Rishuan lotion and its preparation method and use

Abstract

The present invention relates to a Rishuan lotion with excellent pharmaceutical and biological effects, and its preparation method and use. The Rishuan lotion is made of the following eight medicinal materials in the following proportions by weight: 38-58 parts of Sophora flavescens, 18-38 parts of Verbena officinalis, 5-25 parts of Taraxacum officinale, 5-25 parts of Cnidium monnieri, 5-15 parts of Galla chinensis, 25-45 parts of Stemona officinalis, 5-15 parts of Zanthoxylum bungeanum, and 5-15 parts of Alum, wherein pharmaceutical excipients are optionally added. The present invention also relates to a method for preparing the Rishuan lotion, and their use in preparing a medicine having the effects of clearing away heat and detoxifying, promoting dampness and relieving itching and / or being clinically used for women's vulvar itching or men's scrotal eczema. The Rishuan lotion of the present invention has excellent effects as described in the specification.

Description

Technical Field

[0001] The present invention belongs to the field of traditional Chinese medicine, and specifically relates to a Rishuan lotion, and in particular to a Rishuan lotion with excellent pharmaceutical and biological effects. The present invention also relates to a method for preparing the Rishuan lotion with excellent pharmaceutical and biological effects. The present invention further relates to the use of the Rishuan lotion in preparing a drug with the effects of clearing away heat and detoxifying, promoting dampness and relieving itching, and clinically used for female vulvar itching or male scrotal eczema. Background Art

[0002] The Chinese patent ZL03117386.1 (CN1440796B) of the applicant discloses a medicine for clearing away heat, detoxifying, removing dampness and relieving itching. The medicine is a Chinese medicine preparation prepared by conventional preparation process with the following main raw materials in weight ratio: 20-45 parts of Sophora flavescens, 10-25 parts of Verbena officinalis, 4-18 parts of Taraxacum officinale, 2-12 parts of Cnidium monnieri, 2-10 parts of Galla chinensis, 8-28 parts of Stemona tuberosa, 2-12 parts of Zanthoxylum bungeanum, and 2-12 parts of Alum. The medicine uses local Chinese herbal medicines as raw materials. The medicine has the functions of clearing away heat, detoxifying, removing dampness and relieving itching; it is easy to prepare, low in cost and has good therapeutic effect; it can be used to treat women's vulvar itching, men's scrotal eczema and other diseases. Example 1 of the Chinese patent ZL03117386.1 (CN1440796B) records a specific washing liquid, and its preparation method is as follows: 4.8kg of Sophora flavescens, 2.8kg of Verbena officinalis, 1.5kg of Taraxacum officinale, 1.5kg of Cnidium monnieri, 1kg of Galla chinensis, 3.5kg of Stemona japonica, 1kg of Zanthoxylum bungeanum, and 1kg of alum are taken as raw materials, and 1kg of benzoic acid and 0.03kg of ethyl hydroxybenzoate are taken as auxiliary materials; after mixing the above 8 medicinal materials, 7 of which, except alum, are added with 10 times the amount of water and boiled for 1 hour, filtered, and the filtrate is reserved; the medicinal residue is mixed with alum, boiled twice with 5 times the amount of water, each time for 1 hour, filtered, combined with the above filtrate and mixed, left to stand for 24 hours, filtered, adjusted to a pH value of 4-6, added with benzoic acid and ethyl hydroxybenzoate, and then added with water to 100L, mixed to obtain a finished washing liquid.

[0003] In addition, the applicant's Chinese patent application No. 201711249921.1 (CN107961341A) discloses a method for preparing Rishuan lotion, which includes sequentially putting Sophora flavescens, Stemona radix, Verbena officinalis, Galla chinensis, Taraxacum officinale, Zanthoxylum bungeanum and Cnidium monnieri into an extraction tank, adding drinking water, turning on steam heating, controlling the steam pressure at 0.20-0.25Mpa, turning on the circulation, heating, and when the decoction temperature reaches 95°C~98°C, the steam pressure is maintained at 0.1~ 0.15MPa, keep circulating; decoction, filter the decoction liquid, discharge it to the liquid medicine storage tank, add drinking water and alum to the medicine residue in turn, decoct twice according to the above method, filter the decoction liquid, and place the liquid medicine insulation storage tank through the pipe row; return all the liquid medicine in the liquid medicine insulation storage tank to the extraction tank, open the bottom steam, heat it in a cycle, boil and sterilize the liquid medicine, place the sterilized liquid medicine in the intermediate storage tank and cool it to below 30°C, filter it, adjust the pH value to 4-6, add 1-benzoic acid and ethyl hydroxybenzoate, add water, and obtain the product. The Rishuan washing liquid produced by the method of the present invention has qualified microbial content, does not need to be reworked and sterilized, and saves manpower and material resources.

[0004] The National Drug Standard WS-10806 (ZD-0806)-2002-2012Z of the State Food and Drug Administration discloses the quality standard of Rishuan Wash developed by the applicant. The prescription of Rishuan Wash is: 48g of Sophora flavescens, 28g of Verbena officinalis, 15g of Taraxacum mongolicum, 15g of Cnidium monnieri, 10g of Galla chinensis, 35g of Stemona radix, 10g of Zanthoxylum bungeanum, and 10g of Alum; the preparation method is: the above eight flavors, except for Alum, Sophora flavescens and other seven flavors, add water to decoct for 1 hour, filter, and the filtrate is reserved; the residue and Alum are decocted twice with water, each time for 1 hour, filtered, combined with the above filtrate, and left to stand for 24 hours; filtered, adjusted the pH value to 4-6, added 10g of benzoic acid, 0.3g of ethylparaben, and added water to 1000ml, that is, the Rishuan Wash is a yellow-brown liquid with a slight precipitation and a fragrant smell. The functions and indications of the Rishuan Wash in Miao medicine: Mengkai, Mengayang, Gajiangdaiwonu, Bufajianggang, Chaowonuoluo, Gangganjiu; the functions and indications of traditional Chinese medicine: clearing away heat and detoxifying, promoting dampness and relieving itching, used for female vulva itching and male scrotal eczema. The usage and dosage of the Rishuan Wash are: for external use, shake during use, take an appropriate amount of this product before going to bed every night, dilute it with 10 times the amount of warm water, and then sit in a bath for 5 minutes. For severe cases, the liquid can be directly applied to the affected area.

[0005] In the national drug standard WS-10806 (ZD-0806)-2002-2012Z of Risuan wash solution, the pH value of the liquid is stipulated to be 4~6. It is also stipulated that alum, Sophora flavescens, Cnidium monnieri and Galla chinensis must be identified, and matrine derived from Sophora flavescens is determined in the content determination item. In addition, there are no special testing items for Risuan wash solution.

[0006] Quality control of Chinese patent medicines is an important part of ensuring the quality of medicines. Verbena is an important medicinal material in Rishuan lotion. However, various literatures on Rishuan lotion in the prior art do not pay attention to verbena and its possible impact on product quality. Therefore, those skilled in the art still expect to provide Rishuan lotion with excellent performance, such as excellent pharmaceutical and biological effects, expect to provide a method for preparing such Rishuan lotion, and expect to provide pharmaceutical uses of such Rishuan lotion with excellent performance, such as excellent pharmaceutical and biological effects. Summary of the invention

[0007] The object of the present invention is to provide a Rishuan lotion with excellent pharmaceutical and biological effects. Another object of the present invention is to provide a method for preparing a Rishuan lotion with excellent pharmaceutical and biological effects. The present invention further relates to the use of such Rishuan lotion in preparing a drug with the effects of clearing away heat and detoxifying, promoting dampness and relieving itching, and / or clinically used for female vulvar itching or male scrotal eczema. It has been found that one or more objects have been achieved through the scheme of the present invention. The present invention is completed based on such findings.

[0008] To this end, the first aspect of the present invention provides a Rishuan wash, which is made from eight medicinal materials including Sophora flavescens, Verbena officinalis, Taraxacum officinale, Cnidium monnieri, Galla chinensis, Stemona tuber, Zanthoxylum bungeanum and Alum, and optional pharmaceutical excipients.

[0009] According to the first aspect of the present invention, the eight medicinal materials are added in the following proportions by weight: 38-58 parts of Sophora flavescens, 18-38 parts of Verbena officinalis, 5-25 parts of Taraxacum officinale, 5-25 parts of Cnidium monnieri, 5-15 parts of Galla chinensis, 25-45 parts of Stemona japonica, 5-15 parts of Zanthoxylum bungeanum, and 5-15 parts of Alum.

