CN109700899B - Sichuan blackberry lily scutellaria baicalensis flavone extract and preparation method and application thereof - Google Patents
Sichuan blackberry lily scutellaria baicalensis flavone extract and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a Sichuan blackberry lily scutellaria flavone extract, which is an extract prepared by using Sichuan blackberry lily and scutellaria powder as raw materials, extracting with water, separating and purifying an extracting solution, filtering and drying. The anti-inflammatory, analgesic and antitussive effects of the Sichuan blackberry lily radix scutellariae flavone extract are better than that of the Sichuan blackberry lily flavone extract, the radix scutellariae flavone extract and the physical mixture of Sichuan blackberry lily radix scutellariae flavone extract in other proportions, and are also better than those of the Sichuan blackberry lily flavone extract and the Sichuan blackberry lily radix scutellariae flavone extract with the same crude drug amount. The invention also provides a preparation method of the Sichuan blackberry lily scutellaria flavonoid extract, which has strong practical application value and is easy to popularize and use.
Description
Technical Field
The invention particularly relates to a Sichuan blackberry lily scutellaria baicalensis flavone extract, and a preparation method and application thereof.
Background
The Scutellariae radix is dried root of Scutellaria baicalensis Georgi of Labiatae, has bitter and cold nature, has effects of clearing heat, eliminating dampness, clearing pathogenic fire and removing toxic substance, and can be used for treating damp warmth, summer dampness, chest distress, nausea, damp heat, abdominal fullness, dysentery, jaundice, cough due to lung heat, hyperpyrexia, polydipsia, hematemesis, etc. Rhizoma Belamcandae is dry rhizome of Belamcanda chinensis (L) DC of Iridaceae, has bitter and cold nature, has effects of clearing heat and detoxicating, eliminating phlegm, and relieving sore throat, and can be used for treating stagnation of heat-toxin and phlegm-fire, sore throat, excessive phlegm and saliva, cough, asthma, etc.
Modern researches show that the main active ingredients of the scutellaria baicalensis are flavonoid ingredients mainly comprising baicalin, wogonoside, baicalein and wogonin, and the main active ingredients of the blackberry lily are isoflavone chemical ingredients mainly comprising blackberry lily glycoside, wild tectoridin, blackberry lily aglycone, wild tectoridine and sub-wild tectorigenin. The main active ingredients of the blackberrylily rhizome and the baical skullcap root are flavonoid compounds, the main pharmacological activities are anti-inflammatory, antibacterial, antiviral, antipyretic, analgesic, cough relieving and the like, and the pharmaceutical composition is clinically used for treating acute and chronic tonsillitis, sphagitis, upper respiratory tract infection and other symptoms.
Baikal skullcap root and blackberry lily decoction is recorded in volume twelve (throat prescription) from Yi Xie Ke Shu (money of medicine) code and is composed of Baikal skullcap root and blackberry lily and used for treating the fishy smell in throat caused by heat-toxicity in the two channels of intestines and stomach. The literature reports that the rhizoma polygonati buccal tablets prepared by the radix scutellariae rhizoma belamcandae decoction through the macroporous resin method can be used for acute pharyngitis and acute attack period of chronic pharyngitis, and also can be used for researching the fingerprint spectrum of flavonoid components in the radix scutellariae rhizoma belamcandae decoction, preliminarily researching the change rule of the components of the radix scutellariae rhizoma belamcandae decoction with time, and measuring the content of oroxylin A and sub-wild tectorigenin in the radix scutellariae rhizoma belamcandae decoction. The patent (CN 101185707B) discloses an anti-inflammatory and antiviral pharmaceutical composition, and a preparation method and application thereof: disclosed is an anti-inflammatory and antiviral pharmaceutical composition, which comprises total flavonoids of scutellaria and blackberry lily as active ingredients, and the curative effect is better than that of using the total flavonoids of scutellaria or blackberry lily alone.
Rhizoma Belamcandae is dry rhizome of Iris tectorum Maxim of Iridaceae, and has bitter and cold nature, and has effects of clearing away heat and toxic materials, eliminating phlegm, and relieving sore throat. Can be used for treating stagnation of heat-toxin and phlegm-fire, sore throat, excessive phlegm and saliva, cough and asthma. The patent (CN 100448450C) application of iris tectorum total flavone extract discloses the application of iris tectorum total flavone extract in preparing anti-inflammatory and antiviral drugs. The Sichuan blackberry lily flavone capsule (Chinese medicine standard Z20140008) is a hard capsule prepared from Sichuan blackberry lily flavone extract, and is used for treating sore throat, hoarseness, cough and the like caused by acute pharyngitis wind-heat syndrome and mild acute simple laryngitis wind-heat syndrome.
