CN116077554B - Preparation method of Guanxinning composition - Google Patents

Preparation method of Guanxinning composition Download PDF

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CN116077554B
CN116077554B CN202211509444.9A CN202211509444A CN116077554B CN 116077554 B CN116077554 B CN 116077554B CN 202211509444 A CN202211509444 A CN 202211509444A CN 116077554 B CN116077554 B CN 116077554B
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guanxinning
percolate
preparation
solution
composition
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CN116077554A (en
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李响明
李菲
杨琴
郑国成
姜国志
刘铁军
李振江
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HEBEI SHINEWAY PHARMACEUTICAL CO Ltd
Yunnan Shenwei Shipurui Pharmaceutical Co ltd
Shenwei Pharmaceutical Group Co Ltd
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HEBEI SHINEWAY PHARMACEUTICAL CO Ltd
Yunnan Shenwei Shipurui Pharmaceutical Co ltd
Shenwei Pharmaceutical Group Co Ltd
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    • A61K36/236Ligusticum (licorice-root)
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention provides a preparation method of a Guanxinning composition, which belongs to the technical field of traditional Chinese medicine preparations, and the preparation method is that red sage root and szechuan lovage rhizome are extracted by an ethanol aqueous solution with the concentration of 80-85wt% through a percolation method, and percolate and dregs are obtained; treating the percolate to obtain percolate; the dregs are treated, and the obtained decoction filtrate is mixed with the percolate to obtain a mixed solution; the mixed solution is adopted to prepare the Guanxinning composition. The invention adopts ethanol water solution with specific concentration and adopts a percolation method to extract, so that the effective components of salvianolic acid (especially salvianolic acid B), tanshinone and ferulic acid contained in the salvia miltiorrhiza and the ligusticum wallichii can be effectively reserved, and the effective components are not degraded, thereby improving the content of the effective components in the Guanxin composition.

Description

Preparation method of Guanxinning composition
Technical Field
The invention relates to a traditional Chinese medicine preparation, in particular to a preparation method of a Guanxinning composition.
Background
The coronary heart disease relieving medicine is a compound traditional Chinese medicine preparation which is composed of red sage root and szechuan lovage rhizome and has the effects of activating blood circulation to dissipate blood stasis, promoting blood circulation to nourish heart, regulating qi and relieving pain. Pharmacological studies show that the coronary heart disease treating injection has the functions of dilating coronary artery, promoting coronary collateral circulation, accelerating the repair of ischemic myocardium, protecting ischemic and anoxic myocardium, and the like, and is clinically mainly used for treating cardiovascular and cerebrovascular diseases such as coronary heart disease, angina pectoris, cerebral embolism, and the like. The chemical components in red sage root are classified into water-soluble and fat-soluble. The water soluble components mainly comprise phenolic compounds, polysaccharides and pachyma, including salvianic acid, caffeic acid, rosmarinic acid, salvianolic acid, lithospermic acid and ethyl lithospermate, and protocatechuic aldehyde, protocatechuic acid, etc. The liposoluble component is mainly conjugated quinone and ketone compound, including tanshinone, cryptotanshinone, hydroxy tanshinone, methyl tanshinol, methine tanshinone, tanshinol, 3 alpha-hydroxy tanshinone IIA, nortanshinone, tanshinol, and tanshinol. The rhizoma Ligustici Chuanxiong mainly contains volatile oil compounds such as ligustilide, 3-butylphthalide, butylphthalide and caryophyllene; alkaloids such as ligustrazine and choline; organic acids such as ferulic acid, sirtuin, rhein, palmitic acid, chrysophanol, and caffeic acid.
The existing method for preparing the Guanxinning mainly comprises the steps of removing macromolecular substances such as protein, pectin and the like through water decoction and alcohol precipitation, removing tannins through acid-base treatment or removing tannins through macroporous resin, and then decoloring, adding auxiliary materials and the like to prepare the preparation.