[0010] According to the first aspect of the present invention, the Risuan lotion, wherein the eight medicinal materials are added in the following proportions by weight: 45-51 parts of Sophora flavescens, 25-31 parts of Herba Cynanchifoliae, 13-17 parts of Taraxaci, 13-17 parts of Fructus Cnidium, 8-12 parts of Galla chinensis, 30-40 parts of Stemona, 8-12 parts of Zanthoxylum bungeanum, and 8-12 parts of Alum.

[0011] According to the first aspect of the present invention, the Risuan lotion, wherein the eight medicinal materials are added in the following proportions by weight: 48 parts of Sophora flavescens, 28 parts of Herba Lycopodii, 15 parts of Herba Taraxaci, 15 parts of Fructus Cnidium, 10 parts of Galla chinensis, 35 parts of Radix Stemonae, 10 parts of Zanthoxylum bungeanum, and 10 parts of Alum.

[0012] According to the first aspect of the present invention, the Risuan wash liquid is made of eight medicinal materials in the following weight proportions per 1000 ml: 38-58g of Sophora flavescens, 18-38g of Verbena officinalis, 5-25g of Taraxacum officinale, 5-25g of Cnidium monnieri, 5-15g of Galla chinensis, 25-45g of Stemona bulbus, 5-15g of Zanthoxylum bungeanum, and 5-15g of Alum.

[0013] According to the first aspect of the present invention, the Risuan wash liquid is made of eight medicinal materials in the following weight proportions per 1000 ml: 45-51g of Sophora flavescens, 25-31g of Herba Cynanchum, 13-17g of Taraxaci, 13-17g of Fructus Cnidium, 8-12g of Galla chinensis, 30-40g of Stemona bulbus, 8-12g of Zanthoxylum bungeanum, and 8-12g of Alum.

[0014] According to the first aspect of the present invention, the Risuan wash liquid is made of eight medicinal materials in the following weight proportions per 1000 ml: 48g of Sophora flavescens, 28g of Herba Cynanchum, 15g of Herba Taraxaci, 15g of Fructus Cnidium, 10g of Galla chinensis, 35g of Radix Stemonae, 10g of Zanthoxylum bungeanum, and 10g of Alum.

[0015] According to the first aspect of the present invention, the Rishuan lotion is made of the following materials in weight proportion per 1000 ml: 38-58g of Sophora flavescens, 18-38g of Verbena officinalis, 5-25g of Taraxacum officinale, 5-25g of Cnidium monnieri, 5-15g of Galla chinensis, 25-45g of Stemona japonica, 5-15g of Zanthoxylum bungeanum, 5-15g of Alum, 5-15g of benzoic acid, 0.1-0.5g of ethylparaben, and an appropriate amount of water.

[0016] According to the first aspect of the present invention, the Rishuan lotion is made of the following materials in weight proportion per 1000 ml: 45-51g of Sophora flavescens, 25-31g of Saddle Grass, 13-17g of Taraxacum officinale, 13-17g of Cnidium monnieri, 8-12g of Galla chinensis, 30-40g of Stemona japonica, 8-12g of Zanthoxylum bungeanum, 8-12g of Alum, 7.5-12.5g of benzoic acid, 0.2-0.4g of ethylparaben, and an appropriate amount of water.

[0017] According to the first aspect of the present invention, the Risuan lotion is made of the following materials in the following weight proportions per 1000 ml: 48g of Sophora flavescens, 28g of Saddle Grass, 15g of Taraxacum, 15g of Cnidium monnieri, 10g of Galla chinensis, 35g of Stemona bulb, 10g of Zanthoxylum bungeanum, 10g of Alum, 10g of benzoic acid, 0.3g of ethylparaben, and an appropriate amount of water.

[0018] According to the first aspect of the present invention, the Rishuan washing liquid is prepared by a method comprising the following steps, based on the amount of 1000 ml: the seven medicinal materials except alum of the above eight medicinal materials are decocted in water for 1 hour, filtered, and the filtrate is reserved; the medicinal residues and alum are decocted in water twice, each time for 1 hour, filtered, combined with the above filtrate, and allowed to stand for 24 hours; filtered, adjusted the pH value to 4-6, added benzoic acid and ethylparaben, stirred to dissolve, and added water to 1000 ml to obtain the washing liquid.

[0019] According to the first aspect of the present invention, the Rishuan lotion is prepared by a method comprising the following steps, based on the amount of 1000 ml:

[0020] Add 550-650ml of water to the above eight herbs, except alum and verbena, and boil for 1 hour. Filter and set aside the filtrate.

[0021] Add 350-450 ml of water to the residue and alum for the first time, boil for 1 hour, filter, then add 250-350 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0022] Verbena was boiled with 80-120ml, 40-80ml and 30-50ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use;

[0023] Combine the three groups of filtrates and let stand for 24 hours;

[0024] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0025] According to the first aspect of the present invention, the Rishuan lotion is prepared by the following formula and preparation method based on the amount of 1000 ml:

[0026] Formula: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona tuberosa 35g, Zanthoxylum bungeanum 10g and Alum 10g, auxiliary materials: Benzoic acid 10g, ethylparaben 0.3g;

[0027] Preparation method:

[0028] The above eight herbs, except alum and verbena, are boiled in 650ml of water for 1 hour, filtered, and the filtrate is reserved;

[0029] The residue and alum were first boiled with 390 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0030] Verbena was boiled with 100ml, 50ml and 30ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0031] Combine the three groups of filtrates and let stand for 24 hours;

[0032] Filter, adjust the pH to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0033] According to the first aspect of the present invention, the Rishuan lotion is prepared by the following formula and preparation method based on the amount of 1000 ml:

[0034] Formula: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona tuberosa 35g, Zanthoxylum bungeanum 10g and Alum 10g, auxiliary materials: Benzoic acid 10g, ethylparaben 0.3g;

[0035] Preparation method:

[0036] The above eight herbs, except alum and verbena, are boiled in 600ml of water for 1 hour, filtered, and the filtrate is reserved;

[0037] The residue and alum were first boiled with 400 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0038] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0039] Combine the three groups of filtrates and let stand for 24 hours;

[0040] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0041] According to the first aspect of the present invention, the Rishuan lotion is prepared by the following formula and preparation method based on the amount of 1000 ml:

[0042] Formula: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona tuberosa 35g, Zanthoxylum bungeanum 10g and Alum 10g, auxiliary materials: Benzoic acid 10g, ethylparaben 0.3g;

[0043] Preparation method:

[0044] The above eight herbs, except alum and verbena, are boiled in 550ml of water for 1 hour, filtered, and the filtrate is reserved;

[0045] The residue and alum were first boiled with 450 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0046] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0047] Combine the three groups of filtrates and let stand for 24 hours;

[0048] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0049] Furthermore, the second aspect of the present invention provides a method for preparing the Rishuan lotion described in any one of the first aspect of the present invention, which comprises the following steps based on the amount of 1000 ml:

[0050] Add 550-650ml of water to the other six herbs except alum and verbena and boil for 1 hour, filter and set aside the filtrate;

[0051] Add 350-450 ml of water to the residue and alum for the first time, boil for 1 hour, filter, then add 250-350 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0052] Verbena was boiled with 80-120ml, 40-80ml and 30-50ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use;

[0053] Combine the three groups of filtrates and let stand for 24 hours;

[0054] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0055] According to the method of the second aspect of the present invention, the formula of the Rishuan lotion is: 48g of Sophora flavescens, 28g of Verbena officinalis, 15g of Taraxacum officinale, 15g of Cnidium monnieri, 10g of Galla chinensis, 35g of Stemona radix, 10g of Zanthoxylum bungeanum and 10g of Alum, and auxiliary materials are: 10g of benzoic acid and 0.3g of ethylparaben; the method comprises the following steps:

[0056] The above eight herbs, except alum and verbena, are boiled in 650ml of water for 1 hour, filtered, and the filtrate is reserved;

[0057] The residue and alum were first boiled with 390 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0058] Verbena was boiled with 100ml, 50ml and 30ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0059] Combine the three groups of filtrates and let stand for 24 hours;

[0060] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0061] According to the method of the second aspect of the present invention, the formula of the Rishuan lotion is: 48g of Sophora flavescens, 28g of Verbena officinalis, 15g of Taraxacum officinale, 15g of Cnidium monnieri, 10g of Galla chinensis, 35g of Stemona radix, 10g of Zanthoxylum bungeanum and 10g of Alum, and auxiliary materials are: 10g of benzoic acid and 0.3g of ethylparaben; the method comprises the following steps:

[0062] The above eight herbs, except alum and verbena, are boiled in 600ml of water for 1 hour, filtered, and the filtrate is reserved;

[0063] The residue and alum were first boiled with 400 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0064] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0065] Combine the three groups of filtrates and let stand for 24 hours;

[0066] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0067] According to the method of the second aspect of the present invention, the formula of the Rishuan lotion is: 48g of Sophora flavescens, 28g of Verbena officinalis, 15g of Taraxacum officinale, 15g of Cnidium monnieri, 10g of Galla chinensis, 35g of Stemona radix, 10g of Zanthoxylum bungeanum and 10g of Alum, and auxiliary materials are: 10g of benzoic acid and 0.3g of ethylparaben; the method comprises the following steps:

[0068] The above eight herbs, except alum and verbena, are boiled in 550ml of water for 1 hour, filtered, and the filtrate is reserved;

[0069] The residue and alum were first boiled with 450 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0070] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0071] Combine the three groups of filtrates and let stand for 24 hours;

[0072] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0073] Furthermore, the third aspect of the present invention provides the use of the Risuan wash described in any one of the first aspect of the present invention in the preparation of a drug having the effects of clearing away heat and detoxifying, promoting dampness and relieving itching, and / or clinically used for female vulvar itching or male scrotal eczema.