At present, no pharmacological active component compatible with rhizoma Belamcandae and Scutellariae radix and the report of the pharmacological active component for treating acute and chronic pharyngolaryngitis and upper respiratory infection diseases are reported.
Disclosure of Invention
The invention provides a rhizoma belamcandae scutellaria flavone extract, which is an extract prepared by taking rhizoma belamcandae and scutellaria as raw materials, extracting with water, separating and purifying an extracting solution, filtering and drying.
Further, the mass ratio of the Sichuan blackberry lily to the scutellaria baicalensis is 1: (0.1 to 9).
Furthermore, the mass ratio of the Sichuan blackberry lily to the baical skullcap root is 1: 1.
the invention also provides a preparation method of the Sichuan blackberry lily scutellaria flavone extract, which comprises the following steps:
weighing the medicinal materials according to the proportion, grinding into fine powder, extracting with water, filtering, loading the extract on a macroporous adsorption resin column, eluting with water and alcohol in sequence, collecting alcohol eluent, filtering, concentrating the filtrate under reduced pressure to obtain extract, and drying the extract under reduced pressure to obtain the Sichuan blackberry lily root scutellaria flavone extract.
Further, the water extraction is to use 10-30 times v/w of water for decoction and extraction for 2-3 times, and each time lasts for 1-2 hours; the step of eluting with water and alcohol sequentially is that water with the amount of 1-3 times of v/w resin is used for eluting, and then 60-100% ethanol with the amount of 5-7 times of v/w resin is used for eluting.
Further, the water extraction is to use 20 times of v/w of water for decoction and extraction for 3 times, and each time is 1 h; the elution with water and ethanol in sequence is that the elution is carried out by using water with 2 times of resin amount by v/w, and then the elution is carried out by using ethanol with 6 times of resin amount by v/w.
Further, the macroporous adsorbent resin is D101Macroporous adsorption resin, D101The dosage of the macroporous adsorbent resin is 3 times of that of the medicinal materials.
Further, said D101Soaking the macroporous adsorption resin in a 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until the pH value of the effluent is 7, draining, soaking in a 5% hydrochloric acid solution for 8-12 h, draining, and washing with running water until the pH value of the effluent is 7.
Further, the temperature of the reduced pressure drying was 60 ℃.
The invention also provides application of the Sichuan blackberry lily scutellaria flavone extract in preparing anti-inflammatory drugs.
The invention also provides application of the Sichuan blackberry lily scutellaria flavone extract in preparing an analgesic drug.
The invention also provides application of the Sichuan blackberry lily scutellaria flavone extract in preparing a cough relieving medicine.
The invention finally provides a preparation containing the Sichuan blackberry lily scutellaria flavone extract, which is prepared by taking the Sichuan blackberry lily scutellaria flavone extract as an effective component and adding pharmaceutically acceptable auxiliary materials.
Further, the preparation is an oral preparation or an injection.
The Sichuan blackberry lily root and baical skullcap root flavone extract is added with a pharmaceutically acceptable carrier to prepare different medicinal preparations, wherein the injections comprise freeze-dried powder injection, tablets and injection, and the oral preparations comprise powder, granules, capsules, pills, oral solution, nasal drops, spray and the like, and the tablets comprise: common compressed tablets, chewable tablets, effervescent tablets, multilayer tablets, sustained release tablets, controlled release tablets, coated tablets, dispersible tablets, buccal tablets, sublingual tablets and the like; the pill includes dripping pill, buccal dripping pill, pellet, etc. The capsule comprises: hard capsule, soft capsule, enteric capsule, sustained release capsule, microcapsule, etc.
The Chuanbelamcanda chinensis baikal skullcap root flavone extract has the functions of resisting inflammation, easing pain and relieving cough better than the physical mixture of the Chuanbelamcanda chinensis baikal skullcap root flavone extract and the Chuanbelamcanda chinensis baikal skullcap root flavone extract in different proportions and also better than the blackberrylily shoot rhizome baikal skullcap root flavone extract and the blackberrylily shoot rhizome baikal skullcap root flavone extract with the same crude drug amount.
