CN103142677A - Method for extracting phenolic acid compound from honeysuckle leaves - Google Patents
Method for extracting phenolic acid compound from honeysuckle leaves Download PDFInfo
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Abstract
The invention discloses a method for extracting a phenolic acid compound from honeysuckle leaves. The method comprises the following steps of soaking proper amount of honeysuckle leaves in water, cooking the honeysuckle leaves, extracting the cooked honeysuckle leaves for 2 to 3 times, combining filtrates, concentrating the mixed filtrate, adjusting the pH value to be between 1 and 4 by using hydrochloric acid, centrifuging the filtrate, filtering the supernatant by using 14-90-mesh polyamide, washing the solution by using water and ethanol with the concentration of 30 to 95 percent respectively, collecting the ethanol washing solution, reclaiming the ethanol, and drying the solution to obtain the phenolic acidic extract with over 50 percent of phenolic acid compound. The method has high repeatability, the content of extracted phenolic acid compound is stable, and the method is simply and conveniently operated, low in cost and suitable for industrial production. The product prepared by the method can be prepared into formulations, such as capsules, tablets, granules, pills, particles, injections, dripping pills, oral solution and subcutaneous preparations or suppository, or sustained-release formulations.
Description
Technical field
The present invention relates to a kind of method of extracting phenolic acid compound, more specifically say a kind of employing polycaprolactam technology, improve the method for phenolic acid compound content in the Folium Lonicerae extract, belong to medical technical field.
Background technology
Folium Lonicerae be conventional Chinese medicine Flos Lonicerae same plant Radix Ophiopogonis (
Lonicera japonicaThunb.) tradition is discarded part.Flos Lonicerae is one of 38 kinds of conventional Chinese medicines, has stronger antibiotic, antivirus action, is widely used in tradition and modern traditional Chinese patent medicine recipe and a large amount of clinical prescription.In the Radix Ophiopogonis planting process, be the growth that guarantees alabastrum, need repeatedly trimming and finishing and discarded a large amount of Folium Lonicerae (be same plant Flos Lonicerae output 10 times), the wasting of resources is huge.The effective constituent that mainly contains of Folium Lonicerae and Flos Lonicerae is phenolic acid compound, same units weight Folium Lonicerae organic acid content is 70% of Flos Lonicerae, have quite high research for application and development and be worth, but to not yet finding to make take Folium Lonicerae as medical material at present the precedent of Chinese patent medicine preparation both at home and abroad.Studies confirm that, antiviral and antibiotic drug effect that Folium Lonicerae extracts composition are better than Flos Lonicerae extract.Result of study also shows, the Folium Lonicerae purified product to the antibacterial activity of staphylococcus aureus, Shigella flexneri, beta hemolytic streptococcus, escherichia coli and streptococcus pneumoniae higher than the Flos Lonicerae purified product, the MBC value differs 1-2 doubling dilution degree, and its possible cause is that the content of Folium Lonicerae and Flos Lonicerae phenolic acids chemical composition forms the difference that exists.According to data; Flos Lonicerae mainly contains chlorogenic acid (Chlorogenicacid); the main effective ingredient of Folium Lonicerae is isochlorogenic acid (dicaffeoyl-quinic acid; Dicaffeoylquinic acids); wherein 4; 5-dicaffeoyl-quinic acid (4,5-Dicaffeoyl quinic acid) content is higher.