[0074] Any embodiment of any aspect of the present invention or any technical feature thereof can be combined with each other, as long as such combination does not conflict. The present invention is further described below.

[0075] Sophorae Flavescentis Radix, which is included in the 2020 edition of the Chinese Pharmacopoeia, is the dried root of Sophora flavescens Ait. of the Leguminosae family. It is dug in spring and autumn, the root head and small branch roots are removed, washed and dried, or sliced ​​and dried while fresh. Sophorae Flavescentis Radix is ​​a perennial subshrub of the Leguminosae family, 1-2 meters high. The stem is erect and branched; the leaves are ovate-lanceolate, with dense soft hairs on the back; the racemes are terminal, the corolla is yellow-white, and the standard petals are ovate-spoon-shaped; the fruit is cylindrical and beaded; the seeds are brown and flat-globose; the flowering period is June-July, and the fruiting period is July-September. The origin of the name of Sophora Flavescentis is recorded in the Compendium of Materia Medica: "It is named after its taste, it is named after its merits, and it is named after its leaf shape." Sophora Flavescentis is native to China. Except for Qinghai and Xinjiang, it is distributed all over the country, and it is also distributed in India, Japan, North Korea, and Russia. It is commonly found in shrub forests on hillsides, sandy grass slopes or near fields. Sophora flavescens likes warm and dry climates, is cold-resistant and high-temperature-resistant, likes fertilizers and is afraid of waterlogging and tolerates saline-alkali sandy soil. The main propagation methods are sowing and root division. According to the "Shennong Bencao Jing", "Sophora flavescens tastes bitter and cold, and can treat abdominal qi stagnation, lumps, accumulation, jaundice, residual urine, water expelling, carbuncle, and can nourish the middle, improve eyesight and stop tears". Modern pharmacological research has shown that Sophora flavescens contains matrine, which has an inhibitory effect on a variety of skin fungi and tuberculosis bacteria. Sophora flavescens has good moisturizing and spreading effects and can be used as an adjuvant; the stem bark fiber can also be used to weave sacks; the seeds can be used as pesticides.

[0076] Verbena (Verbenae Herba), included in the 2020 edition of the Chinese Pharmacopoeia, is the dried aerial part of Verbena officinalis L., a plant of the Verbenaceae family. It is harvested when the flowers bloom from June to August, and the impurities are removed and dried. Verbena tastes bitter and cool, and it enters the liver and spleen meridians. It has the functions of promoting blood circulation and dispersing blood stasis, detoxifying, promoting diuresis, relieving jaundice, and stopping malaria. It is often used clinically for accumulation of masses, dysmenorrhea, amenorrhea, laryngeal paralysis, carbuncle, edema, jaundice, and malaria. Verbena is a perennial herb with an upright dark green stem, quadrangular in shape, and sparse coarse hairs; the green leaves are long ovate, cherry-shaped at the base, and coarsely serrated on the edges; the slender spike inflorescence grows at the top of the branches or in the axils, the flowers are small and sparse, and the flowering period is July; the fruit is oblong, with a thin pericarp that cracks when ripe, and the fruiting period is September. According to the Compendium of Materia Medica, verbena is named for its terminal spike-shaped flowers that resemble whips. Verbena is produced in Jiangsu, Hubei, Guangxi, Guizhou and other places, but it is also distributed in other provinces. It is commonly found on hillsides and wastelands. It likes warm climates, is not cold-resistant, and has low requirements for soil, as long as it has good drainage. Verbena is mainly propagated by seeds. Just sow the seeds and fill them with soil. It can also be propagated by division. The whole plant of verbena is used for medicinal purposes. It is cool in nature and slightly bitter in taste. It has the effects of cooling blood, dispersing blood stasis, dredge menstruation, clearing heat, detoxifying, relieving itching, repelling insects, and reducing swelling. According to the Compendium of Materia Medica, verbena clears heat and detoxifies, promotes diuresis and reduces swelling, and can be used to treat malaria, colds and other diseases. Verbena has a refreshing and pleasant aroma. It can be used as a raw material for cosmetics and perfumes. It is also often used to make tea. It is one of the popular herbal teas. At the same time, it is also a nutritious food. Eating it can promote blood circulation and remove blood stasis.

[0077] The dandelion (Taraxaci Herba) included in the 2020 edition of the Chinese Pharmacopoeia, page 367, is the dried whole grass of the Asteraceae plant Taraxacum mongolicum Hand. -Mazz., the alkali dandelion Taraxacum borealisinenseKitam. or several plants of the same genus, which are dug when the flowers first bloom from spring to autumn, removed from impurities, washed and dried. The dandelions used in the specific experiments of the present invention refer to Taraxacum mongolicum Hand. -Mazz. unless otherwise specified. Dandelion is a perennial herbaceous plant of the genus Taraxacum in the Asteraceae family, also known as Mongolian dandelion, yellow flower ground Ding, mother-in-law Ding, lantern grass, etc. The root is cylindrical, dark brown and sturdy. The leaves are obovate-lanceolate, oblanceolate or oblong-lanceolate; the scapes are 1 to several, as long as the leaves or slightly longer, with a head-shaped inflorescence, yellow ligulate flowers, purple-red stripes on the back of the marginal flower tongues, and dark green anthers and stigmas; achenes are obovate-lanceolate and dark brown. The flowering period is from April to September, and the fruiting period is from May to October. Most dandelions grow in temperate and subtropical regions of the northern hemisphere, and a few grow in tropical regions. They often grow on hillside grasslands, roadsides, fields, and riverbanks in medium and low altitude areas. Dandelions are cool-loving plants with strong adaptability, both cold-resistant and heat-resistant. Dandelions also have a certain resistance to drought and acidity, and can grow in all soil types, but grow better in sandy soils. The native range of dandelions in the world is from Siberia to East Asia. Dandelion is a plant with both medicinal and edible properties. Its dried whole herb can be used as medicine, which has the effects of clearing away heat and detoxification, reducing swelling and dispersing knots, and promoting diuresis and relieving stranguria. At the same time, dandelion is rich in nutrients, rich in various vitamins, minerals, polysaccharides and other active ingredients. Both raw or cooked young leaves and flowers of dandelion can be eaten.

[0078] Cnidium monnieri (L.) Cuss., which is included in the 2020 edition of the Chinese Pharmacopoeia, is the dried mature fruit of Cnidium monnieri (L.) Cuss., a plant of the Apiaceae family. The fruit is harvested in summer and autumn when it is ripe, and the impurities are removed and dried. Cnidium monnieri is an annual herbaceous plant of the genus Cnidium in the Apiaceae family. The stem is erect, branched, sparsely covered with fine soft hairs, with longitudinal ridges; the basal leaves are rectangular or ovate, and the leaf sheaths are short and wide; the upper petiole has a white leaf sheath, the leaves are ovate to triangular ovate, the top is tail-shaped, with a white tip; the terminal lobes are narrow or linear lanceolate, the umbel inflorescence is linear to linear lanceolate; the base of the style is raised; the double-hanging fruit is wide and elliptical. The flowering period is from April to July, and the fruiting period is from June to October. Because the snake likes to lie down and eat its children, it is called snake bed and snake millet. Cnidium monnieri is mainly produced in Europe and Asia, and is distributed throughout China. Cnidium monnieri has strong adaptability, is not strict with climate and soil, likes warmth and is cold-resistant; it grows mostly in grass beside mountain roads, and is occasionally found in ponds. The fruit of Cnidium monnieri is slightly poisonous, and tastes spicy and bitter. It has the effects of drying dampness and dispelling wind, killing insects and relieving itching, and warming the kidney and strengthening yang. In addition to its medicinal uses, Cnidium monnieri can also be eaten as a vegetable because of its green leaves and special fragrance.