Experiments prove that when the Sichuan blackberry lily and the baical skullcap root are compatible, the obtained flavone extract is obviously higher than the obtained flavone extract when the Sichuan blackberry lily and the baical skullcap root are in the same amount or the obtained flavone extract is extracted independently, and particularly when the Sichuan blackberry lily and the baical skullcap root are compatible in a ratio of 1:1, the Sichuan blackberry lily and the baicalin in the extract have the highest transfer rate and the maximum extract yield because the baical skullcap root contributes to the solubilization of the Sichuan blackberry lily. The Sichuan blackberry lily scutellaria flavone extract and the preparation method thereof have strong practical application value and are easy to popularize and use.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 ultraviolet absorption spectrum of Chuanbelong dried Scutellariae radix Brass extract
FIG. 2 shows the identification of Chuanbelamcanda baicalensis flavone extract (Chuanbelamcanda baicalensis: 1) (from left to right, Chuanbelamcanda baicalensis extract, Chuanbelamcanda chinensis contrast medicinal material, Scutellaria baicalensis contrast medicinal material, tectoridin and baicalin)
FIG. 3 shows the identification of Chuanbelamcanda baicalensis flavone extract (Chuanbelamcanda rhizome: radix Scutellariae 1:1) (from left to right, Chuanbelamcanda rhizome extract, Chuanbelamcanda rhizome reference medicinal material, radix Scutellariae reference medicinal material, blackberry lily aglycone, baicalein)
FIG. 4 shows a comparative characteristic spectrum (Peak 2 (S): belamcandin, Peak 3: tectoridin B, Peak 5: tectoridin A, Peak 6: wild tectoridin, Peak 7: baicalin, Peak 8: norwogonoside, Peak 11: oroxylin A glycoside, Peak 12: wogonoside, Peak 13: belamcandin, Peak 14: tectorigenin B, Peak 15: tectorigenin A, wild tectorigenin, Peak 16: baicalein, Peak 18: wogonin)
Detailed Description
Example 1 preparation of Chuanbelamcanda baicalensis flavone extract (I)
Decocting rhizoma Belamcandae coarse powder 100g and Scutellariae radix coarse powder 900g in boiling water 20 times for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking the macroporous adsorption resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until the pH value of the effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining,washing with running water until the pH of the effluent is 7, to obtain D)101Washing the resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying the extract at 60 deg.C under reduced pressure to obtain rhizoma Belamcandae radix Scutellariae flavone extract.
Sichuan blackberry lily scutellaria flavone extract (207.8 g) is brown yellow dry loose powder, lot number 180401.
Example 2 preparation of Chuanbelamcanda baicalensis flavone extract (C)
Decocting rhizoma Belamcandae coarse powder 300g and Scutellariae radix coarse powder 700g in boiling water 20 times for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorption resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract under reduced pressure at 60 deg.C to obtain rhizoma Belamcandae radix Scutellariae flavone extract.
Chuanbelamcanda rhizome flavone extract, rhizoma Belamcandae flavone powder, 208.5g in weight, lot number 180402.
Example 3 preparation of flavonoid extract from Chuanbelamcanda chinensis
Decocting rhizoma Belamcandae coarse powder 500g and Scutellariae radix coarse powder 500g in boiling water 20 times for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and applying the extractive solution to the treated product (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, and eluting with 6 times of resin amount of 70% ethanolCollecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying the extract at 60 deg.C under reduced pressure to obtain rhizoma Belamcandae radix Scutellariae flavone extract.
Sichuan blackberry lily root and baicalin extract (III) is brown yellow dry loose powder, the obtained amount is 212.3g, batch number is 180403.
Example 4 preparation of Chuanbelamcanda baicalensis flavone extract
Decocting rhizoma Belamcandae coarse powder 700g and Scutellariae radix coarse powder 300g in boiling water 20 times for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorption resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract under reduced pressure at 60 deg.C to obtain rhizoma Belamcandae radix Scutellariae flavone extract.
Sichuan blackberry lily root and baicalin flavone extract (4) is brown yellow dry loose powder, the obtained amount is 203.7g, and the batch number is 180404.
Example 5 preparation of Sichuan blackberry lily root scutellaria flavone extract (C. belamcanda root)
Decocting rhizoma Belamcandae coarse powder 900g and Scutellariae radix coarse powder 100g in boiling water 20 times for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract at 60 deg.C under reduced pressure to obtain rhizoma Belamcandae radix Scutellariae flavone extract.
Sichuan blackberry lily root scutellaria flavone extract (WU penetrate dry scutellaria flavone) is dry loose powder with brown yellow color, the yield is 200.2g, and the batch number is 180405.
The advantageous effects of the present invention are further described below by way of test examples.
Test example 1 preparation of flavone extract of Sichuan blackberry lily
Decocting rhizoma Belamcandae coarse powder 1kg in 20 times of boiling water for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract under reduced pressure at 60 deg.C to obtain rhizoma Belamcandae flavone extract.
The Sichuan blackberry lily flavone extract is yellow-brown dry loose powder, obtained 175.3g, lot number 180301.
Test example 2 preparation of flavone extract of scutellaria
Decocting Scutellariae radix coarse powder 1kg in 20 times of boiling water for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract under reduced pressure at 60 deg.C to obtain Scutellariae radix flavone extract.