In recent years, domestic many units had once carried out the research of extracting method to the Folium Lonicerae composition, comprised (Chinese Forest by-product and speciality, 2002, the 1:38-39 such as water extraction, alcohol extracting method, microwave-assisted extraction method, enzyme process and macroreticular resin absorbing method; The Sichuan food and fermentation, 2006,130:52-57; The Shaanxi traditional Chinese medical science, 2008,6:734-735; Agricultural University Of Jiangxi's journal, 2008,1:137); According to the test of data and repeated authentication, it is lower that above offering of materials method is extracted Folium Lonicerae effective ingredient (being mainly liposoluble ingredient) purity, how below 20-30%.Publication number is Chinese patent application and " Chinese patent medicine " the 7th phase in 2007 (attached 6-7) of 101269107A to disclose the result of study that adopts D101 macroporous resin extraction Folium Lonicerae chlorogenic acid composition; According to report, adopt the Folium Lonicerae extract Content of Chlorogenic Acid of this method preparation can reach more than 50%; But the method exists the more difficult control of experiment condition, the relatively poor shortcoming of repeatability.Publication number is the process that the Chinese patent of CN1398845A discloses macroporous resin adsorption raising chlorogenic acid content; This process falls behind situation for the technique of chlorogenic acid extracting from Flos Lonicerae, and the process for extracting of Chlorogenic Acid of Flos Lonicerae composition is optimized, and extracts Flos Lonicerae composition Content of Chlorogenic Acid and has reached more than 80%; But, because there is notable difference in composition and the content of (main effective ingredient be isochlorogenic acid) phenolic acid compound in Flos Lonicerae (mainly containing chlorogenic acid) and Folium Lonicerae, adopt publication number not reach similar effect for the method that the Chinese patent of CN1398845A provides in the extraction of Folium Lonicerae liposoluble ingredient; And adopting methanol in this patent process is the eluent of isochlorogenic acid in macroporous adsorbent resin, the residual and environmental pollution due to the methanol in its extract that may cause, and this technique is not suitable for using in suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting phenolic acid compound from Folium Lonicerae, to improve phenolic acid compound content in the Folium Lonicerae extract, overcome the shortcoming of prior art.
Method of the present invention comprises the following steps:
(1) soak 0.5-1.5h after Folium Lonicerae cutting or pulverizing, boil and carry 2-3 time, the 10-20 water doubly that at every turn adds the Folium Lonicerae raw materials quality, extract 50-100min under 80-100 ℃ of condition, merge extractive liquid,, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby;
(2) adding hydrochloric acid to adjust pH value in the gained supernatant is 1-4, centrifugalize, supernatant with polycaprolactam after, be washed till neutrality with purified water, be the ethanolysis absorption of 30%-95% with mass concentration again, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry, namely get required product at last.
In the present invention, the described extracting method of step (1) can also adopt water temperature to soak the methods such as method or ethanol refluxing process or ethanol warm macerating method or ultrasonic extraction and extract phenolic acid compound in Folium Lonicerae.
Wherein, water temperature lixiviate access method is: add the 10-20 water doubly that water adds the Folium Lonicerae raw materials quality after Folium Lonicerae cutting or pulverizing, soak 2-3 time under 40-80 ℃ of condition, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby.
Wherein, the alcohol reflux method is: the Folium Lonicerae cutting or pulverize after add the 10-20 60%-80% alcohol reflux doubly 2-3 time of Folium Lonicerae raw materials quality, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby.
Wherein, ethanol warm macerating extracting method is: the 10-20 70%-95% ethanol doubly that adds the Folium Lonicerae raw materials quality after Folium Lonicerae cutting or pulverizing, soak 2-3 time in 50-70 ℃, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets clear liquid standby.
Wherein, ultrasonic extracting method is: the Folium Lonicerae cutting or pulverize after add the 10-20 water supersound extraction doubly 3 times of Folium Lonicerae raw materials quality, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby.
Method of the present invention, in step (2), in absorption Folium Lonicerae extract, the granularity of phenolic acid compound polyamide used is the 14-90 order, consumption and quality of medicinal material ratio are 0.5-1:1.
Method of the present invention, in step (2), after the polycaprolactam of absorption Folium Lonicerae extract with the 1.0-3.0BV(BV-bed volume, in full with) water rinse, then add the 5.0BV(bed volume) mass concentration be the ethanol elution of 30%-95%.
In the resulting Folium Lonicerae extract of the present invention, the content of phenolic acid compound is more than 50%.
The resulting product of the present invention can be made dosage form or their the slow release forms such as clinical capsule commonly used, tablet, electuary, pill, granule, injection, drop pill, oral liquid, subcutaneous administration preparation or suppository according to a conventional method.