[0079] Galla Chinensis, included in page 68 of Volume 1 of the 2020 edition of the Chinese Pharmacopoeia, is a gall on the leaves of Rhus chinensis Mill., Rhus potaninii Maxim. or Rhuspunjabensis Stew. var. sinica (Diels) Rehd. et Wits. of the Anacardiaceae family. It is mainly formed by the parasitism of the gall aphid Melaphis chinensis (Bell) Baker. It is picked in autumn, boiled or steamed in boiling water until the surface turns gray to kill the aphids, taken out and dried. According to their appearance, they are divided into "belly gall" and "horn gall". Gallnut is distributed in Sichuan, Guizhou, Yunnan, Shaanxi, Guangxi and other places; it has the effects of astringing the lungs and reducing fire, astringing the intestines and stopping diarrhea, astringing sweat, stopping bleeding, collecting moisture and astringing sores; it is commonly used for long-term cough due to lung deficiency, cough due to lung heat and phlegm, long-term diarrhea and dysentery, spontaneous sweating and night sweats, thirst, blood in stool and hemorrhoids, bleeding due to trauma, carbuncle, sore and skin rot. The gallnut used in the specific test of the present invention, if not otherwise specified, refers to the gallnut from Rhus chinensis. Rhus chinensis is a deciduous small tree plant of the genus Rhus chinensis of the Anacardiaceae family, up to 10 meters, with brown twigs, polymorphic leaves, round base, dark green leaf surface, pink green leaf back, and sessile. The panicle is wide, multi-branched, the female inflorescence is shorter, dense and soft; the bracts are white, the petals are oblong, and they are rolled outward when blooming; the drupes are spherical and red when mature. It blooms in August and September and bears fruit in October. Salt bran wood can absorb salt in the soil and secrete it in the form of brine. When the water evaporates, the salt adheres to the tree, hence the name. Salt bran wood is a widespread species, now distributed in India, Japan and other countries. In China, except for Northeast China, Inner Mongolia and Xinjiang, it is distributed in other provinces and regions. Salt bran wood likes light, warm and humid climate, strong adaptability and cold resistance. It is not strict with soil. It grows in sparse forests or shrubs such as sunny slopes and valleys at medium and high altitudes. Salt bran wood has seed propagation, rooting and cutting methods. "Rihuazi Zhujia Bencao" and "Compendium of Materia Medica" record that salt bran wood can "produce fluid and reduce fire, resolve phlegm, moisten the lungs and nourish the kidneys, disinfect, stop diarrhea and sweat." The fresh stems and leaves of salt bran wood are rich in nitrogen, phosphoric acid, etc., and the stems and leaves are soft, juicy and easy to rot and decompose, making it a good green manure. In addition, the tender stems and leaves of salt bran wood can be eaten as wild vegetables. It is the main wild feed for pig farming in the mountainous areas of western Henan, and the flowers are a high-quality source of honey and pollen in early autumn.

[0080] Stemonae RadixX, which is included in the 2020 edition of the Chinese Pharmacopoeia, is the dried root tubers of Stemona sessilifolia (Miq.) Miq., Stemona japonica (Bl.) Miq. or Stemona tuberosa Lour. of the Stemonaceae family. They are excavated in spring and autumn, the fibrous roots are removed, washed, slightly blanched in boiling water or steamed until there is no white core, taken out, and dried. The Stemonae used in the specific experiments of the present invention refers to the erect Stemonae unless otherwise specified. Stemonae is a perennial climbing herb of the Stemonaceae family. The underground roots are tuberous, bundled, fleshy, and long spindle-shaped; the stems are long; the leaves are ovate, ovate-lanceolate, with acuminate or acute tips, and the leaves have petioles; the pedicels grow close to the midrib of the leaves, and the flowers are solitary or arranged in racemes; the capsules are ovate, slightly flat, and dark red-brown on the surface; the seeds of Stemona are elliptical and purple-brown. The flowering period is from May to July, and the fruiting period is from July to October. Stemona is distributed in Zhejiang, Jiangsu, Anhui, Jiangxi and other provinces in China. Japan has introduced it for cultivation; it grows in grass on hillsides, roadsides and under forests at an altitude of 300-400 meters. Its main reproduction methods include seed reproduction in sexual reproduction, root division reproduction in asexual reproduction, and tissue culture in asexual reproduction. Stemona was first recorded in "Famous Doctors' Records" and was listed as a medium-grade product. It has a long history of medicinal use in China and is a commonly used Chinese medicine in clinical practice of traditional Chinese medicine. It is sweet and bitter in nature, and the ones that are thick, plump, solid and white are preferred. It can kill insects, relieve itching and kill lice when used externally; it can moisten the lungs, relieve cough and eliminate phlegm when taken internally. Its effects have been recorded in herbal works of all dynasties, such as "Compendium of Materia Medica" and "Bencao Jingshu".

[0081] The pepper (Zanthoxyli Pericarpium) included in the 2020 edition of the Chinese Pharmacopoeia, Volume 1, Page 166, is the dried mature peel of the Rutaceae plant Zanthoxylum schinifolium Sieb. et Zucc. or Zanthoxylum bungeanumMaxim. The mature fruits are harvested in autumn, dried in the sun, and the seeds and impurities are removed. The pepper used in the specific test of the present invention refers to Zanthoxylum bungeanum Maxim. unless otherwise specified. Zanthoxylum is a perennial deciduous small tree of the Rutaceae family and the Zanthoxylum genus. It ranks first among the "thirteen spices" of condiments and is known as the "king of seasoning". It has a tall stem, short thorns on the branches, and small leaves that are opposite and sessile. The inflorescence is terminal or terminal on the side branches; the tepals are yellow-green, and the shape and size are roughly the same; female flowers rarely have developed stamens. The fruit is purple-red, with a single merophyte scattered with slightly raised oil spots. It blooms in April and May and bears fruit in August, September or October. Because the skin has small protruding oil spots that are spotted and look like flowers, it is called "peppercorn". Peppercorn is a widespread species. It is native to China and native to the Himalayas. It is now also distributed in Japan, South Korea and other countries. There are two ways of reproduction for peppercorns. Sexual reproduction is completed by seed sowing, and vegetative reproduction is completed by root and stem grafting, cuttings, etc. Peppercorns are mostly found in plains to high-altitude mountains. They are drought-resistant, like sunshine, have strong ability to survive alone, and are planted in many places. Peppercorns are recorded in Chinese herbal books of all dynasties. They were first seen in the "Book of Songs" and were first used as medicine in the "Shennong Bencao Jing". Peppercorns are pungent, warm and dry in nature, enter the spleen and stomach, and are good at warming the middle and drying dampness, dispersing cold and relieving pain, stopping vomiting and diarrhea. It is often used for symptoms such as cold pain in the abdomen, vomiting, diarrhea, and loss of appetite. In addition, peppercorns can also expel ascariae and kill insects, and can be used for abdominal pain caused by worm accumulation in children.

[0082] Alum, which is included in the 2020 edition of the Chinese Pharmacopoeia, is made from alumite of the sulfate mineral alumite family through processing and refining, and mainly contains hydrated potassium aluminum sulfate [KAl(SO4)2·12H2O]. Alum is in irregular blocks or granules, colorless or light yellowish white, transparent or translucent. The surface is slightly smooth or uneven, with fine longitudinal edges and a glassy luster; it is hard and brittle; it has a slight odor, tastes sour, slightly sweet and extremely astringent. Alum aqueous solution shows the identification reaction of aluminum salts (Pharmacopoeia General Chapter 0301), potassium salts (Pharmacopoeia General Chapter 0301) and sulfates (Pharmacopoeia General Chapter 0301). Alum aqueous solution is acidic, easily soluble in water, and hydrolyzed to form aluminum hydroxide colloidal precipitates, etc. Alum is a mineral Chinese medicine. It can detoxify, kill insects, dry dampness and relieve itching when used externally; it can stop bleeding, stop diarrhea and resolve phlegm when used internally. Alum tastes sour and astringent, is cold in nature, and enters the lung, spleen, liver, and large intestine meridians. Indications: stroke, epilepsy, throat paralysis, scabies, eczema, carbuncle, swelling, burns, mouth sores, ulcers, pus in the ears, nasal polyps, pain in sores and hemorrhoids, metrorrhagia, epistaxis, bleeding from injuries, chronic diarrhea, leucorrhea, itching in the genitals, rectal prolapse, uterine prolapse, etc. Alum tastes sour and astringent, is cold in nature, and has antibacterial and astringent effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0083] Figure 1 : Chromatogram of verbena herb test sample solution. DETAILED DESCRIPTION

[0084] The embodiments of the present invention can prepare Rishuan lotion by referring to the method described in the national drug standard WS-10806 (ZD-0806)-2002-2012Z. In the preparation of Rishuan lotion in each embodiment of the present invention, unless otherwise specified, the various medicinal materials used are from the same batch.