The Scutellariae radix flavone extract is brown yellow dry loose powder with a yield of 185.6g, lot number 180302.
Test example 3 preparation of flavonoid extract of Belamcanda chinensis
1kg of blackberry lily coarse powder is taken,decocting in 20 times of boiling water for 3 times, each for 1 hr, filtering, mixing extractive solutions, and applying the extractive solution to the treated material (i.e. D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract under reduced pressure at 60 deg.C to obtain rhizoma Belamcandae flavone extract.
Belamcanda chinensis flavone extract is a yellow-brown dry loose powder, 60.5g, lot number 180303.
Test example 4 Belamcanda chinensis Baikal skullcap root flavone extract (Belamcanda chinensis: Scutellaria baicalensis 1:1)
Decocting rhizoma Belamcandae coarse powder 500g and Scutellariae radix coarse powder 500g in 20 times of boiling water for 3 times, each time for 1 hr, filtering, mixing extractive solutions, and loading onto treated material (D)101Soaking macroporous adsorbent resin in 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until pH of effluent is 7, draining, soaking in 5% hydrochloric acid solution for 8-12 h, draining, washing with running water until pH of effluent is 7, and getting final product D)101Macroporous adsorbent resin column (resin amount: medicinal material amount: 3:1, W/W), washing resin column with 2 times of resin amount of water, eluting with 6 times of resin amount of 70% ethanol, collecting ethanol eluate, filtering, recovering solvent from filtrate under reduced pressure to obtain extract, and drying extract at 60 deg.C under reduced pressure to obtain rhizoma Belamcandae radix Scutellariae flavone extract (rhizoma Belamcandae: radix Scutellariae 1: 1).
Belamcanda chinensis Baikal skullcap root flavone extract is brown yellow dry loose powder with the weight of 125g, batch number 180304.
Comparing examples 1 to 5 with test examples 1 to 4, it can be seen that: when the rhizoma Belamcandae and Scutellariae radix are combined, the water decoction is passed through D101The yield of the extract obtained by the macroporous adsorption resin purification process is obviously higher than that of the extract which is prepared by singly taking the rhizoma belamcandae, the rhizoma belamcandae and the scutellaria baicalensis in the same amount or taking the rhizoma belamcandae and the scutellaria baicalensis in a compatible manner as raw materials, when the rhizoma belamcandae and the scutellaria baicalensis are mixed in a ratio of 1:1 when the medicine is combined, the extract is obtained in the largest quantity.
Test example 5 measurement of Belamcanda chinensis glycoside and baicalin content in rhizoma Belamcandae, Scutellariae radix, rhizoma Belamcanda chinensis flavone extract, Scutellariae radix flavone extract, and rhizoma Belamcanda chinensis Scutellariae flavone extract
The content of belamcanda chinensis glycoside in the belamcanda chinensis and belamcanda chinensis flavone extract is measured according to the item of P41-42 'belamcanda chinensis' in the 2015 edition of Chinese pharmacopoeia.
The content determination of the baicalin in the scutellaria baicalensis and the scutellaria baicalensis flavone extract is carried out according to the item of P301-302 'scutellaria' in 2015 edition of Chinese pharmacopoeia.
Determination of contents of tectoridin and baicalin in Sichuan blackberry lily scutellaria baicalensis flavone extract
Determination of belamcandoside by high performance liquid chromatography (0512 in the four headquarters of the Chinese pharmacopoeia 2015)
Chromatographic conditions and system applicability tests adopt octadecylsilane chemically bonded silica as a filler; using methanol-0.02 mol/L sodium dihydrogen phosphate solution (pH value is adjusted to 3.0 by phosphoric acid) (35:65) as a mobile phase; the detection wavelength was 266 nm. The number of theoretical plates is not less than 2500 calculated according to the belamcanda chinensis glycoside peak.
Preparation of the tectoridin reference substance solution A proper amount of tectoridin reference substance is precisely weighed, and 70% methanol water solution is added to prepare a solution containing 0.05mg of tectoridin per 1mL, so as to obtain the tectoridin.
Preparing test solution by adding 12.5mg of rhizoma Belamcandae radix Scutellariae flavone extract into 25ml volumetric flask, adding 70% methanol water solution, ultrasonic treating to dissolve completely, cooling, diluting with 70% methanol water solution to desired volume, and shaking.
The determination method comprises respectively sucking 5 μ L of reference solution and sample solution, injecting into liquid chromatograph, and determining.
The product contains tectoridin (C) calculated on dry basis22H24O11) Not less than 10%.