The beneficial effect that the present invention obtains is:
1, in the Folium Lonicerae extract that extracts of the inventive method in thing phenolic acid compound content higher, more than 50%.
2, process of the present invention is easy, condition is controlled, has good repeatability.
3, the present invention is fit to the extraction of phenolic acid compound in Folium Lonicerae, and process non-environmental-pollution and the residual shortcoming of extract methanol are conducive to environmental conservation and drug safety.
The Pharmacodynamic test of active extract conclusion of the phenolic acid compound that 4, extracts from Folium Lonicerae by method of the present invention is: the phenolic acid compound that Folium Lonicerae extracts is better than same procedure to the antibacterial activity of staphylococcus aureus, Shigella flexneri, beta hemolytic streptococcus, escherichia coli and streptococcus pneumoniae and extracts and the identical or close Flos Lonicerae extract of phenolic acid compound content, and minimal bactericidal concentration (MBC value) differs 1-2 doubling dilution degree.See embodiment 5 for details.
The specific embodiment
Following examples only represent illustrative embodiment of the present invention, but the present invention is not subjected to the restriction of these embodiment.
Embodiment 1
soak 0.5h after the dry medical material cutting of Folium Lonicerae or pulverizing, boil and carry 2 times, the water of 15 times that at every turn adds the Folium Lonicerae raw materials quality, extract 75min under 100 ℃ of conditions, merge above-mentioned 2 extracting solution, 60 ℃ the decompression or normal pressure be concentrated into 4 times of medical material amounts, centrifugalize, get supernatant, adding hydrochloric acid to adjust pH value is 1, centrifugalize, polyamide column on supernatant, adsorb with 2.0BV/h, be washed till neutrality with the 1BV purified water with the 3.0BV/h flow velocity, be that 30% ethanol is with 2.0BV/h flow velocity desorption with concentration again, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry are to doing at last, and get final product.Product is through check, and total phenolic content is 51.92%, yield 1.61%.
The detection method of total phenolic content: adopt the HPLC method, Discovery C
18Analyze chromatographic column, water-formic acid (100: 0.5) and acetonitrile are mobile phase, and flow 1.0 ml/min adopt the gradient program, 328 nm wavelength detected peaks areas.Peak before 25min is take chlorogenic acid as contrast, and the peak after 25min for contrast, calculates the content of phenolic acid compound with 4,5-O-dicaffeoyl-quinic acid.
Yield (%)=paste-forming rate * total phenolic content.
Paste-forming rate (%)=(preparation finished product quality/extraction medical material (Folium Lonicerae) quality) * 100%.
Embodiment 2
soak 0.5h after the dry medical material cutting of Folium Lonicerae or pulverizing, boil and carry 2 times, the water of 15 times that at every turn adds the Folium Lonicerae raw materials quality, extract 75min under 100 ℃ of conditions, merge above-mentioned 2 extracting solution, 60 ℃ the decompression or normal pressure be concentrated into 5 times of medical material amounts, centrifugalize, get supernatant, adding hydrochloric acid to adjust pH value is 1, centrifugalize, polyamide column on supernatant, adsorb with 2.0BV/h, be washed till neutrality with the 2BV purified water with the 3.0BV/h flow velocity, be that 50% ethanol is with 2.0BV/h flow velocity desorption with concentration again, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry are to doing at last, and get final product.Product is with embodiment 1 method check, and total phenolic content is 52.53%, yield 1.68%.
Embodiment 3
soak 0.5h after the dry medical material cutting of Folium Lonicerae or pulverizing, boil and carry 2 times, the water of 15 times that at every turn adds the Folium Lonicerae raw materials quality, extract 75min under 100 ℃ of conditions, merge above-mentioned 2 extracting solution, 60 ℃ the decompression or normal pressure be concentrated into 6 times of medical material amounts, centrifugalize, get supernatant, adding hydrochloric acid to adjust pH value is 1, centrifugalize, polyamide column on supernatant, adsorb with 2.0BV/h, be washed till neutrality with the 3BV purified water with the 3.0BV/h flow velocity, be that 95% ethanol is with 2.0BV/h flow velocity desorption with concentration again, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry are to doing at last, and get final product.Product is with embodiment 1 method check, and total phenolic content is 52.74%, yield 1.71%.