[0085] Example 1: Preparation of Rishuan Lotion

[0086] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0087] Preparation method:

[0088] Add 600ml of water to the above eight herbs, except alum, and boil them for 1 hour, filter and set aside the filtrate;

[0089] The residue and alum were first boiled with 600 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the three filtrates were combined and allowed to stand for 24 hours.

[0090] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0091] Example 2: Preparation of Rishuan Lotion

[0092] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0093] Preparation method:

[0094] Add 700ml of water to the above eight herbs, except alum, and boil them for 1 hour, filter and set aside the filtrate;

[0095] Add 500ml of water to the residue and alum for the first time, boil for 1 hour, filter, add 300ml of water again, boil for 1 hour, filter, combine the three filtrates, and let stand for 24 hours;

[0096] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0097] Example 3: Preparation of Rishuan Lotion

[0098] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0099] Preparation method:

[0100] Add 650ml of water to the above eight herbs, except alum, and boil for 1 hour, filter and set aside the filtrate;

[0101] Add 550ml of water to the residue and alum for the first time, boil for 1 hour, filter, add 300ml of water again, boil for 1 hour, filter, combine the three filtrates, and let stand for 24 hours;

[0102] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0103] Example 4: Preparation of Rishuan Lotion

[0104] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0105] Preparation method:

[0106] The above eight herbs, except alum and verbena, are boiled in 650ml of water for 1 hour, filtered, and the filtrate is reserved;

[0107] The residue and alum were first boiled with 390 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0108] Verbena was boiled with 100ml, 50ml and 30ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0109] Combine the three groups of filtrates and let stand for 24 hours;

[0110] Filter, adjust the pH to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0111] Example 5: Preparation of Rishuan Lotion

[0112] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0113] Preparation method:

[0114] The above eight herbs, except alum and verbena, are boiled in 600ml of water for 1 hour, filtered, and the filtrate is reserved;

[0115] The residue and alum were first boiled with 400 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0116] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0117] Combine the three groups of filtrates and let stand for 24 hours;

[0118] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0119] Example 6: Preparation of Rishuan Lotion

[0120] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0121] Preparation method:

[0122] The above eight herbs, except alum and verbena, are boiled in 550ml of water for 1 hour, filtered, and the filtrate is reserved;

[0123] The residue and alum were first boiled with 450 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0124] Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0125] Combine the three groups of filtrates and let stand for 24 hours;

[0126] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0127] Test Example 1: Determination of oleanolic acid and ursolic acid in Rishuan lotion

[0128] The Chinese Pharmacopoeia records methods for determining oleanolic acid and ursolic acid in verbena. This test example refers to these methods to determine oleanolic acid and ursolic acid in verbena herbs or in Rishuan lotion prepared therefrom.

[0129] Determined by high performance liquid chromatography (General Chapter 0512 of the 2020 edition of the Chinese Pharmacopoeia);

[0130] Chromatographic conditions and system suitability test: A chromatographic column with octadecylsilane bonded silica as filler (Phenomenex Luna C 18 Chromatographic column, column specifications are 4.6mm×250mm, 5μm); methanol-0.2% acetic acid solution (82.5:17.5) is used as the mobile phase; evaporative light scattering detector detection, the theoretical plate number calculated based on the ursolic acid peak should be no less than 5000;

[0131] Preparation of reference solution: Take appropriate amount of oleanolic acid reference substance and ursolic acid reference substance (both purchased from China Food and Drug Inspection Institute), accurately weigh, add methanol to make a mixed solution containing 50μg oleanolic acid and 100μg ursolic acid per 1ml;

[0132] Preparation of the test solution of the verbena herb: Take about 0.5g of the powder of this product (passed through a No. 4 sieve), weigh it accurately, place it in a stoppered conical bottle, accurately add 25ml of anhydrous ethanol, weigh it, heat and reflux for 4 hours, cool it, weigh it again, make up the lost weight with anhydrous ethanol, shake it well, and filter it. Accurately measure 10ml of the filtrate, add 3ml of 1% ammonia solution, mix it well, shake it with petroleum ether (30-60°C) for 3 times, 15ml each time, discard the petroleum ether liquid, take the ethanol liquid and evaporate it to dryness, dissolve the residue in methanol, transfer it to a 5ml volumetric bottle, add methanol to the scale, shake it well, filter it through a 0.22µm microporous filter membrane, and take the filtrate to obtain;

[0133] Preparation of the test solution of Rishuan Lotion: Take Rishuan Lotion, shake well, filter through a 0.22µm microporous membrane, and take the filtrate to obtain;

[0134] Determination method: Accurately pipette 10μl and 20μl of reference solution, 20μl of verbena herb test solution, and 20μl of Rishuan lotion test solution, respectively, inject into liquid chromatograph, determine, and calculate with external standard two-point method logarithmic equation to obtain the result.

[0135] The Pharmacopoeia stipulates that the total amount of oleanolic acid (C30H48O3) and ursolic acid (C30H48O3) in verbena herbs, calculated on a dry basis, must not be less than 0.30%.

[0136] The verbena materials used in each embodiment are from the same batch, and the verbena materials are calculated as dry products.

[0137] Each 28g of verbena contains 65.32mg (0.233%) of oleanolic acid and 116.43mg (0.416%) of ursolic acid; [this result is the theoretical content of oleanolic acid and ursolic acid in the medicinal material, which can be used to calculate the recovery rate of oleanolic acid and ursolic acid in the washing solution];

[0138] Every 1000 ml of the Rishuan lotion obtained in Example 1 (equivalent to the amount of lotion prepared from 28 g of verbena) contains 56.87 mg of oleanolic acid [the recovery rate of oleanolic acid recovered from 28 g of verbena is 87.06%, i.e. (56.87÷65.32)×100%], and 106.81 mg of ursolic acid (the recovery rate is 91.74%, i.e. (106.81÷116.43)×100%); [for convenience, the oleanolic acid and ursolic acid present in every 1000 ml of lotion prepared herein (i.e., the amount of lotion equivalent to that prepared from 28 g of verbena) can be characterized by the term “recovery rate”];

[0139] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 2 was 88.42% and 90.67% respectively;

[0140] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 3 was 87.36% and 90.16% respectively;

[0141] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 4 was 88.63% and 91.52% respectively;

[0142] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 5 was 86.93% and 90.58% respectively;

[0143] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 6 was 87.72% and 91.24% respectively;

[0144] The above results show that in the process of preparing the lotion, verbena and the other seven herbs were extracted together in Examples 1 to 3, and verbena and the other seven herbs were extracted separately in Examples 4 to 6. The oleanolic acid and ursolic acid in the lotions obtained by the two sets of process methods were basically equivalent.

[0145] However, the inventors unexpectedly found that there was a significant difference in the recovery rates of verbenaside and verbenaside contributed by verbena in the washing solutions obtained by the two groups of process methods of Examples 1 to 3 and Examples 4 to 6, and found that this difference was likely caused by whether verbena was extracted together with alum. The specific experiments are described in the context of the present invention.

[0146] Test Example 2: Determination of verbenaside and verbenaside in Rishuan lotion

[0147] Although the verbena content determination item included in the Chinese Pharmacopoeia uses oleanolic acid and ursolic acid as indicators, it is generally believed in the art that verbenaside and verbenaside are also the main components of verbena with excellent biological activity. Therefore, understanding the migration behavior of these two components from the medicinal material to the lotion is beneficial to improving the quality of the drug.

[0148] There are already documented methods for determining verbenaside and verbenaside in verbena, and this test example refers to these methods to determine verbenaside and verbenaside in verbena herbs or in the Rishuan lotion prepared therefrom, wherein verbenaside is also called 5-hydroxyverboside.

[0149] 1. Preparation of reference substances

[0150] In this test example, verbena glycoside reference substance and euphorbia verbena glycoside reference substance were first prepared with reference to the method of Zhang Tao's literature (Zhang Tao, et al., Research on iridoid glycosides of verbena, Chinese Herbal Medicine. 2000(10):721). Among them, verbena glycoside reference substance (HPLC purity 99.2%): white powder, mp183.2~183.8℃, elemental analysis measured values ​​(%): C52.48, H6.27, O41.25, consistent with the theoretical molecular formula C17H24O10 contained in the literature, the maximum absorption of the ultraviolet spectrum in ethanol is 237.1nm; IR (KBr, cm-1): 3485, 3350, 3313, 2971, 2949, 2942, 2895, 1740, 1693, 1644, 1447, 1295, 1102, 1076, 1033, 993, 870, these data are consistent with the literature. Verbenside reference substance (HPLC purity 98.8%): white powder, mp188.9~189.4℃, elemental analysis measured values ​​(%): C50.46, H5.95, O43.59, consistent with the theoretical molecular formula C17H24O11 contained in the literature, the maximum absorption of the ultraviolet spectrum in ethanol is 231.2nm; IR (KBr, cm-1): 3423, 2959, 2931, 2882, 1756, 1710, 1624, 1440, 1371, 1295, 1223, 1189, 1145, 1075, 1041, 1021, 932, 867, 864, these data are consistent with the literature.