However, because the chemical components of salvianolic acid (especially salvianolic acid B), tanshinone, ferulic acid and the like contained in the red sage root and the ligusticum wallichii are easy to degrade when heated in the water decoction process, the content of the salvianolic acid in the water decoction is affected, and the drug effect is further affected; meanwhile, volatile oil compounds in the ligusticum wallichii volatilize along with the temperature rise in the water decoction process, so that the curative effect of the guanxinning is further affected; and because part of the effective components are fat-soluble compounds, the fat-soluble compounds are extracted by a water decoction mode, the extraction rate of the fat-soluble compounds is low, and the curative effect of the Guanxin is also influenced.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a Guanxinning composition.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method of preparing a perhexiline composition, the method comprising the steps of:
extracting Saviae Miltiorrhizae radix and rhizoma Ligustici Chuanxiong with 80-85wt% ethanol water solution by percolation method to obtain percolate and residue;
treating the percolate to obtain percolate;
the dregs are treated, and the obtained decoction filtrate is mixed with the percolate to obtain a mixed solution;
the mixed solution is adopted to prepare the Guanxinning composition.
Further, the treatment mode of the percolate is that after the percolate is concentrated, gelatin solution with the weight percent of 4 percent is dripped to remove tannins, and the percolate is obtained by refrigerating and filtering.
Further, the density of the percolate after concentration is 1.15-1.20.
Further, in the treatment process of the percolate, the refrigerating time is more than 24 hours.
Further, the process of preparing the guan Xin ning composition by the mixed solution is that the mixed solution is ultrafiltered, the pH value is regulated, and the guan Xin ning composition is obtained by preparation treatment of the guan Xin ning solution.
Further, the weight ratio of the red sage root to the ligusticum wallichii is 1:1;
after ultrafiltration, the pH value is regulated to 5.5-6.0.
Further, the preparation treatment is to take a Guanxinning solution to prepare a liquid preparation or a solid preparation;
the liquid preparation comprises but is not limited to injection, transfusion or oral liquid;
the solid formulations include, but are not limited to, granules, tablets, capsules or pills.
Further, the extraction time of the percolation method is 4-6 hours.
Further, the treatment process of the dregs is to take dregs and decoct with water for 2 times, each time for 1-1.5 hours, combine decoctions, filter, concentrate, add ethanol until the alcohol content is 85%, cool and filter, concentrate filtrate again until the relative density is 1.15-1.20, add gelatin solution of 4wt% to remove tannins, cool and filter, concentrate filtrate at 70 ℃ to obtain fluid extract with the relative density of 1.10-1.15, adjust pH value to 2-3 with hydrochloric acid, cool and filter, and obtain the decoction filtrate.
Further, when the dregs are decocted, the water is 4 to 6 times of the weight of the red sage root or the szechuan lovage rhizome;
the decoction is mixed and filtered, and then concentrated until the relative density is 1.16-1.26.
The preparation method of the Guanxinning composition has the beneficial effects that:
the invention adopts ethanol water solution with specific concentration to extract by percolation method, can effectively keep the effective components of salvianolic acid (especially salvianolic acid B), tanshinone and ferulic acid contained in the red sage root and the ligusticum chuanxiong rhizome to be extracted without degradation, thereby improving the content of the effective components in the guanxinning composition;
the invention adopts ethanol water solution with specific concentration to carry out diacolation extraction, can effectively extract liposoluble effective components such as tanshinone, cryptotanshinone, ligustilide, butenyl phthalide and the like, and further improves the curative effect of the Guanxin composition;
the invention can effectively extract volatile oil compounds (such as ligustilide, butenyl phthalide and the like) contained in the ligusticum wallichii by adopting ethanol water solution with specific concentration for diacolation extraction, thereby preventing the volatile oil compounds from volatilizing;
the invention adopts ethanol water solution with specific concentration to carry out diacolation extraction, which can inhibit macromolecular substances such as protein, polysaccharide and the like from being dissolved in diacolation liquid, thereby reducing the amount of impurities required to be treated in the alcohol precipitation process;
according to the invention, 4wt% gelatin solution is dripped into the percolate (or liquid obtained after decoction alcohol precipitation), so that the gelatin solution can fully form precipitation with tannins in the percolate (or liquid obtained after decoction alcohol precipitation) to remove the tannins, the tannins treatment process is simplified, and meanwhile, the decomposition of substances such as salvianolic acid (especially salvianolic acid B), protocatechol, ferulic acid, and deluxe acid caused by pH change in the process of removing the tannins by adding alkali is avoided;
the invention can effectively extract the water-soluble effective components such as senkyunolide and the like remained in the medicine residues after the completion of percolation by re-using water for decoction of the medicine residues;
the invention is regulated to a specific pH value in the preparation process, and can effectively maintain the stability of the substances such as salvianolic acid (especially salvianolic acid B), protocatechol, ferulic acid, and the like in the subsequent preparation process;
the invention has simple process route and convenient operation, and is suitable for industrial production.