Embodiment 4
The present embodiment is comparison example, namely adopts phenolic acid compound in water extraction, macroporous resin adsorption purification Folium Lonicerae.Detailed process is as follows:
(1) the dry medical material 50g of Folium Lonicerae, soak 0.5h after cutting or pulverizing, boil and carry 2 times, add the water of 15 times of Folium Lonicerae raw materials quality at every turn, extract 75min under 100 ℃ of conditions, merge above-mentioned 2 extracting solution, 60 ℃ the decompression or normal pressure be concentrated into 5 times of medical material amounts, centrifugalize, get supernatant, adding hydrochloric acid to adjust pH value is 1, centrifugalize, preparation Folium Lonicerae extract sample liquid.
(2) nonpolar SP-700, HPD-700, X-5, D101, the AB-8 of low pole and 6 kinds of macroporous adsorbent resins that suitable phenolic acid compound separates with flavone compound such as NKA-9 of polarity have been compared in test.Take respectively 6 kinds of each 50g of model macroporous adsorbent resin, carry out pretreatment by soak with ethanol, alcohol wash, pickling, alkali cleaning program, sample liquid is added respectively macroporous resin adsorption after above processing, adsorption rate 2.0BV/h is washed till neutrality with the 2BV purified water with the 3.0BV/h flow velocity, then is that 95% ethanol is with 2.0BV/h flow velocity desorption with concentration, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry, namely obtain purified product at last.
Content and the yield result of pressing embodiment 1 method calculating extract phenolic acid compound are as follows:
Result of the test, SP-700 type macroporous resin is to the absorbability of phenolic acid compound in the Folium Lonicerae resin apparently higher than other types, yield 2.30%, product phenolic acid compound content is 25.79%, but SP-700 type macroporous resin is not high to the selectivity of phenolic acid compound, and being the import resin, price is higher, is unsuitable for suitability for industrialized production.Selection is carried out the further test of purifying process to the AB-8 type macroporous resin (yield 1.20%, product phenolic acid compound content is 25.75%) that phenolic acid compound absorbability in Folium Lonicerae is only second to SP-700 type macroporous resin.
(3) leakage plot, loading concentration, sample liquid pH value, absorption flow velocity, eluting water flow velocity, ethanol elution agent concentration, eluant consumption, the elution speed of AB-8 type macroporous resin investigated in test, optimizes AB-8 type purification with macroreticular resin Radix Ophiopogonis heaf total phenolic acid technique as follows:
It is 1:5 that extracting solution is concentrated into solid-liquid ratio, and transferring pH is 2, and the flow velocity take flow velocity as 3.0BV/h is by the AB-8 macroporous adsorbent resin, add 2BV water and rinse resin with the flow velocity of 3.0BV/h, then add 50% the ethanol elution of 5BV, collect eluent, decompression recycling ethanol, the concentrated cream of receiving.Press the content that embodiment 1 method is calculated the extract phenolic acid compound.Result of the test, above technique purification Folium Lonicerae extract yield on average is about 2.0%, total phenolic content is stabilized in 27.12%-28.17%(average 27.47%), do not reach more than 50%.
Embodiment 5
The present embodiment is for comparing by the Folium Lonicerae of the inventive method extraction and the main antibiotic drug effect result of the test of the phenolic acid compound in same plant Different plant parts Flos Lonicerae thereof.
1, experiment material
(1) tested medicine
Extract 1(crude extract): Folium Lonicerae water boiling and extraction, content 12.1%, the total phenolic acid 6.05mg/ml of stock solution 50mg/ml();
Extract 2(purified): the Folium Lonicerae crude extract is through the polyamide adsorption and purification, content 51.92%, the total phenolic acid 26mg/ml of stock solution 50mg/ml();
Extract 3(crude extract): Flos Lonicerae water boiling and extraction, content 11.1%, the total phenolic acid 5.56mg/ml of stock solution 50mg/ml();
Extract 4(purified): the Flos Lonicerae crude extract is through the polyamide adsorption and purification, content 50.39%, the total phenolic acid 25.1mg/ml of stock solution 50mg/ml().