[0151] 2. HPLC determination

[0152] Then, verbenaside and verbenaside in the verbena herb or the Rishuan lotion prepared therefrom were determined according to the following method.

[0153] Determined by high performance liquid chromatography (General Chapter 0512 of the 2020 edition of the Chinese Pharmacopoeia);

[0154] Chromatographic conditions and system suitability test: chromatographic column with octadecylsilane bonded silica as filler (Agilent, Polaris 180Å C8-Ether, 4.6x250mm, 3µm, No: A2031250X046); column temperature 30℃; mobile phase methanol-water (20:80), flow rate 1.0mL / min; UV detector detection wavelength 235nm; injection volume 20μL. The theoretical plate number calculated for verbena glycoside and verbena glycoside was not less than 4000, the separation between adjacent peaks was greater than 2.0, and the symmetry factor was in the range of 0.95~1.05.

[0155] Preparation of reference solution: Take appropriate amount of verbena glycoside and verbena glycoside reference substances, accurately weigh, add methanol to prepare reference substance stock solution containing about 750 μg / ml verbena glycoside and about 1250 μg / ml verbena glycoside per 1 ml; accurately measure 5 ml of reference substance stock solution and place it in a 50 ml volumetric flask, add water to dilute to the scale, and obtain reference substance solutions containing verbena glycoside and verbena glycoside (concentrations are about 75 μg / ml and about 125 μg / ml, respectively);

[0156] Preparation of the test solution of Rishuan Lotion: Take Rishuan Lotion, shake well, filter through a 0.22µm microporous membrane, and take the filtrate to obtain;

[0157] Preparation of the test solution of verbena herb: take about 1g of the powder of this product (passed through a No. 4 sieve), accurately weigh it, put it in a stoppered conical bottle, accurately add 10ml of 65% methanol, weigh it, heat and reflux for 2 hours, cool it, weigh it again, make up the lost weight with 65% methanol, shake it well, filter it, accurately take 5ml of the filtrate and put it in a 20ml volumetric bottle, add water to dilute to the scale, shake it well, filter it through a 0.22µm microporous filter membrane, and take the filtrate to obtain;

[0158] Determination method: Accurately pipette 20μ1 of each of the reference solution, verbena herb test solution, and Rishuan lotion test solution, and inject them into liquid chromatograph respectively for determination. Calculate the contents of verbena glycoside and verbena glycoside in the two test solutions by external standard method.

[0159] A typical chromatogram is shown in the chromatogram of the verbena herb test solution. Figure 1 , among which the retention time of verbena glycoside is about 8 minutes, and the retention time of verbena glycoside is about 15.5 minutes.

[0160] 3. HPLC methodology investigation

[0161] Linearity: 1.0, 3.0, 5.0, 7.0, 9.0, 12.0 mL of the reference stock solution was accurately drawn and placed in a 50 mL volumetric flask, diluted to the mark with water, shaken, and the peak area was determined under the above chromatographic conditions. The standard curve was drawn with the mass concentration of the reference as the abscissa and the corresponding peak area as the ordinate, and the regression equation was calculated. Verbena glycoside: Y = 23.38X-44.62, r = 0.9999, and the linear range was 15-180 μg / mL; Verbena glycoside: Y = 30.42X + 31.58, r = 0.9998, and the linear range was 25-300 μg / mL; the results showed that the linear relationship of the two substances was excellent.

[0162] Precision: Accurately pipette 20 μL of the reference solution, repeat the injection 6 times to determine the peak areas of verbenaside and verbenaside, and calculate their respective RSDs. The RSDs of the peak areas of verbenaside and verbenaside were 0.56% and 0.44%, respectively.

[0163] Reproducibility: Take 6 portions of the same batch of verbena herbs, prepare them separately according to the method under the preparation of the test solution of verbena herbs, and obtain 6 test solutions. The amount of verbena glycoside and verbena glycoside was determined under the above chromatographic conditions. The verbena glycoside content in the medicinal material was 3.094±0.019 mg / g (RSD=0.61%) and the verbena glycoside content was 5.132±0.029 mg / g (RSD=0.57%) after 6 treatments, indicating that the method of the present invention has good reproducibility in determining verbena glycoside and verbena glycoside in the medicinal material. The above-mentioned verbena glycoside and verbena glycoside content means of 3.094 mg / g and 5.132 mg / g can be used as the theoretical content of the two substances in this batch of medicinal materials, which can be used to calculate the recovery rate of the two substances in the washing solution.

[0164] Determination of solution stability: Take the reference solution, Rishuan lotion test solution and verbena herb test solution, place them at room temperature, and determine the concentrations of verbena glycoside and verbena glycoside at 0, 2, 4, 6, 8, 10, 12, 18, and 24 h (n=9), and calculate the RSDs of verbena glycoside and verbena glycoside. As a result, the RSDs of the reference solution were 0.31% and 0.27%, the Rishuan lotion test solution were 0.24% and 0.29%, and the verbena herb test solution were 0.35% and 0.32%, respectively, indicating that the various sample solutions were stable within 24 h.

[0165] 4. Test results of Rishuan lotion sample:

[0166] As mentioned above, the theoretical contents of verbenaside and verbenaside in verbena herb are 3.094 mg / g (0.3094%) and 5.132 mg / g (0.5132%), respectively, which can be used to calculate the recovery rates of the two substances in the washing liquid (i.e., the percentage of verbenaside in the washing liquid to the verbenaside content in the equivalent amount of medicinal materials from the addition of medicinal materials to the preparation of the washing liquid, and other terms with similar contexts as "recovery rate" have similar meanings).

[0167] Each 28g of verbena contains 86.63mg (0.309%) of verbenaside and 143.70mg (0.513%) of verbenaside.

[0168] Every 1000 ml of the Rishuan lotion obtained in Example 1 (equivalent to the amount of lotion prepared from 28 g of verbena herb) contains 53.07 mg of verbena glycoside [the recovery rate of verbena glycoside recovered from 28 g of verbena herb is 61.26%, i.e. (53.07÷86.63)×100%], and 93.28 mg of verbena glycoside (recovery rate 64.91%, i.e. (93.28÷143.70)×100%); [for convenience, the verbena glycoside and verbena glycoside presented in every 1000 ml of lotion prepared herein (i.e., the amount of lotion prepared from 28 g of verbena herb) can be characterized by the term “recovery rate”];

[0169] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 2 was 60.37%, and the recovery rate of verbena glycosides in the euphorbia pulex was 64.48%;

[0170] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 3 was 61.82%, and the recovery rate of verbena glycosides in the euphorbia pulex was 65.13%;

[0171] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 4 was 88.87%, and the recovery rate of verbena glycosides in the euphorbia pulex was 92.24%;

[0172] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 5 was 90.26%, and the recovery rate of verbena glycosides in the euphorbia pulex was 91.86%;

[0173] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 6 was 89.58%, and the recovery rate of verbena glycosides in the euphorbia pulex was 91.93%;

[0174] The above results show that in the process of preparing the washing solution, when verbena and the other seven herbs were extracted together in Examples 1 to 3, verbena glycoside and verbena glycoside were significantly lower than those when verbena and the other seven herbs were extracted separately in Examples 4 to 6, indicating that the recovery rates of verbena glycoside and verbena glycoside in the washing solutions obtained by the two groups of process methods showed significant differences, and this difference may be related to whether alum is extracted together.