Baicalin is determined by high performance liquid chromatography (China pharmacopoeia 2015 general rules 0512)
Chromatographic conditions and system applicability tests adopt octadecylsilane chemically bonded silica as a filler; methanol-water-phosphoric acid (47:53:0.2) is used as a mobile phase; the detection wavelength was 280 nm. The number of theoretical plates is not less than 2500 calculated by baicalin peak.
Preparation of baicalin reference substance solution A proper amount of baicalin reference substance is precisely weighed, and 70% methanol water solution is added to prepare a solution containing baicalin 0.10mg per 1 mL.
Preparing test solution by adding 12.5mg of rhizoma Belamcandae radix Scutellariae flavone extract into 25ml volumetric flask, adding 70% methanol water solution, ultrasonic treating to dissolve completely, cooling, diluting with 70% methanol water solution to desired volume, and shaking.
The determination method comprises respectively sucking 5 μ L of reference solution and sample solution, injecting into liquid chromatograph, and determining.
The product contains baicalin (C) calculated on dry basis21H18O11) Not less than 22%.
The results of the content measurement are shown in Table 1.
TABLE 1 measurement results of Belamcandin and baicalin content in sample
Amount of extract: the raw material medicine feeding amount is 1 kg; belamcandoside or baicalin amount: the extract amount is multiplied by the content of belamcandin (baicalin).
As can be seen from the above table: when the Sichuan blackberry lily is compatible with the scutellaria baicalensis, the flavone extract obtained by extraction has more components, and when the Sichuan blackberry lily and the scutellaria baicalensis are mixed according to the ratio of 1:1, the flavonoid components are more uniform.
Experimental example 6 Scutellaria baicalensis Georgi solubilization
The method comprises the steps of examining the solubilizing and solubilizing effects of scutellaria on rhizoma Belamcandae from the flavonoid extract yield of rhizoma Belamcandae and the transfer rate of belamcanda chinensis glycosides and baicalin
The transfer rates of belamcandin and baicalin in the samples were calculated according to the results of test example 5, and the results are shown in Table 2.
TABLE 2 conversion rates of Belamcanda chinensis glucoside and baicalin in the samples
| Sample (I) | Extract yield | Tectoridin transfer rate | Baicalin transfer Rate |
| Sichuan blackberry lily flavone extract | 175.3 | 87.27 | |
| Scutellaria baicalensis flavone extract | 185.6 | 95.35 | |
| Rhizoma Belamcandae radix Scutellariae flavone extract | 207.8 | 93.55 | 94.92 |
| Rhizoma Belamcandae radix Scutellariae flavone extract (rhizoma Belamcandae) | 208.5 | 93.59 | 95.24 |
| Sichuan blackberry lily scutellaria root flavone extract | 212.3 | 93.72 | 95.83 |
| Sichuan blackberry lily root and baicalin extract | 203.7 | 90.49 | 95.29 |
| Sichuan blackberry lily scutellaria root flavone extract (fifthly) | 200.2 | 88.93 | 94.63 |
The tectoridin or baicalin transfer rate, taking the tectoridin transfer rate in the extract of scutellaria baicalensis chuanensis as an example, is calculated as follows:
as can be seen from the above table, the flavonoid extracts of the Sichuan blackberry lily and the baical skullcap root are obtained in larger amounts than the same amount of the Sichuan blackberry lily or the baical skullcap root flavonoid extracts, which proves that the Sichuan blackberry lily and the baical skullcap root have the cosolvent and cosolvent phenomena; observed from the transfer rate of baicalin, the transfer rate of baicalin in the Sichuan blackberry lily baicalein extract and the baicalin in the baicalin extract is almost unchanged, which proves that the Sichuan blackberry lily does not have solubilizing and dissolving-assisting effects on the baical skullcap root; observed from the blackberry lily glycoside transfer rate, the blackberry lily glycoside transfer rate in the blackberry lily scutellaria flavone extract is higher than that in the blackberry lily flavone extract, and the scutellaria is proved to have the functions of solubilizing and dissolving; the best result is obtained when the ratio of the Sichuan blackberry lily to the scutellaria baicalensis is 1:1 by integrating the extract yield and the tectoridin transfer rate.
The method comprises the steps of preparing a Sichuan blackberry lily flavone extract, a baicalein extract, a Sichuan blackberry lily baicalein extract (I) - (V), a Sichuan blackberry lily flavone extract and a baicalein extract according to the proportion of 1:9, 3:7, 5:5, 7:3 and 9:1 respectively to prepare physical mixtures, weighing 1.0g of each sample, adding 50ml of boiling water respectively, heating for slightly boiling for 1 minute, cooling to room temperature, transferring to a 50ml volumetric flask, adding water to a constant volume until the volume is scaled, shaking uniformly, and standing overnight. The dissolution was observed, the solution shaken and dried with a weighed G4 sintered glass funnel, filtered, dried at 60 ℃ under reduced pressure to constant weight, weighed and the weight of the insoluble material calculated, the test results are shown in table 3.
