Preparation method of Goutongling tincture

Abstract

The application belongs to the technical field of medicine, and provides a preparation method of Goutongling tincture. The preparation method of the Goutongling tincture comprises the following steps: (1) washing, drying, crushing and soaking Artemisia rupestris L. in first ethanol with a concentration of 45-55%, then performing microwave extraction, and separating Artemisia rupestris L. residues and an extract; (2) uniformly mixing the Artemisia rupestris L. residues, dried ginger, myrrh and frankincense to obtain a premix, then performing percolation extraction on the premix with ethanol, collecting the last percolation liquid, and combining the percolation liquid with the extract to obtain 950 ml; (3) dissolving dragon's blood and borneol in 50 ml of ethanol, combining the ethanol solution with the percolation liquid and the extract, uniformly mixing, standing for 48 hours, filtering, and preparing 1000 ml, thereby obtaining the Goutongling tincture. The Goutongling tincture prepared by the preparation method can obviously improve the yield of effective components of the final product, improve the treatment effect, and reduce the treatment cycle.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of medicine, and particularly relates to a preparation method of Goutongling tincture. BACKGROUND

[0002] Goutongling tincture is a kind of external traditional Chinese medicine, and its main components include artemisia rupestris l., dried ginger, dragon's blood, frankincense, myrrh and borneol. The whole prescription of Goutongling tincture has the effects of warming meridians and dispelling cold, dispelling wind and activating blood, dredging collaterals and relieving pain. It can be used for treating lumbar and cervical spondylosis, osteoarthritis, scapulohumeral periarthritis and rheumatoid arthritis.

[0003] According to the page number Z19-142 and the standard number WS3-B-3645-98 in the 19th volume of Traditional Chinese Medicine Prescription of Ministry of Health, the prescription of Goutongling tincture is as follows: artemisia rupestris l. 80g, dried ginger 110g, dragon's blood 1.0g, frankincense 5.0g, myrrh 5.0g and borneol 1.5g. The preparation method is as follows: the above six components are ground into coarse powder, mixed, and subjected to percolation according to the percolation method (Appendix I0) under the item of flow extract and extract, using 50% ethanol as a solvent, collecting 950ml of percolate; the dragon's blood and borneol are dissolved in 50ml of ethanol, mixed with the above percolate, and then subjected to standing for 48 hours, filtering, and preparing 1000ml, thereby obtaining the product.

[0004] The above traditional preparation method has the problems of single extraction mode, long time consumption, low effective component yield and narrow effective component range. Generally, the dosage of Goutongling tincture is 10ml once, and the treatment is performed once a day. The medicine liquid is immersed on a bandage and applied to the affected area for 30-60 minutes. One treatment cycle is 20 days, the effect is slow, and the treatment cycle is long. SUMMARY

[0005] In view of the above problems in the prior art, the present application provides a preparation method of Goutongling tincture. The Goutongling tincture prepared by the preparation method can obviously improve the effective component yield of the final product, improve the treatment effect and reduce the treatment cycle.

[0006] In order to achieve the above purpose, the solution adopted by the present application is as follows:

[0007] The preparation method of the Goutongling tincture comprises the following steps: (1) washing, drying, and crushing Herba Artemisiae Scopariae, and then soaking the crushed Herba Artemisiae Scopariae in first ethanol with a concentration of 45-55%, and then performing microwave extraction, and then separating the residue of the Herba Artemisiae Scopariae and the extracted liquid; (2) mixing the residue of the Herba Artemisiae Scopariae, dried ginger, myrrh, and frankincense to obtain a premix, and then performing percolation extraction with ethanol, and then collecting the percolation liquid, and then combining the percolation liquid with the extracted liquid to obtain 950 ml; and (3) dissolving dragon's blood and borneol in 50 ml of ethanol, and then combining the ethanol solution with the percolation liquid and the extracted liquid, and then uniformly mixing the combined solution, and then standing for 48 hours, and then filtering to obtain 1000 ml of the Goutongling tincture.

[0008] The preparation method of the Goutongling tincture provided by the application has the following beneficial effects:

[0009] (1) The preparation method of the Goutongling tincture provided by the application can greatly improve the dissolution rate of alkaloids in the Herba Artemisiae Scopariae by performing microwave extraction on the Herba Artemisiae Scopariae, and then performing percolation extraction on the extracted liquid.

[0010] (2) The preparation method of the Goutongling tincture provided by the application can maximize the dissolution of the effective components in the Herba Artemisiae Scopariae by using the extracted liquid for percolation extraction. DETAILED DESCRIPTION

[0011] In order to make the purpose, technical scheme and advantages of the embodiments of the application clearer, the technical scheme of the embodiments of the application will be clearly and completely described below. If the specific conditions are not specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturers are used. If the manufacturers of the reagents or instruments are not specified, the conventional products that can be purchased in the market are used.