Detailed Description
The following description of the technical solution in the embodiments of the present invention is clear and complete. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Example 1A method for preparing a Guanxinning composition
The embodiment is a preparation method of a Guanxinning composition, and the specific preparation process comprises the following steps in sequence:
1) Soaking 1000g of radix Salviae Miltiorrhizae and 1000g of rhizoma Chuanxiong in 85wt% ethanol water solution, percolating and extracting for 5 hr to obtain percolate and residues;
2) Concentrating the percolate to a relative density of 1.20, dropwise adding 4wt% gelatin solution under stirring until no precipitate is generated, refrigerating at 2deg.C for 24 hr, and filtering to obtain percolate;
decocting the residues with 5 times of water (the multiple of water is the multiple of the weight of radix Salviae Miltiorrhizae or rhizoma Chuanxiong, i.e. 5 kg) for 2 times, each time for 1h, mixing decoctions, filtering, concentrating the filtrate to relative density of 1.24, adding ethanol to ethanol content of 85%, refrigerating at 2deg.C for 24h (i.e. ethanol precipitation), filtering, concentrating the filtrate again to relative density of 1.20, dripping 4wt% gelatin solution until no precipitate is generated, refrigerating at 2deg.C for 24h, filtering, recovering ethanol from the filtrate until no ethanol smell, diluting with injectable water, refrigerating, filtering, concentrating the filtrate again at 70deg.C to obtain fluid extract with relative density of 1.15, adjusting pH to 2.5 with 10wt% hydrochloric acid, refrigerating, and filtering to obtain decoction filtrate;
3) Mixing the percolate and the decoction filtrate, ultrafiltering the obtained mixture (removing microorganism, heat source, etc.), and adjusting pH to 5.5 to obtain GUANXINNING solution, labeled as M1;
taking a Guanxin solution M1, fixing the volume to 1000mL, filling, sealing and sterilizing to obtain a Guanxin liquid preparation (marked as G1), wherein the Guanxin liquid preparation contains 38.7231mg/mL of salvianolic acid B, 0.9214mg/mL of tanshinone I, 1.3675mg/mL of tanshinone IIA, 1.3627mg/mL of ferulic acid, 0.7243mg/mL of cryptotanshinone, 37.9465mg/mL of ligustilide, 0.4798mg/G of protocatechuic aldehyde, 2.9614mg/mL of rosmarinic acid, 0.3971mg/mL of ligustrazine, 0.9215mg/G of senkyunolide I, 0.2627mg/G of senkyunolide H, 4.678 mg/G of senkyunolide A, 0.4896mg/mL of butenyl phthalide and 2.1mg/mL of tannins.
The content of the active ingredient in the Guanxinning liquid preparation G1 is detected according to the method in the content determination of the ingredient in Guanxinning 14 (Li Qingqing, zhang Jifen, modern salt chemical industry, period 6 of 12 months in 2019); the content of tannin is based on quality study of Guanxinning injection of different manufacturers (Li Xiangming, etc., modern Chinese medicine, volume 36, 2 nd stage of 2016, 03 month)
The guanxinning liquid preparation comprises but is not limited to injection, transfusion or oral liquid.