TABLE 3 solubilizing and solubilizing effects of Scutellaria baicalensis on Szechwan blackberry lily
As can be seen from the above table, the scutellaria has the solubilizing and dissolving-assisting function to the belamcanda chinensis, and the solubility of the scutellaria flavone extract of the belamcanda chinensis is higher than that of the corresponding physical mixture of the belamcanda chinensis and the scutellaria extract.
Test example 7 identification of flavonoid extract from Chuanbelamcanda chinensis Baical (Chuanbelamcanda chinensis Baical 1:1)
(1) About 25mg of the product was taken, placed in a 50ml volumetric flask, dissolved and diluted to the mark with 70% ethanol, and shaken up to obtain solution A (0.5 mg/ml). Precisely sucking 1ml of the solution A into a 50ml volumetric flask, diluting with 70% ethanol, fixing the volume to the scale, and shaking up to obtain solution B. And B, performing ultraviolet-visible spectrophotometry (0401 in the four parts of the pharmacopoeia 2015 edition), scanning in a wavelength range of 200-400 nm by taking 70% ethanol as a blank, recording a spectrogram, and obtaining maximum absorption at 272 +/-2 nm.
(2) Taking appropriate amount of the product, adding methanol to make into solution containing 1mg per 1ml as test solution. Taking Sichuan blackberry lily control medicinal material and baical skullcap root control medicinal material 0.1g respectively, adding 10ml of methanol, carrying out ultrasonic treatment for 30 minutes, and filtering to obtain a control solution. And adding methanol to appropriate amount of tectoridin and baicalin as control solution containing 0.2mg per 1 ml. Performing thin layer chromatography (0401 in the four parts of the pharmacopoeia 2015 edition) by suckingThe five solutions are respectively spotted in 5 mul on the same silica gel GF254Developing on the thin layer plate with chloroform-methanol-formic acid (10: 2: 0.1) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm). Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the control solution and the reference solution.
(3) Taking appropriate amount of the product, adding methanol to make into solution containing 1mg per 1ml as test solution. Taking Sichuan blackberry lily control medicinal material and baical skullcap root control medicinal material 0.1g respectively, adding 10ml of methanol, carrying out ultrasonic treatment for 30 minutes, and filtering to obtain a control solution. And adding methanol to appropriate amount of rhizoma Belamcandae aglycone and baicalein as control solution containing 0.2mg per 1 ml. Performing thin layer chromatography (0401 in the four parts of the pharmacopoeia 2015 edition), sucking 5 μ l of the above five solutions, and adding onto the same silica gel GF254Developing the thin layer plate with toluene-ethyl acetate-methanol-formic acid (10: 3: 1: 0.5) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (254 nm). Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the control solution and the reference solution.
The ultraviolet spectrogram and the thin-layer chromatogram map are shown in figures 1-3.
Experimental example 8 characteristic chromatogram of Chuan blackberry lily scutellaria flavone extract (Chuan blackberry lily: scutellaria baicalensis 1:1)
The measurement is carried out according to high performance liquid chromatography (China pharmacopoeia 2015 edition of the general rules 0512 in four parts).
The chromatographic condition and the system applicability test use octadecylsilane bonded silicon as a filler; using methanol as a mobile phase A and 0.02mol/L sodium dihydrogen phosphate solution (pH value is adjusted to 3.0 by phosphoric acid) as a mobile phase B, and performing gradient elution according to the specification in the following table; the detection wavelength was 272 nm. The number of theoretical plates is not less than 2500 calculated according to the belamcanda chinensis glycoside peak.
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～35 | 35 | 65 |
| 35～45 | 48 | 52 |
| 45～47 | 70 | 30 |
Preparation of reference substance solution A proper amount of tectoridin reference substance is precisely weighed, and 70% methanol is added to make into solution containing 50 μ g per 1 ml.
Preparation of test solution 12.5mg of the product is precisely weighed, placed in a 25ml measuring flask, added with a proper amount of 70% methanol, ultrasonically treated (power 400W, frequency 58KHz) for 10 minutes, cooled, fixed to a certain volume, and shaken uniformly to obtain the product.
The determination method comprises precisely sucking 5 μ l of reference solution and sample solution respectively, injecting into liquid chromatograph, and determining.