[0012] The preparation method of the Goutongling tincture provided by the embodiments of the application will be specifically described below.

[0013] The preparation method of the Goutongling tincture comprises the following steps:

[0014] (1) washing, drying, and crushing Herba Artemisiae Scopariae to a particle size of 0.5-1.0 cm, and then soaking the crushed Herba Artemisiae Scopariae in ethanol with a concentration of 45-55% according to a solid-liquid ratio of 80 g:100-200 ml for 4-6 hours, and then performing ultrasonic treatment on the Herba Artemisiae Scopariae at a power of 200-400 W for 25-30 minutes, and then performing microwave extraction at a temperature of 50-65 ℃, a microwave frequency of 720-950 MHz, and a microwave power of 540-630 W for 5-8 minutes, and then separating the residue of the Herba Artemisiae Scopariae and the extracted liquid.

[0015] Ultrasonic extraction method is a method of using cavitation effect, mechanical effect and thermal effect generated by ultrasonic to accelerate the release, diffusion and dissolution of effective components in cells. In the embodiment, Artemisia rupestris L. is further extracted in the above specific technical conditions by using ultrasonic-microwave combined method, so as to fully promote the dissolution of alkaloids in Artemisia rupestris L. in a short time.

[0016] (2) The residue of Artemisia rupestris L. is mixed with dry ginger, myrrh and frankincense to obtain a premix; then ethanol is used for percolation extraction, the flow rate of percolation is 5-7 ml / min, the percolation liquid is collected and combined with the extraction liquid to obtain 950 ml.

[0017] (3) Dragon's blood and borneol are dissolved in 50 ml of ethanol, combined with the percolation liquid and the extraction liquid, mixed, and then left to stand for 48 hours, filtered, and prepared into 1000 ml, thereby obtaining the tincture.

[0018] The features and performances of the present application are further described in detail in combination with the embodiments.

[0019] Embodiment 1

[0020] The present embodiment provides a preparation method of Goutalingle tincture, which comprises the following steps:

[0021] (1) Artemisia rupestris L. is washed, dried, and crushed to a particle size of 0.5 cm, soaked in 50% ethanol for 5 hours according to a solid-liquid ratio of 80 g:160 ml, then microwave extracted for 7 minutes under the conditions of a temperature of 58 ℃, a microwave frequency of 830 MHz, and a microwave power of 590 W, and the residue of Artemisia rupestris L. is separated from the extraction liquid;

[0022] (2) The residue of Artemisia rupestris L. is mixed with dry ginger, myrrh and frankincense to obtain a premix; then ethanol is used for percolation extraction, the flow rate of percolation is 6 ml / min, the percolation liquid is collected and combined with the extraction liquid to obtain 950 ml;

[0023] (3) Dragon's blood and borneol are dissolved in 50 ml of ethanol, combined with the percolation liquid and the extraction liquid, mixed, and then left to stand for 48 hours, filtered, and prepared into 1000 ml, thereby obtaining the tincture.

[0024] Embodiment 2

[0025] The present embodiment provides a preparation method of Goutalingle tincture, which comprises the following steps: the microwave extraction conditions are as follows: microwave extraction for 5 minutes under the conditions of a temperature of 65 ℃, a microwave frequency of 720 MHz, and a microwave power of 630 W; and the rest is the same as in Embodiment 1.

[0026] Embodiment 3

[0027] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: microwave extraction under the conditions of a temperature of 50 DEG C, a microwave frequency of 950 MHz, a microwave power of 540 W and microwave extraction for 8 min; and the rest is the same as in the embodiment 1.

[0028] Embodiment 4

[0029] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: (1) washing, drying and crushing Artemisia rupestris L. to a particle size of 0.8 cm, soaking the Artemisia rupestris L. in 50% ethanol according to a solid-liquid ratio of 80 g:160 ml for 5 h, then ultrasonically treating the Artemisia rupestris L. at a power of 300 W for 28 min, then microwave extracting under the conditions of a temperature of 58 DEG C, a microwave frequency of 830 MHz, a microwave power of 590 W and microwave extraction for 7 min, and separating Artemisia rupestris L. residues and an extract; and the rest is the same as in the embodiment 1.

[0030] Embodiment 5

[0031] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: ultrasonically treating the Artemisia rupestris L. at a power of 200 W for 30 min; and the rest is the same as in the embodiment 4.

[0032] Embodiment 6

[0033] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: ultrasonically treating the Artemisia rupestris L. at a power of 300 W for 25 min; and the rest is the same as in the embodiment 4.

