvent from the Fructus Cnidii coarse powder, to extract crude extract through heating reflux method; Concentrate and obtain extractum, extractum is carried out further macroporous adsorbent resin column chromatography separate, effectively extracted component.
Concrete steps are following:
Step 1: get the Fructus Cnidii coarse powder, add 95% ethanol, heating and refluxing extraction 1-5 time, each 1-2h, merging filtrate, decompression recycling ethanol, concentrate extractum,
Step 2: get macroporous adsorbent resin, soaked overnight, wet method dress post to there not being the alcohol flavor, is gone up appearance with above-mentioned extractum with 95% ethanol liquid dissolving back with the distilled water flushing chromatographic column,
Step 3: carry out eluting with 40%-95% ethanol, preferred 50-60%, each 4～8 times of column volumes of eluting do not wait, and the eluent concentrating under reduced pressure reclaims solvent to small size, merges fraction, reconcentration, cold drying gets Fructus Cnidii tranquilizing soporific active component.
The component that above extraction obtains is carried out the hypnosis experiment, prove that there is certain syngignoscism at Fructus Cnidii 40%～95% ethanol column chromatography position, has certain inhibitory action to the central nervous system.Application of B liss 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, explains that safety is bigger.
Characteristics of the present invention are:
1. reported first of the present invention Fructus Cnidii syngignoscism ethanol column chromatography preparation technology, be development and use Fructus Cnidii herb 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, and is simple for process, is fit to large-scale industrial production, can increase economic efficiency.The present invention requires low, easy to implement to appointed condition, step is succinct, and production cost is low.
Description of drawings
Fig. 1 is the standard diagram HPLC of Fructus cnidii extract
Fig. 2 is the Fructus cnidii extract collection of illustrative plates that utilizes water elution to obtain
Fig. 3 is the Fructus cnidii extract collection of illustrative plates that utilizes 30% ethanol elution to obtain
Fig. 4 is the Fructus cnidii extract collection of illustrative plates that utilizes 40% ethanol elution to obtain
Fig. 5 is the Fructus cnidii extract collection of illustrative plates that utilizes 50% ethanol elution to obtain
Fig. 6 is the Fructus cnidii extract collection of illustrative plates that utilizes 60% ethanol elution to obtain
Fig. 7 is the Fructus cnidii extract collection of illustrative plates that utilizes 70% ethanol elution to obtain
Fig. 8 is the Fructus cnidii extract collection of illustrative plates that utilizes 80% ethanol elution to obtain
Fig. 9 is the Fructus cnidii extract collection of illustrative plates that utilizes 95% ethanol elution to obtain.
Figure 10 is the tester collection of illustrative plates.
The specific embodiment
1 instrument and reagent
The Aglient1200 high performance liquid chromatograph, vacuum degassing machine, (G1322A) quaternary pump (G1311A), automatic sampler (G1329A), column oven (G1316A), PDAD (G1315D), HP Chemstation chromatographic work station; : U.S.'s Agilent company limited;
Sartorious 100,000/analytical balance: Sartorius AG;
D101 macroporous adsorbent resin: Tianjin sea light chemical industry company limited lot number 030510 (1-3);
The Fructus Cnidii medical material: purchase the institute of traditional Chinese medicine in the Shanxi Province, Specimen Room liked that the professor of pharmacy identified in high day through the institute for drug control, Shanxi Province;
Osthole (lot number 0822-9802), imperatorin (lot number 11826-200308): all purchase in Nat'l Pharmaceutical & Biological Products Control Institute.
2 experimental techniques and result
2.1 the preparation of the different extracts of Fructus Cnidii column chromatography
Get Fructus Cnidii coarse powder 300g, add the ethanol of 4 times of amounts 95%, heating and refluxing extraction 3 times, each 1.5h, merging filtrate, decompression recycling ethanol concentrates, and cold drying gets the heavy 22.752g of cream.
Take by weighing the 500gD101 macroporous adsorbent resin, 95% soak with ethanol is spent the night, and wet method dress post is not distinguished the flavor of to there being alcohol with the distilled water flushing chromatographic column; Above-mentioned 22.752g extractum is gone up appearance with 95% ethanol liquid dissolving back, add filter paper, bead lid appearance, water, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol carry out eluting successively; Each 4～8 times of column volumes of eluting do not wait, and according to the eluent shade, judge whether to change eluting solvent and form; The eluent decompression and solvent recovery is to small size, merges stream part, altogether 8 components; With each flow point solvent reclaim under reduced pressure, concentrate, cold drying gets 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 μ m, (chromatographic column of 4.6mm * 250mm) is with acetonitrile-0.1% aqueous acetic acid gradient elution; Elution program is: 0 ~ l5min, and acetonitrile is increased to 45%, 15 ~ 30min acetonitrile by 23% and is increased to l00% by 45%; 30 ~ 40min, acetonitrile are l00%; Detect wavelength: 245nm (0 ~ 26 min), 322nm (26 ~ 30 min), 245nm (30 ~ 40 min); Column temperature: 40 ℃.