There should be 19 characteristic peaks in the sample characteristic map (figure 4), the peak corresponding to the reference peak is the S peak, the relative retention time of each characteristic peak and the S peak is calculated, and the relative retention time should be within + -5% of the specified value. The specified values are: 0.939 (peak 1), 1.000[ peak 2(S) ], 1.063 (peak 3), 1.147 (peak 4), 1.237 (peak 5), 1.275 (peak 6), 1.476 (peak 7), 1.722 (peak 8), 1.789 (peak 9), 1.834 (peak 10), 1.884 (peak 11), 1.978 (peak 12), 2.172 (peak 13), 2.233 (peak 14), 2.341 (peak 15), 2.505 (peak 16), 2.663 (peak 17), 2.737 (peak 18), 2.810 (peak 19).
Test example 9 Effect of the drug of the present invention on swelling of mouse auricle caused by Paralyne
150 mice with the weight of 18-22 g are taken, the male and female halves are randomly divided into 15 groups according to sex and weight, and are respectively perfused with a physical mixture consisting of Sichuan blackberry lily flavone extract, baical skullcap root flavone extract, blackberry lily baical skullcap root flavone extract, Sichuan blackberry lily baical skullcap root flavone extract (I) to (V), Sichuan blackberry lily flavone extract and baical skullcap root flavone extract according to the proportion of 1:9, 3:7, 5:5, 7:3 and 9:1, and a blank control group ig equal volume of 1% tragacanth solution. The above groups are continuously administrated for 6 days, after administration for 30min on the 6 th day, the right ear of each mouse is coated with 0.1ml of inflammation-causing modeling, after 4 hours, the mouse is pulled off the cervical vertebra to be killed, the auricles on the two sides of the mouse are immediately cut off, ear discs are respectively punched on the same part by a puncher with the diameter of 8mm, the mouse is weighed by an electronic balance, the weight of the right ear of each mouse minus the weight of the left ear is taken as an index of swelling degree, and the swelling degrees of a control group and an administration group are compared and statistically processed. The results are shown in Table 4.
TABLE 4 Effect of the drug of the present invention on swelling of mouse auricle by Paralyne (X Shi SD)
Dosage of belamcanda chinensis flavone extract: the same is true for the calculation of the yield converted into the same weight of medicinal materials.
Dose of blackberry lily scutellaria flavone extract: the same is true for the calculation of the yield converted into the same weight of medicinal materials.
As can be seen from the above table, the medicament (Chuanbelamcanda baicalensis flavone extract ③) has obvious inhibiting effect on mouse auricle swelling caused by dimethylbenzene, and is stronger than other groups, namely when the ratio of the Chuanbelamcanda chinensis to the baical skullcap root is 1:1, the effect of the total flavone extract obtained by decocting the medicinal materials on resin is the best.
Test example 10 Effect of the drug of the present invention on mouse Cotton boll granuloma
150 mice with the weight of 18-22 g are taken, the male and female parts are divided into 15 groups randomly according to sex and weight, the chest of the mice is disinfected by iodine tincture, a small opening is cut on the chest after the iodine of a 70% alcohol cotton ball is removed, 5mg of autoclaved cotton ball is implanted into the subcutaneous axillary part from the cut by an ophthalmic forceps, and then the skin is sutured immediately. The administration is started from the day of surgery, 12 administration groups are respectively administered with 0.5g/kg dosage ig, and a control group ig is dosed with distilled water with the same volume once a day. The above groups were administered continuously for 7 days, and after administration for 1 hour on day 8, the mice were sacrificed by neck-breaking, the implanted cotton ball was taken out together with the surrounding connective tissue, the adipose tissue was removed, dried in an oven at 60 ℃ for 12 hours, and weighed on an electronic balance. Subtracting the original weight of the cotton ball to obtain the weight of granuloma, calculating according to mg/10g · bw, and carrying out comparison and statistical treatment among groups. The results are shown in Table 5.
TABLE 5 Effect of the drugs of the present invention on mouse Cotton boll granuloma (X Shi SD)
From the above table, it can be seen that the drug (Chuan blackberry lily scutellaria flavone extract) of the invention has significant inhibition effect on mouse cotton ball granuloma, and is stronger than other groups, that is, when the ratio of Chuan blackberry lily to scutellaria is 1:1, the effect of the total flavone extract obtained by decocting the drugs with resin is the best.
Test example 11 analgesic Effect of the drug of the present invention
150 mice with the weight of 18-22 g are taken, the male and female halves are randomly divided into 15 groups according to sex and weight, ig is respectively administrated (distilled water with the same volume is given to a control group), 0.5 percent HAC0.2m1/mouse is ip after 60 minutes of administration, and the body twisting frequency within 15 minutes is observed. And carrying out comparative statistics on the results. The results are shown in Table 6.