[0175] Example 7: Preparation of Rishuan Lotion

[0176] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0177] Preparation method:

[0178] The above eight herbs, except alum and verbena, are boiled in 650ml of water for 1 hour, filtered, and the filtrate is reserved;

[0179] Add 390 ml of water to the residue and boil for 1 hour, filter, then add 280 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0180] Verbena and alum were decocted with 100ml, 50ml and 30ml of water respectively for 3 times, each time for 1 hour, filtered, and the combined filtrate was reserved for later use;

[0181] Combine the three groups of filtrates and let stand for 24 hours;

[0182] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0183] Example 8: Preparation of Rishuan Lotion

[0184] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0185] Preparation method:

[0186] The above eight herbs, except alum and verbena, are boiled in 600ml of water for 1 hour, filtered, and the filtrate is reserved;

[0187] Add 400 ml of water to the residue and boil for 1 hour, filter, then add 300 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0188] Verbena and alum were decocted with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered, and the combined filtrate was reserved for later use;

[0189] Combine the three groups of filtrates and let stand for 24 hours;

[0190] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0191] Example 9: Preparation of Rishuan Lotion

[0192] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0193] Preparation method:

[0194] The above eight herbs, except alum and verbena, are boiled in 550ml of water for 1 hour, filtered, and the filtrate is reserved;

[0195] Add 450 ml of water to the residue and boil for 1 hour, filter, then add 300 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0196] Verbena and alum were decocted with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered, and the combined filtrate was reserved for later use;

[0197] Combine the three groups of filtrates and let stand for 24 hours;

[0198] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0199] The method of Experimental Example 1 was used to determine the contents of oleanolic acid and ursolic acid in the three Rishuan lotions obtained in Examples 7 to 9, and the recovery rates of oleanolic acid and ursolic acid in the lotions were calculated using the verbena as the raw material. The results were as follows:

[0200] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 7 was 89.13% and 90.35% respectively;

[0201] The recovery rate of oleanolic acid was 87.84% and the recovery rate of ursolic acid was 91.13% per 1000 ml of the Rishuan lotion obtained in Example 8;

[0202] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 9 was 88.37% and 90.26% respectively;

[0203] The above results show that in the process of preparing the lotion, when verbena and alum are extracted separately, the recovery rates of oleanolic acid and ursolic acid are consistent with the quality standard method, and alum will not affect the extraction of oleanolic acid and ursolic acid in verbena.

[0204] The method of Experimental Example 2 was used to determine the contents of verbena glycoside and verbena glycoside in the three Rishuan lotions obtained in Examples 7 to 9, and the recovery rates of verbena glycoside and verbena glycoside in the lotions were calculated using the verbena herbal material. The results were as follows:

[0205] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 7 was 83.31%, and the recovery rate of verbena glycosides in the euphorbia pulex was 85.23%;

[0206] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 8 was 82.62%, and the recovery rate of verbena glycosides in the euphorbia pulex was 86.07%;

[0207] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 9 was 83.35%, and the recovery rate of verbena glycosides in the euphorbia pulex was 85.47%;

[0208] The above results show that, in the process of preparing washing solution, when verbena and alum are extracted separately, the recovery rate of verbena glycoside and verbena glycoside is obviously higher than the quality standard method (Examples 1 to 3), but still lower than the verbena separate extraction process (Examples 4 to 6), indicating that alum affects the extraction of verbena glycoside and verbena glycoside in verbena to a certain extent, but is not completely an independent factor.

[0209] The inventors tried to investigate the factors that affect the low extraction rate of verbena and verbena glycosides when other materials were co-extracted with verbena, and unexpectedly found that the co-extracted dandelion also had a certain adverse effect on the extraction of verbena and verbena glycosides from verbena, as shown in the following examples.

[0210] Example 10: Preparation of Rishuan Lotion

[0211] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0212] Preparation method:

[0213] The above eight herbs, except alum, dandelion and verbena, are boiled in 550ml of water for 1 hour, filtered and the filtrate is reserved;

[0214] The residue and alum were first boiled with 400 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0215] Verbena and dandelion were decocted with 150ml, 70ml and 50ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use;

[0216] Combine the three groups of filtrates and let stand for 24 hours;

[0217] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0218] Example 11: Preparation of Rishuan Lotion

[0219] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0220] Preparation method:

[0221] The above eight herbs, except alum, dandelion and verbena, are boiled in 550ml of water for 1 hour, filtered and the filtrate is reserved;

[0222] The residue and alum were first boiled with 380 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0223] Verbena and dandelion were decocted with 150ml, 80ml and 60ml of water respectively for 3 times, each time for 1 hour, filtered, and the combined filtrate was reserved for later use;

[0224] Combine the three groups of filtrates and let stand for 24 hours;

[0225] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0226] Example 12: Preparation of Rishuan Lotion

[0227] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0228] Preparation method:

[0229] The above eight herbs, except alum, dandelion and verbena, are boiled in 500ml of water for 1 hour, filtered and the filtrate is reserved;

[0230] The residue and alum were first boiled with 430 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use;

[0231] Verbena and dandelion were decocted with 150ml, 80ml and 60ml of water respectively for 3 times, each time for 1 hour, filtered, and the combined filtrate was reserved for later use;

[0232] Combine the three groups of filtrates and let stand for 24 hours;

[0233] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0234] The contents of oleanolic acid and ursolic acid in the three Rishuan lotions obtained in Examples 10 to 12 were determined using the method of Test Example 1, and the recovery rates of oleanolic acid and ursolic acid in the lotions were calculated using the verbena as the raw material. The results were as follows:

[0235] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 10 was 90.82% and 91.48% respectively;

[0236] The recovery rate of oleanolic acid was 89.57% and the recovery rate of ursolic acid was 90.55% per 1000 ml of the Rishuan lotion obtained in Example 11;

[0237] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 12 was 89.52% and 91.41% respectively;

[0238] The above results show that in the process of preparing the lotion, when verbena and dandelion are extracted separately, the recovery rates of oleanolic acid and ursolic acid are consistent with the quality standard method, and dandelion will not affect the extraction of oleanolic acid and ursolic acid in verbena.

[0239] The method of Experimental Example 2 was used to determine the contents of verbena glycoside and verbena glycoside in the three Rishuan lotions obtained in Examples 10 to 12, and the recovery rates of verbena glycoside and verbena glycoside in the lotions were calculated using the verbena feed medicinal material. The results were as follows:

[0240] The recovery rate of verbena glycosides per 1000 ml of the Rishuan lotion obtained in Example 10 was 86.57%, and the recovery rate of verbena glycosides in the euphorbia pulex was 87.47%;

[0241] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 11 was 85.74%, and the recovery rate of verbena glycosides in the euphorbia pulex was 88.52%;

[0242] The recovery rate of verbena glycosides per 1000 ml of the Rishuan lotion obtained in Example 12 was 85.93%, and the recovery rate of verbena glycosides in the euphorbia pulex was 87.34%;

[0243] The above results show that in the process of preparing the washing solution, when verbena and dandelion are extracted separately, the recovery rate of verbena glycoside and verbena glycoside is significantly higher than the quality standard method (Examples 1 to 3), but slightly lower than the verbena single extraction process (Examples 4 to 6), indicating that dandelion has a certain influence on the extraction of verbena glycoside and verbena glycoside in verbena.

[0244] The inventors tried to investigate the factors that affect the low extraction rate of verbena and verbena glycosides when other materials were co-extracted with verbena, and unexpectedly found that the co-extracted dandelion also had a certain adverse effect on the extraction of verbena and verbena glycosides from verbena, as shown in the following examples.

[0245] The present invention then investigates the effects of both alum and dandelion on verbena extraction.

[0246] Example 13: Preparation of Rishuan Lotion

[0247] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0248] Preparation method:

[0249] The above eight herbs, except alum, dandelion and verbena, are boiled in 550ml of water for 1 hour, filtered and the filtrate is reserved;

[0250] Add 380 ml of water to the residue and boil for 1 hour, filter, then add 260 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0251] Verbena, alum and dandelion were decocted with 170ml, 80ml and 60ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use;

[0252] Combine the three groups of filtrates and let stand for 24 hours;

[0253] Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0254] Example 14: Preparation of Rishuan Lotion

[0255] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0256] Preparation method:

[0257] The above eight herbs, except alum, dandelion and verbena, are boiled in 550ml of water for 1 hour, filtered and the filtrate is reserved;

[0258] Add 360 ml of water to the residue and boil for 1 hour, filter, then add 260 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0259] Verbena, alum and dandelion were decocted with 170ml, 90ml and 70ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use;

[0260] Combine the three groups of filtrates and let stand for 24 hours;

[0261] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0262] Example 15: Preparation of Rishuan Lotion

[0263] Recipe: 48g Sophora flavescens, 28g Verbena, 15g Taraxacum, 15g Cnidium monnieri, 10g Galla chinensis, 35g Stemona bulbus, 10g Zanthoxylum bungeanum and 10g Alum. Excipients: 10g benzoic acid, 0.3g ethylparaben.

[0264] Preparation method:

[0265] The above eight herbs, except alum, dandelion and verbena, are boiled in 500ml of water for 1 hour, filtered and the filtrate is reserved;

[0266] Add 400 ml of water to the residue and boil for 1 hour, filter, then add 290 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use;

[0267] Verbena, alum and dandelion were decocted with 170ml, 80ml and 60ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use;

[0268] Combine the three groups of filtrates and let stand for 24 hours;

[0269] Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

[0270] The content of oleanolic acid and ursolic acid in the three Rishuan lotions obtained in Examples 13 to 15 was determined using the method of Test Example 1, and the recovery rates of oleanolic acid and ursolic acid in the lotions were calculated using the verbena as the raw material. The results were as follows:

[0271] The recovery rate of oleanolic acid was 89.54% and the recovery rate of ursolic acid was 90.33% per 1000 ml of the Rishuan lotion obtained in Example 13;

[0272] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 14 was 90.16% and 91.38% respectively;

[0273] The recovery rate of oleanolic acid and ursolic acid per 1000 ml of the Rishuan lotion obtained in Example 15 was 90.63% and 91.14% respectively;

[0274] The above results show that in the process of preparing the lotion, when verbena is extracted separately with alum and dandelion, the recovery rates of oleanolic acid and ursolic acid are consistent with the quality standard method, and alum and dandelion will not affect the extraction of oleanolic acid and ursolic acid in verbena.