2.2.2 the preparation of reference substance solution
Precision takes by weighing osthole and imperatorin is an amount of, adds methanol and processes the mixed solution that every 1ml contains 50 μ g and 45 μ g respectively, as reference substance solution.
2.2.3 the preparation of need testing solution
Get each extract of Fructus Cnidii an amount of (being equivalent to the 1g crude drug), put in the 10ml measuring bottle, add 70% ethanol, shake up, filter, as need testing solution to scale.
2.2.4 the preparation of control medicinal material solution
It is an amount of to get the Fructus Cnidii control medicinal material, puts in the 25ml measuring bottle, adds ethanol 15ml, and supersound extraction 30 minutes is put cold rnning ethanol to scale, shakes up, and filters, as control medicinal material solution solution.
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 medical material samples under these conditions, the result sees Fig. 1.8 peaks are that each test sample is common in the chromatographic fingerprinting, confirm that therefore these 8 peaks are total peak.Do the peak purity inspection with PDAD, these 8 peaks are pure chromatographic peak, and wherein the 6# peak is an imperatorin, and the 7# peak is an osthole.
Adopt high performance liquid chromatograph to set up eight component efficient liquid-phase chromatograph finger print atlas of column chromatography at last, see Fig. 2-9.
2.2.6 methodological study
1. control medicinal material solution is got in the precision test, continuous sample introduction 5 times, and the RSD that records each total peak RRT of test sample (is contrast with the osthole) shows that all less than 3% the precision of sample introduction and instrument is good, sees 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 is got 6 parts of control medicinal materials, prepares solution according to the 2.2.4 method, respectively sample introduction record each total peak RRT (is contrast with the osthole) RSD all less than 3%, show that method repeatability better, sees 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 is got control medicinal material solution, and respectively 0,2,4,6,8,12 h sample introductions, the RSD that records each total peak RRT (is contrast with the osthole) show that all less than 3% sample is stable in 12h, see 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 is measured and measured Fructus Cnidii variable concentrations column chromatography sample under these conditions, the result sees Fig. 2.Near the peak that keeps 25min, the 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 medicine and reagent
Fructus Cnidii: take from Shanxi Institute of Traditional Chinese Medicine medical herbs room, Specimen Room liked that a professor of pharmacy identified in high day through the institute for drug control, Shanxi Province, confirm as Cnidium Cusson plant cnidium monnieri [
Cnidium monnieri(L.) Cuss.] dry mature fruit, the time spent 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, the Kunming kind, the cleaning level, body weight (20 ± 2) g is by Institute of Experimental Animals, Chinese Academy of Medical Sciences's breeding field
Provide, licence is numbered SCXK (capital) 2004-0001,0089322.
2 methods
2.1 Fructus Cnidii column chromatography water extract, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction preparation (the same)
2.2 animal divides into groups and administration
Get for a short time 100, male and female half and half are divided into totally 10 groups of blanks, diazepam positive control (3mg/kg), water extract, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction at random; The Fructus cnidii extract dosage is 62.5mg/kg; Irritate stomach volume 20ml/kg, all be made into suspension, every day 1 time with 10% alcoholic solution; Continuous 3 days, the blank group was irritated with 10% alcoholic solution.
2.3 the sleep index detects
Behind last administration 60min; Each organizes the equal lumbar injection pentobarbital sodium of mice 50mg/kg; Sleep is index with the righting reflex loss, keeps the above person of 30s with the downward posture of animal back, is judged as righting reflex loss; Behind the record injection pentobarbital sodium to the mice righting reflex loss time as dropping asleep latency, and the time of observed and recorded righting reflex loss to awakening is as the prolonged sleep time.
3 results
The result shows, Fructus Cnidii column chromatography water extract, 30%, 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction group dropping asleep latency and blank group be each difference of organizing that there are no significant relatively; Fructus Cnidii column chromatography water extract, 30% ethanol extraction group prolonged sleep time and blank group be there was no significant difference relatively; Fructus Cnidii column chromatography 40%, 50%, 60%, 70%, 80%, 95% ethanol extraction and blank group relatively can the significant prolongation pentobarbital sodium HD mice prolonged sleep times (
P<0.01,
P<0.001,
P<0.001,
P<0.05,
P<0.05,
P<0.01); The active component that shows performance Fructus Cnidii syngignoscism is 40%, 50%, 60%, 70%, 80%, 95% ethanol column chromatography position, and the central nervous system is had certain inhibitory action.The result sees table 4.