TABLE 6 analgesic Effect of the present invention on mice (writhing method) (X native SD)
As can be seen from the above table, the drug (Chuanbelamcanda baicalensis flavone extract ③) of the invention has obvious analgesic effect, and is stronger than other groups, namely when the ratio of the Chuanbelamcanda rhizome to the baical skullcap root is 1:1, the effect of the total flavone extract obtained by decocting the resin is the best.
Test example 12 antitussive Effect of the drug of the present invention
Taking 150 mice with the weight of 18-22 g and each half of the mice in male and female, randomly dividing the mice into 15 groups according to sex and weight, respectively administering the medicines for 3 days in ig mode (the control group is administered with distilled water with the same volume), respectively placing the mice into an inverted 500ml beaker after 40 minutes of final administration, injecting 0.15 ml/piece of concentrated ammonia water into the beaker, fumigating the mice for 15 seconds by ammonia gas, taking out the mice, counting the cough frequency of the mice within 2 minutes, and carrying out statistical treatment on the results. The results are shown in Table 7.
TABLE 7 antitussive effect of the inventive drugs on mice (X native SD)
As can be seen from the above table, the drug (Chuanbelamcanda baicalensis flavone extract. c.) of the invention has obvious cough relieving effect, and is stronger than other groups, namely when the ratio of Chuanbelamcanda and baical skullcap root medicinal materials is 1:1, the effect of the total flavone extract obtained by decocting the resin is the best.
In conclusion, when Chuan she gan and Huang Qin are combined, the water decoction is passed through D101The yield of the extract obtained by the macroporous adsorption resin purification process is obviously higher than the yield of the extract obtained by the same amount and prepared from the rhizoma Belamcandae, the rhizoma Belamcandae and the radix Scutellariae alone or the rhizoma Belamcandae and the radix Scutellariae in a compatible manner as raw materials, when the rhizoma Belamcandae and the radix Scutellariae are mixed by a ratio of 1:1 when the medicine is combined, the extract is obtained in the largest quantity. Proved by experiments, the Sichuan blackberry lily root-baicaleinThe anti-inflammatory, analgesic and antitussive effects of the extract are obviously better than that of the single rhizoma Belamcandae flavone extract, the single Scutellaria baicalensis flavone extract and the physical mixture of the rhizoma Belamcandae and the single Scutellaria baicalensis flavone extract in various proportions, and the extract is also stronger than the rhizoma Belamcandae flavone extract and the single rhizoma Belamcandae and Scutellaria baicalensis flavone extract with the same crude drug amount, and has practical application value.
Claims (8)
1. A Sichuan blackberry lily scutellaria flavone extract is characterized in that: the weight ratio of the components is 1:1, grinding rhizoma ligustici wallichii and scutellaria baicalensis into fine powder, decocting and extracting for 2-3 times by using water with the amount of 10-30 times v/w of medicinal materials, each time for 1-2 hours, filtering, and loading an extracting solution on a container D101And (3) eluting the macroporous adsorption resin column with water with the amount of 1-3 times v/w of the resin, then eluting with 60-100% ethanol with the amount of 5-7 times v/w of the resin, collecting ethanol eluent, filtering, concentrating the filtrate under reduced pressure to obtain extract, and drying the extract under reduced pressure to obtain the Sichuan blackberry lily root baical skullcap root flavone extract.
2. The extract of claim 1, wherein: the water extraction is to use 20 times v/w of water for decoction and extraction for 3 times, and each time lasts for 1 hour; the amount of water elution is 2 times of the amount of v/w resin, the concentration of ethanol elution is 70%, and the amount of ethanol elution is 6 times of the amount of v/w resin.
3. The extract of claim 1, wherein: said D101The dosage of the macroporous adsorption resin is 3 times of that of the medicinal materials; the temperature of the reduced pressure drying was 60 ℃.
4. The extract of claim 3, wherein: said D101Soaking the macroporous adsorption resin in a 5% NaOH ethanol solution for 8-12 h, draining, washing with running water until the pH value of the effluent is 7, draining, soaking in a 5% hydrochloric acid solution for 8-12 h, draining, and washing with running water until the pH value of the effluent is 7.
5. A preparation containing the extract as claimed in any one of claims 1 to 4, which is prepared by using Sichuan blackberry lily scutellaria flavone extract as an active ingredient and adding pharmaceutically acceptable auxiliary materials.
6. The formulation of claim 5, wherein the formulation is an oral formulation.
7. The preparation of claim 6, wherein the oral preparation is a paste, a pill, an oral liquid, a powder, a tablet, a granule or a capsule.
8. Use of the extract according to any one of claims 1 to 4 for the preparation of a medicament for anti-inflammatory, analgesic and/or antitussive effect.
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