[0034] Embodiment 7

[0035] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: the concentration of ethanol is 45%, and the percolation flow rate is 5 ml / min; and the rest is the same as in the embodiment 4.

[0036] Embodiment 8

[0037] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: the concentration of ethanol is 55%, and the percolation flow rate is 7 ml / min; and the rest is the same as in the embodiment 4.

[0038] Embodiment 9

[0039] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: the solid-liquid ratio of ethanol and Artemisia rupestris L. is 80 g:100 ml; and the rest is the same as in the embodiment 4.

[0040] Embodiment 10

[0041] The embodiment provides a preparation method of Goutongling tincture, which comprises the following steps: the solid-liquid ratio of ethanol and Artemisia rupestris L. is 80 g:200 ml; and the rest is the same as in the embodiment 9.

[0042] Comparative Example 1

[0043] The present comparative example provides a preparation method of Goutali tincture, comprising: (1) washing and drying Xueshuan Zhimu, crushing to a particle size of 0.8 cm, soaking in 50% ethanol according to a solid-liquid ratio of 80 g:160 ml for 5 h, then microwave extracting under the conditions of a temperature of 58 ℃, a microwave frequency of 830 MHz, and a microwave power of 590 W for 7 min, and separating Xueshuan Zhimu dregs and the extract; (2) mixing the Xueshuan Zhimu dregs, dry ginger, myrrh, and frankincense powders to obtain a premix; then performing percolation extraction with ethanol, and collecting the percolate at a flow rate of 6 ml / min, and combining the percolate with the extract to obtain 950 ml; (3) dissolving dragon's blood and borneol in 50 ml of ethanol, combining with the percolate and the extract, mixing uniformly, standing for 48 h, filtering, and preparing 1000 ml, to obtain the Goutali tincture.

[0044] Comparative Example 2

[0045] The present comparative example provides a preparation method of Goutali tincture, comprising: (1) washing and drying Xueshuan Zhimu, crushing to a particle size of 0.8 cm, soaking in 50% ethanol according to a solid-liquid ratio of 80 g:160 ml for 5 h, then ultrasonic treating Xueshuan Zhimu at a power of 300 W for 28 min, and separating Xueshuan Zhimu dregs and the extract; steps (2) and (3) are the same as comparative example 1.

[0046] Comparative Example 3

[0047] The present comparative example provides a preparation method of Goutali tincture, comprising: microwave extraction conditions are as follows: microwave extracting under the conditions of a temperature of 70 ℃, a microwave frequency of 680 MHz, and a microwave power of 650 W for 10 min; and the rest is the same as example 1.

[0048] Comparative Example 4

[0049] The present comparative example provides a preparation method of Goutali tincture, comprising: ultrasonic treating Xueshuan Zhimu at a power of 100 W for 40 min; and the rest is the same as example 4.

[0050] Comparative Example 5

[0051] The present comparative example provides a preparation method of Goutali tincture, comprising: the concentration of ethanol is 60%, and the percolation flow rate is 7 ml / min; and the rest is the same as example 4.

[0052] Comparative Example 6

[0053] The present comparative example provides a preparation method of Goutali tincture, comprising: in step (1), the ethanol and Xueshuan Zhimu are according to a solid-liquid ratio of 80 g:80 ml; and the rest is the same as example 4.

[0054] Experimental Example 1

[0055] Experimental Method: Experimental Method:

[0056] 190 rats were divided into normal group, model group, Goutling tincture group and administration groups 1-16 (corresponding to Examples 1-10 and Comparative Examples 1-6) with 10 rats in each group.

[0057] The administration was performed twice, once at 1 day before modeling and once immediately after modeling. The right hind foot of the rats in the normal group and the model group was soaked in 10 mL of normal saline, once every 5 minutes, for a total of 6 times, each time for 5 minutes. The right hind foot of the rats in the Goutling tincture group was soaked in 10 mL of Goutling tincture, once every 5 minutes, for a total of 6 times. The right hind foot of the rats in administration groups 1-20 was soaked in 10 mL of the combined drug solution provided by Examples 1-10 and Comparative Examples 1-6, once every 5 minutes, for a total of 6 times.

[0058] After 1 day of administration, the normal group was injected with an equal volume of normal saline, and the remaining groups were injected with 1% λ-carrageenan normal saline suspension subcutaneously in the middle of the right hind foot of the rats, with a volume of 0.1 mL per rat. Immediately after modeling, each group was administered again according to the above method. At 0.5, 1, and 2 hours after modeling, the foot volume of the rats in each group was measured using a foot volume meter.

[0059] Foot swelling (mL) = foot volume after injection - baseline volume;

[0060] Foot swelling inhibition rate (%) = (model group swelling - drug group swelling) / model group swelling x 100%.