Table 4 Fructus Cnidii column chromatography different component to the influence 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 is carried | 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 the blank group: *
P<0.05 * *
P<0.01 * * *
P<0.001
Can learn that according to last table data analysis the extract that obtains with the alcohol extraction of 50-60% has hypnotic effect preferably.
(2) Fructus Cnidii ethanol extract LD
50
Mensuration research
Learn through preliminary experiment and to cause that mice 0% and 100% dead dosage are respectively 5g/kg and 30g/kg.
Get body weight and get 60 of mices, male and female half and half are divided into 6 groups at random, are maximum dose level with 30g/kg, and each dose groups is in the 1:0.75 ratio, and concrete dosage is seen table 9.Irritate the stomach proxima luce (prox. luc), each organized the mice fasting 12 hours, freely drank water; Test same day, each is organized mice and once irritates stomach and give Fructus Cnidii 95% ethanol extract, supplies reagent liquid to be made into variable concentrations with 2% Tween 80; Slight fever makes dissolving, reaction of observed and recorded mouse toxicity and death condition after the administration.Calculate Fructus Cnidii ethanol extract LD with the Bliss method
50And 95% credibility interval.The result sees table 5.
Table 5 Fructus Cnidii ethanol extract LD
50
Mensuration result
| Group | Dosage (g/kg) | Log10 dose | The 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 |
The result shows that behind the gastric infusion 30min, each is organized mice and toxic reaction in various degree all occurs, the poisoning severe patient; It is depressed lethargy to occur, movable minimizing, tired contracting, hogback; Feed stops, and death occurs in different time, like not dead person in the 24h, all recovers normal gradually.Application of B liss 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 bigger.
Claims (3)
1. the preparation technology of a Fructus Cnidii hypnotic activity component; It is characterized in that: utilize solvent from the Fructus Cnidii coarse powder, to extract crude extract through heating reflux method; Concentrate and obtain extractum; Extractum is carried out further macroporous adsorbent resin column chromatography separate, use 40%-95% ethanol to carry out eluting, effectively extracted component.
2. the preparation technology of Fructus Cnidii hypnotic activity component according to claim 1 is characterized in that step is following:
Step 1 is got the Fructus Cnidii coarse powder, adds 95% ethanol, heating and refluxing extraction 1-5 time, each 1-2h, merging filtrate, decompression recycling ethanol, concentrate extractum,
Step 2 is got macroporous adsorbent resin, soaked overnight, and wet method dress post to there not being the alcohol flavor, is gone up appearance with above-mentioned extractum with 95% ethanol liquid dissolving back with the distilled water flushing chromatographic column,
Step 3 is carried out eluting with 40%-95% ethanol, and each 4～8 times of column volumes of eluting do not wait, and the eluent concentrating under reduced pressure reclaims solvent to small size, merges fraction, reconcentration, and cold drying gets Fructus Cnidii tranquilizing soporific active component.
3. the preparation technology of Fructus Cnidii hypnotic activity component according to claim 1 is characterized in that: the concentration of alcohol that eluting uses is 50-60%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104127339A (en) * | 2014-07-09 | 2014-11-05 | 扬州中汇生物技术有限公司 | Fructus cnidii anti-allergic effective component, extracting method and applications thereof |
| CN105030863A (en) * | 2015-08-20 | 2015-11-11 | 陈鹏 | Fructus cnidii extract and anti-tumor application thereof |
| CN115813986A (en) * | 2022-11-07 | 2023-03-21 | 山西省中医药研究院（山西省中医院） | Safe and effective traditional Chinese medicine composition for treating insomnia without toxic and side effects and preparation method thereof |
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| CN1724529A (en) * | 2005-07-22 | 2006-01-25 | 中国医学科学院放射医学研究所 | High purity cnidicin and preparation method thereof and be the pharmaceutical composition of activeconstituents with this compound |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1724529A (en) * | 2005-07-22 | 2006-01-25 | 中国医学科学院放射医学研究所 | High purity cnidicin and preparation method thereof and be the pharmaceutical composition of activeconstituents with this compound |
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| 朱艳杰,周洪智: "蛇床子的药理作用研究进展", 《黑龙江医药》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104127339A (en) * | 2014-07-09 | 2014-11-05 | 扬州中汇生物技术有限公司 | Fructus cnidii anti-allergic effective component, extracting method and applications thereof |
| CN105030863A (en) * | 2015-08-20 | 2015-11-11 | 陈鹏 | Fructus cnidii extract and anti-tumor application thereof |
| CN115813986A (en) * | 2022-11-07 | 2023-03-21 | 山西省中医药研究院（山西省中医院） | Safe and effective traditional Chinese medicine composition for treating insomnia without toxic and side effects and preparation method thereof |
| 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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