The GUANXINNING liquid preparation can also be prepared by adding other conventional adjuvants (such as correctant in oral liquid), metering volume to 1000mL, packaging, and sterilizing.
Alternatively, the guan Xin ning solution M1 is lyophilized to obtain guan Xin ning lyophilized powder, which is marked as D1.
The guanxinning freeze-dried powder D1 can also be prepared into other types of solid preparations such as granules, tablets, capsules or pills by adopting the conventional technology in combination with common auxiliary materials according to the types of the required preparations.
For example, in the preparation of granule, conventional adjuvants such as filler, wetting agent, disintegrating agent, and binder can be added; conventional processes such as wet granulation or dry granulation can be used in the preparation process.
In the process of preparing the tablet, conventional auxiliary materials such as filler, wetting agent, disintegrating agent, adhesive and the like can be added; the conventional processes of mixing, stamping and the like are adopted in the preparation process.
When preparing the capsule, conventional auxiliary materials such as filler, lubricant, disintegrating agent and the like can be added; conventional mixing, filling and other conventional processes can be adopted in the preparation process.
When preparing pill, adding conventional adjuvants such as lubricant, binder, and diluent; the preparation process can adopt conventional processes such as traditional molding method, general method and the like.
Examples 2 to 6 Process for the preparation of Guanxinning compositions
Examples 2 to 6 are each a process for the preparation of a composition of Coralline, which steps are substantially the same as in example 1, except for the process parameters, which are specified in Table 1:
table 1 list of process parameters in examples 2 to 6
The process steps and parameters of the other parts of examples 2 to 6 are the same as in example 1.
The Guanxinning solutions M2-M5 can be respectively added or not added with auxiliary materials to prepare liquid preparations, or respectively added or not added with auxiliary materials to prepare solid preparations.
Experimental example 1 comparative test
Comparative examples 1 to 6 are comparative tests of the preparation method of the Coralline composition in example 1, differing only in that:
percolating with 70wt% ethanol water solution to obtain GUANXINNING liquid preparation, labeled DG1, wherein salvianolic acid B24.3274 mg/mL, tanshinone I0.5431 mg/mL, tanshinone IIA0.8651mg/mL, ferulic acid 1.3626mg/mL, cryptotanshinone 0.3574mg/mL, ligustilide 18.1274mg/mL, protocatechuic aldehyde 0.2654mg/g, rosmarinic acid 2.9637mg/mL, ligustrazine 0.3985mg/mL, senkyunolide I0.9208 mg/g, senkyunolide H0.2636 mg/g, senkyunolide A3.1245mg/g, butenyl phthalide 0.3058mg/mL, and tannin 2.2mg/mL; it can be seen that decreasing the ethanol concentration in the aqueous ethanol solution results in decreased extraction of salvianolic acid B, tanshinone I, tanshinone IIA, cryptotanshinone, ligustilide, protocatechuic acid, senkyunolide A, and butenyl phthalide.
Percolating with 95wt% ethanol water solution to obtain GUANXINNING liquid preparation, wherein the preparation is marked as DG1, and the liquid preparation comprises salvianolic acid B35.7216 mg/mL, tanshinone I0.8124 mg/mL, tanshinone IIA 1.2607mg/mL, ferulic acid 1.0103mg/mL, cryptotanshinone 0.6892mg/mL, ligustilide 37.2463mg/mL, protocatechuic aldehyde 0.4214mg/g, rosmarinic acid 2.6385mg/mL, ligustrazine 0.2572mg/mL, senkyunolide I0.8153 mg/g, senkyunolide H0.2452 mg/g, senkyunolide A4.6572mg/g, butenyl phthalide 0.4932mg/mL, and tannin 2.1mg/mL; it can be seen that increasing the ethanol concentration in the ethanol aqueous solution resulted in a decrease in the extraction of salvianolic acid B, tanshinone I, tanshinone IIA, ferulic acid, cryptotanshinone, rosmarinic acid, ligustrazine, senkyunolide I, and senkyunolide H.