(2) test strain
2, experimental technique
(1) preparation of test organisms liquid: respectively streptococcus pneumoniae, 37 ° of С of beta hemolytic streptococcus were increased bacterium in 18 hours with the 10%FCS-nutrient broth medium and cultivate, test organisms liquid forms with same medium 1:10 dilution.Other antibacterial increased bacterium in 18 hours with 37 ° of С of nutrient broth medium respectively to be cultivated, and same medium 1:100 dilution is test organisms liquid.
(2) mensuration of minimal bactericidal concentration (MBC): Folium Lonicerae, Flos Lonicerae extract be the 50mg/ml(raw material respectively) be initial concentration, use culture medium doubling dilution its to 10 concentration.Wherein, streptococcus pneumoniae, beta hemolytic streptococcus are selected nutrient broth medium (containing 10%FCS) during dilution, and other germ experiment dilutes with common nutrient broth medium.In 24 well culture plates, every hole adds the 1ml dilute liquid medicine, and each dilution factor medicinal liquid is established 2 multiple holes, adds respectively experimental bacteria liquid 50 μ l, and 18 hours 37 ° of С of constant incubator cultivate, and with the naked eye have or not bacterial growth with microscopic examination.
Above observation is got 50ul and is inoculated on the plain agar plating medium without the culture of bacterial growth, and wherein, streptococcus pneumoniae, beta hemolytic streptococcus are inoculated in the blood agar plate culture medium.37 ° of С cultivated in 18 hours, the number of counting bacterium colony.
The high dilution of medicine that is less than 5 (2 dull and stereotyped meansigma methodss) take clump count is as the minimal bactericidal concentration (MBC) of medicine to antibacterial.
3, experimental result (MBC value, wherein drug level: mg/ml)
4, interpretation of result
(1) antimicrobial susceptibility of Flos Lonicerae and Folium Lonicerae extract is relatively:
Flos Lonicerae and Folium Lonicerae extract are close to the sensitivity of antibacterial, sort as follows:
Shigella dysenteriae＞staphylococcus aureus＞beta hemolytic streptococcus＞salmonella typhi, colon bacillus＞streptococcus pneumoniae.
(2) antibacterial activity of Flos Lonicerae, Folium Lonicerae crude extract and purified product is relatively:
The performance of the titre (extension rate) of Flos Lonicerae and Folium Lonicerae purified product antibacterial activity (MBC value) is all higher than crude extract, prompting purified product clinical effective dose be better than (lower than) crude extract.
The MBC value that Flos Lonicerae and Folium Lonicerae purified product calculate with total phenolic acid without clear superiority, points out other compositions of still having in Flos Lonicerae and Folium Lonicerae except total phenolic acid (as flavone etc.) also to bring into play antibacterial action with the crude extract comparison in crude extract.
(3) antibacterial activity of Flos Lonicerae and Folium Lonicerae extract is relatively:
The Folium Lonicerae purified product all is better than Flos Lonicerae purified product, the wherein high 1-4 of an extension rate titre to the bactericidal activity (the MBC value of extension rate, former concentration and total phenols acid concentration) of other outer 5 strains of institute trial division salmonella typhi.Analyze in reason and Flos Lonicerae and Folium Lonicerae liposoluble ingredient different with content ratio relevant.Wherein Flos Lonicerae mainly contains chlorogenic acid, and Folium Lonicerae mainly contains isochlorogenic acid, and isochlorogenic acid is the main antimicrobial component of Radix Ophiopogonis plant different parts extract.