[0061] Table 1

[0062]

[0063]

[0064] From the data in Table 1, it can be seen that Goutling tincture has a significant effect 1 hour after modeling administration, while administration groups 1-10 can significantly reduce the foot swelling of rats within 0.5 hours after modeling administration (p<0.05), indicating that the Goutling tincture prepared by the preparation method of Goutling tincture provided in Examples 1-10 has better and faster detumescence efficacy compared to the Goutling tincture prepared by the prior art.

[0065] Experimental Example 2

[0066] Experimental method: After 5h of modeling, the above rats were anesthetized with sodium pentobarbital and sacrificed. The subcutaneous tissue of the right hind toe of the rat was collected, temporarily stored in liquid nitrogen and then transferred to a-80°C refrigerator for storage. After homogenization of the tissue, the levels of TNF-a (pg·mL -1 ) and IL-1β (pg·mL -1 ) were detected by rat ELISA kit:

[0067] Table 2

[0068]

[0069]

[0070] From the data in Table 2, it can be seen that compared with the normal group, the contents of IL-1β and TNF-a in the model group were significantly increased, indicating that modeling caused obvious inflammatory reaction. Compared with the model group, drug group 1-10 had a significant inhibitory effect on the release of TNF-a and IL-1β (p<0.05), and the inhibitory effect was significantly better than that of Goutling Tincture group, indicating that the Goutling Tincture prepared by the preparation method of Goutling Tincture provided by 1-10 of the present application has more excellent anti-inflammatory effect than the Goutling Tincture prepared by the prior art.

[0071] Example 3

[0072] Experimental method:

[0073] 180 mice were divided into model group, Goutling Tincture group and drug groups 1-16 (corresponding to examples 1-10 and comparative examples 1-6), 10 mice / group.

[0074] The liquid (1ml) provided by each group except the model group was poured on the non-woven fabric 2cm 2 (1*2cm), the mouse abdomen was depilated with 8% sodium sulfide, and the non-woven fabric was pasted respectively, covered with two layers of sulfuric acid paper, and fixed and closed with non-irritating adhesive tape. Each group was given drug once a day, and each time for 5h. One hour after the last administration, each group of mice was injected with 0.6% acetic acid (0.1ml / 10g) solution (0.2ml / each) to model.

[0075] The number of writhing times of mice within 15min was recorded (with the standard of abdominal concave, stretched hind limbs and raised hips), and the results are shown in Table 3:

[0076] Table 3

[0077]

[0078]

[0079] As shown in Table 3, compared with the model group, the administration groups 1-10 can significantly reduce the times of mouse writhing caused by acetic acid (p<0.05), and compared with the Goutongling tincture group, also has a significant analgesic effect. It is indicated that the Goutongling tincture prepared by the preparation method of the Goutongling tincture provided in the embodiment 1-10 has a more significant analgesic effect compared with the Goutongling tincture prepared by the prior art.

[0080] In summary, by using the preparation method of the Goutongling tincture provided in the present application, the Goutongling tincture prepared by the preparation method can significantly improve the effective component yield of the final product, improve the treatment effect, and reduce the treatment period.

[0081] The above only describes the preferred embodiments of the present application and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing a bone pain relief tincture, characterized in that: Comprising: (1) Artemisia rupestris L. is cleaned, dried, and ground into particles with a size of 0.5-1.0 cm, soaked in ethanol with a concentration of 45-55%, the solid-liquid ratio of the Artemisia rupestris L. to the ethanol being 80 g:100-200 ml, and the soaking time being 4-6 h; then ultrasonic treatment is performed, the conditions of the ultrasonic treatment including an ultrasonic power of 200-400 W and an ultrasonic time of 25-30 min; then microwave extraction is performed, the conditions of the microwave extraction including a temperature of 50-65 ℃, a microwave frequency of 720-950 MHz, a microwave power of 540-630 W, and an extraction time of 5-8 min; then the Artemisia rupestris L. residues and the extract are separated; (2) the Artemisia rupestris L. residues are mixed with dry ginger, myrrh, and frankincense to obtain a premix; then the premix is subjected to percolation extraction with the ethanol, and the last percolation liquid is collected to obtain 950 ml combined with the extract; (3) another 50 ml of the ethanol is used to dissolve dragon's blood and borneol, and the solution is combined with the percolation liquid and the extract, mixed, and left to stand for 48 hours, filtered, and prepared into 1000 ml, thereby obtaining the product.

2. The method of preparing Gu Tong Ling tincture according to claim 1, characterized in that: In step (2), the flow rate of the percolation is 5-7 ml / min.

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