Concentrating the percolate and the filtrate after alcohol precipitation in comparative example 3 until the relative density is 1.05, adding 4wt% gelatin solution to obtain a Guanxinning liquid preparation, and marking as DG3, wherein salvianolic acid B38.6894mg/mL, tanshinone I0.9279 mg/mL, tanshinone IIA1.3652mg/mL, ferulic acid 1.3643mg/mL, cryptotanshinone 0.7205mg/mL, ligustilide 37.9458mg/mL, protocatechuic aldehyde 0.4783mg/g, rosmarinic acid 2.9598mg/mL, ligustrazine 0.3954mg/mL, ligustilide I0.9207 mg/g, ligustilide H0.2631 mg/g, ligustilide A4.6775mg/g, butenyl phthalide 0.4879mg/mL, tannin 3.1mg/mL; it can be seen that the content of each active ingredient is not changed obviously, the content of tannins is increased obviously, and the tannins can not be separated out completely probably due to the fact that the concentration of the solution is too low.
The percolate and the filtrate after alcohol precipitation in comparative example 4 are concentrated to 1.35, and then 4wt% gelatin solution is added to obtain a Guanxinning liquid preparation, and the Guanxinning liquid preparation is marked as DG4, wherein 36.2143mg/mL of salvianolic acid B, 0.8763mg/mL of tanshinone I, 1.3215mg/mL of tanshinone IIA, 1.3107mg/mL of ferulic acid, 0.7209mg/mL of cryptotanshinone, 36.1521mg/mL of ligustilide, 0.4123mg/g of protocatechuic aldehyde, 2.6954mg/mL of rosmarinic acid, 0.3438mg/mL of ligustrazine, 0.8709mg/g of senkyunolide, 0.2352mg/g of senkyunolide, 4.2745mg/g of senkyunolide A, 0.4198mg/mL of butenyl phthalide and 2.2mg/mL of tannins; it can be seen that the content of each active ingredient is reduced, and the concentration of the active ingredient is reduced probably because the active ingredient is separated out by the sediment coating in the process of removing tannins by adding gelatin due to the excessive concentration of the solution.
After ultrafiltration in the mixed solution in comparative example 5, the pH value is regulated to 7.0, and the obtained Guanxinning liquid preparation is marked as DG5, wherein 37.0123mg/mL of salvianolic acid B, 0.9201mg/mL of tanshinone I, 3682mg/mL of tanshinone IIA1, 1.3176mg/mL of ferulic acid, 0.7213mg/mL of cryptotanshinone, 36.8794mg/mL of ligustilide, 0.4339mg/g of protocatechuic aldehyde, 2.7253mg/mL of rosmarinic acid, 0.3968mg/mL of ligustrazine, 0.9232mg/g of senkyunolide I, 0.2614mg/g of senkyunolide H, 4.6798mg/g of senkyunolide A, 0.4789mg/mL of butenyl phthalide and 2.1mg/mL of tannin; it can be seen that the change of the pH value in the preparation process can cause the content of the effective components such as salvianolic acid (especially salvianolic acid B), protocatechuic acid, ferulic acid, and the like to be reduced to different degrees, possibly due to the degradation of the effective components to different degrees in the subsequent processes such as ultrafiltration, volume fixation, filling and the like.