In the preferred embodiment of the invention, the Folium Lonicerae medical material picks up from the Julu County, Hebei province, through Life Science College professor Zhao Jiancheng of Hebei Normal University be accredited as Caprifoliaceae (
Capriroliaceae) plant Radix Ophiopogonis (
Lonicera japonicaThunb) dry blade; The reference substance chlorogenic acid (lot number 110753-200413, purity〉99.3%) and 4,5-O-dicaffeoyl-quinic acid (lot number 3245-88-0, purity〉99.0%) provided by the calibrating of China pharmaceutical biological product; Polyamide is Taizhou City of Zhejiang Province road and bridge tetramethyl biochemical plastic molding and processing plant product; HPLC is chromatographically pure reagent with mobile phase acetonitrile and methanol, is Tianjin Concord Technology Co., Ltd.'s product; High performance liquid chromatograph (600-2489 type) is the Waters product.
Claims (4)
1. method of extracting phenolic acid compound from Folium Lonicerae is characterized in that comprising the following steps:
(1) soak 0.5-1.5h after Folium Lonicerae cutting or pulverizing, boil and carry 2-3 time, the 10-20 water doubly that at every turn adds the Folium Lonicerae raw materials quality, extract 50-100min under 80-100 ℃ of condition, merge extractive liquid,, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby;
(2) adding hydrochloric acid to adjust pH value in the gained supernatant is 1-4, centrifugalize, supernatant with polycaprolactam after, be washed till neutrality with purified water, be the ethanolysis absorption of 30%-95% with mass concentration again, collect desorbed solution, reclaim ethanol and concentrated, decompression or constant pressure and dry, namely get required product at last.
2. method according to claim 1, is characterized in that: adopt water temperature to soak method or ethanol refluxing process or ethanol warm macerating method or ultrasonic extraction when step (1) is extracted;
Wherein, water temperature lixiviate access method is: add the 10-20 water doubly that water adds the Folium Lonicerae raw materials quality after Folium Lonicerae cutting or pulverizing, soak 2-3 time under 40-80 ℃ of condition, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby;
The alcohol reflux method is: the Folium Lonicerae cutting or pulverize after add the 10-20 60%-80% alcohol reflux doubly 2-3 time of Folium Lonicerae raw materials quality, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby;
Ethanol warm macerating extracting method is: the 10-20 mass concentration 70%-95% ethanol doubly that adds the Folium Lonicerae raw materials quality after Folium Lonicerae cutting or pulverizing, soak 2-3 time in 50-70 ℃, each 0.5-1.5h, merge above-mentioned extracting solution several times, 50-70 ℃ the decompression or normal pressure be concentrated into 4-6 times of quality of medicinal material, centrifugalize gets clear liquid standby;
Ultrasonic extracting method is: the Folium Lonicerae cutting or pulverize after add the 10-20 water supersound extraction doubly 3 times of Folium Lonicerae raw materials quality, each 0.5-1.5h merges above-mentioned extracting solution several times, and 50-70 ℃ reduces pressure or normal pressure is concentrated into 4-6 times of quality of medicinal material, centrifugalize gets supernatant standby.
3. method according to claim 1 and 2 is characterized in that: in absorption Folium Lonicerae extract, the granularity of phenolic acid compound polyamide used is the 14-90 order, and consumption and quality of medicinal material ratio are 0.5-1:1.
4. according to claim 1 and 2 or 3 described methods, is characterized in that: with the water flushing of 1.0-3.0 times of bed volume, then add the ethanol elution of the mass concentration 30%-95% of 5.0 times of bed volumes after polycaprolactam.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1684699A (en) * | 2002-09-11 | 2005-10-19 | Sk化学株式会社 | Extraction and purification method of active constituents from stem of lonicera japonica thunb., its usage for anti-inflammatory and analgesic drug |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1684699A (en) * | 2002-09-11 | 2005-10-19 | Sk化学株式会社 | Extraction and purification method of active constituents from stem of lonicera japonica thunb., its usage for anti-inflammatory and analgesic drug |
Non-Patent Citations (2)
| Title |
|---|
| 刘婵娟等: "忍冬叶的化学成分", 《中国实验方剂学杂志》 * |
| 胡润淮等: "忍冬叶中绿原酸和总黄酮分离工艺的研究", 《河南科学》 * |
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Application publication date: 20130612 |