The preparation process of comparative example 6 comprises decocting 1000g of Saviae Miltiorrhizae radix and 1000g of rhizoma Ligustici Chuanxiong with 8kg of water for three times, the first time for 2 hours, the second time and the third time for 1.5 hours respectively, mixing decoctions, filtering, concentrating the filtrate to obtain fluid extract with relative density of 1.24, adding ethanol to a content of 85%, refrigerating, filtering, adjusting pH of the filtrate to about 8.3 with 40% sodium hydroxide solution, refrigerating, filtering, recovering ethanol from the filtrate to no alcohol smell, diluting with injectable water to about 1000mL, refrigerating, filtering, concentrating the filtrate to fluid extract with relative density of 1.15 (70deg.C), adjusting pH with hydrochloric acid solution to 2.5, refrigerating, filtering, adjusting pH of the filtrate to 7.0 with 10% sodium hydroxide solution, heating and boiling for 30 min, adding appropriate amount of activated carbon, slightly cooling, filtering, refrigerating, ultrafiltering to adjust pH to 5.5, constant volume to 1000mL, bottling, and sterilizing to obtain GUANXINNING liquid preparation, marked as DG6, wherein salvianolic acid B25.3124 mg/mL, tanshinone I0.0023 mg/mL, tanshinone IIA 0.0037mg/mL, ferulic acid 1.0210mg/mL, cryptotanshinone 0.0015mg/mL, ligustilide 0.0024mg/mL, protocatechuic aldehyde 0.0712mg/g, rosmarinic acid 2.8124mg/mL, ligustrazine 0.3805mg/mL, senkyunolide I0.9205 mg/g, senkyunolide H0.2635mg/g, senkyunolide A0.0049mg/g, butenyl phthalide 0.0008mg/mL, and tannin 4.2mg/mL; it can be seen that the existing method of removing tannins by water alkali treatment can reduce the contents of salvianolic acid B, tanshinone I, tanshinone IIA, ferulic acid, cryptotanshinone, ligustilide, protocatechol, senkyunolide A and butenyl phthalide to different degrees, and the content of tannins is obviously increased, probably because part of fat-soluble active ingredients cannot be well extracted in the water extraction process, volatile ingredients volatilize along with the increase of the water extraction temperature, and easily degradable substances such as salvianolic acid (especially salvianolic acid B), tanshinone, ferulic acid and the like degrade to different degrees along with the increase of the temperature or the subsequent alkali addition to remove the tannins. Meanwhile, the removal effect of the alkali-added tannin is obviously poorer than that of the method.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (5)

1. A method of preparing a perhexiline composition, comprising the steps of:
extracting Saviae Miltiorrhizae radix and rhizoma Ligustici Chuanxiong with 80-85wt% ethanol water solution at a weight ratio of 1:1 by percolation method to obtain percolate and residue;
concentrating the percolate to a density of 1.15-1.20, dripping a gelatin solution with the weight percent of 4% to remove tannins, refrigerating, and filtering to obtain a percolate;
decocting the residues in water for 2 times, each time for 1-1.5 hours, mixing decoctions, filtering, concentrating to a relative density of 1.16-1.26, adding ethanol to an alcohol content of 85%, refrigerating, filtering, concentrating the filtrate again to a relative density of 1.15-1.20, adding a gelatin solution with a weight of 4% to remove tannins, refrigerating, filtering, concentrating the filtrate at 70 ℃ to obtain fluid extract with a relative density of 1.10-1.15 at 70 ℃, regulating the pH value to 2-3 with hydrochloric acid, refrigerating, and filtering to obtain a decoction filtrate;
mixing the decoction filtrate and the percolate to obtain a mixed solution;
and (3) taking the mixed solution for ultrafiltration, and then adjusting the pH value to 5.5-6.0, and treating the prepared Guanxin solution by a preparation to obtain the Guanxin composition.
2. The method for preparing a guanxinning composition according to claim 1, wherein the time of cold storage in the percolate treatment process is more than 24 hours.
3. The method for preparing the guanxinning composition according to claim 1, wherein the preparation treatment is to take a guanxinning solution to prepare a liquid preparation or a solid preparation.
4. The method for preparing a guanxinning composition according to claim 1 or 3, wherein the extraction time of the percolation method is 4-6 hours.
5. The method for preparing a guanxinning composition according to claim 1, wherein the water used for decocting the dregs is 4-6 times by weight of the root of red-rooted salvia or the rhizome of chuanxiong.
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