[0275] The method of Experimental Example 2 was used to determine the contents of verbena glycoside and verbena glycoside in the three Rishuan lotions obtained in Examples 13 to 15, and the recovery rates of verbena glycoside and verbena glycoside in the lotions were calculated using the verbena herbal material as feed. The results were as follows:

[0276] The recovery rate of verbena glycosides in every 1000 ml of the Rishuan lotion obtained in Example 13 was 62.13%, and the recovery rate of verbena glycosides in the euphorbia pulex was 66.41%;

[0277] The recovery rate of verbena glycosides per 1000 ml of the Rishuan lotion obtained in Example 14 was 60.54%, and the recovery rate of verbena glycosides in the euphorbia pulex was 67.16%;

[0278] The recovery rate of verbena glycosides per 1000 ml of the Rishuan lotion obtained in Example 15 was 61.37%, and the recovery rate of verbena glycosides in the euphorbia pulex was 65.82%;

[0279] The above results show that, in the process of preparing washing solution, when verbena is extracted separately with alum and dandelion, the recovery rates of verbena glycoside and verbena glycoside are basically the same as the quality standard method (of Examples 1 to 3), indicating that alum and dandelion have an effect on the extraction of verbena glycoside and verbena glycoside in verbena.

[0280] Example 16: Preparation of Rishuan Lotion

[0281] According to the formula and preparation method of Example 5, the only difference is that three batches of verbena materials marked as Verbena A, Verbena B, and Verbena C are used instead of Verbena, and three batches of lotions are obtained, which are respectively called Example 16A, Example 16B, and Example 16C.

[0282] The method of Experimental Example 1 was used to determine the oleanolic acid and ursolic acid in three batches of verbena herbs. The results were as follows:

[0283] Verbena A contains 69.73 mg (0.249%) of oleanolic acid and 108.76 mg (0.388%) of ursolic acid.

[0284] Verbena B contains 63.44 mg (0.227%) of oleanolic acid and 122.57 mg (0.438%) of ursolic acid.

[0285] Verbena C contains 67.52 mg (0.241%) of oleanolic acid and 112.48 mg (0.402%) of ursolic acid.

[0286] The method of Experimental Example 1 was used to determine the oleanolic acid and ursolic acid in three batches of lotions. The results were equivalent to 1000 ml of lotion prepared from 28 g of verbena herb.

[0287] Example 16A washing liquid contains 61.46 mg of oleanolic acid (recovery rate 88.14%) and 98.78 mg of ursolic acid (recovery rate 90.82%).

[0288] The washing liquid of Example 16B contained 56.61 mg of oleanolic acid (recovery rate 89.23%) and 110.14 mg of ursolic acid (recovery rate 89.86%).

[0289] The washing liquid of Example 16C contained 59.91 mg of oleanolic acid (recovery rate 88.73%) and 102.55 mg of ursolic acid (recovery rate 91.17%).

[0290] The method of Experimental Example 2 was used to determine the verbenaside and verbenaside in three batches of verbena herbs. The results were as follows:

[0291] Verbena A contains 88.42 mg (0.316%) of verbenaside and 150.26 mg (0.537%) of verbenaside.

[0292] Verbena B contains 81.27 mg (0.290%) of verbenaside and 138.78 mg (0.496%) of verbenaside.

[0293] The medicinal material Verbena C contains 85.38 mg (0.305%) of verbenaside and 155.84 mg (0.557%) of verbenaside.

[0294] The method of Experimental Example 2 was used to determine the verbenaside and verbenaside in three batches of washing liquid. The results were equivalent to 1000 ml of washing liquid prepared from 28 g of verbena herb.

[0295] The washing liquid of Example 16A contained 80.03 mg of verbena glycoside (recovery rate 90.51%) and 134.83 mg of verbena glycoside (recovery rate 89.73%).

[0296] The washing liquid of Example 16B contained 74.03 mg of verbena glycoside (recovery rate 91.09%) and 125.37 mg of verbena glycoside (recovery rate 90.34%).

[0297] The washing liquid of Example 16C contained 76.72 mg of verbenaside (recovery rate 89.86%) and 142.53 mg of verbenaside (recovery rate 91.46%).

[0298] The results of the above Example 16 show that the method of Example 5 of the present invention can obtain a high recovery rate of verbenaside and verbenaside using different batches of verbena herbs.

[0299] Test Example 3: Quality inspection of Rishuan lotion

[0300] This test example refers to the method set forth in the national drug standard WS-10806 (ZD-0806)-2002-2012Z to prepare the matrine content in the Rishuan lotion.

[0301] Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel was used as filler (Phenomenex Luna C 18 The chromatographic column has a column specification of 4.6 mm × 250 mm, 5 μm, with methanol-water-triethylamine (48:52:0.05) as the mobile phase, a detection wavelength of 220 nm, a column temperature of 35°C, and a theoretical plate number calculated based on the matrine peak that should be no less than 4000.

[0302] Preparation of reference solution: Take an appropriate amount of matrine reference substance, weigh accurately, and add mobile phase to make a solution containing 0.3 mg per 1 ml.

[0303] Preparation of test solution: take the product, shake well, filter, accurately pipette 5 ml of the filtrate, add 1.5 ml of concentrated ammonia test solution, shake and extract with ether 4 times (30 ml, 20 ml, 20 ml), combine the ether solutions, place in a 60°C water bath to evaporate the ether, dissolve the residue with the mobile phase, transfer to a 5 ml volumetric flask, add the mobile phase to the scale, shake well, filter, and take the filtrate.

[0304] Determination method: Accurately pipette 20µl of reference solution and test solution respectively, inject into liquid chromatograph, and determine.

[0305] The standard stipulates that the content of Sophora flavescens in each 1 ml of washing liquid, calculated as matrine (C15H24N2O), should not be less than 0.22 mg.

[0306] It has been determined that:

[0307] The matrine content of the washing liquid of Examples 1 to 3 is 0.27 to 0.30 mg / ml. For example, the matrine content of the washing liquid of Example 1 is 0.287 mg / ml.

[0308] The matrine contents of the wash solutions of Examples 4, 5 and 6 are 0.292 mg / ml, 0.306 mg / ml and 0.288 mg / ml respectively.

[0309] The matrine content of the washing liquids of Examples 7 to 15 is 0.27 to 0.31 mg / ml. For example, the matrine content of the washing liquid of Example 7 is 0.303 mg / ml.

[0310] The matrine contents of the A, B and C lotions of Example 6 were 0.304 mg / ml, 0.292 mg / ml and 0.297 mg / ml respectively.

[0311] The above results show that the matrine contents in the lotions obtained by the different methods described in the present invention are substantially the same and all meet the requirements of the national drug standards.

[0312] In addition, the pH values ​​of all the washing solutions obtained in Examples 1 to 16 were measured, and the results were all within the range of 4.3 to 5.7. For example, the pH values ​​of the three washing solutions in Examples 4 to 6 were 4.93, 4.86, and 5.23, respectively, all meeting the standard requirements.

[0313] Test Example 4: Investigation of the biological properties of Rishuan lotion

[0314] The Rishuan lotion of the present invention has the effects of clearing away heat and detoxifying, promoting dampness and relieving itching, and is clinically used for female vulvar itching or male scrotal eczema. Its ingredients, such as Sophora flavescens, Verbena officinalis, and Cnidium monnieri, have typical biological activity of inhibiting a variety of microorganisms. This test example investigates the activity of the Rishuan lotion of the present invention in inhibiting typical microorganisms.

[0315] 1. Test materials

[0316] Test drugs: The lotions were prepared according to the formula and preparation method of the lotions in Examples 2, 5, and 14, except that benzoic acid and ethyl hydroxybenzoate were not added. Test strains: Escherichia coli, Staphylococcus aureus, Bacillus subtilis, Candida tropicalis, and Aspergillus flavus were purchased from Guizhou University of Traditional Chinese Medicine. Culture medium: Beef extract peptone water culture medium and potato culture medium were purchased from Bio-Inno Biotechnology Co., Ltd.

[0317] 2. Experimental methods

[0318] Preparation of test bacterial solution: inoculate the test bacteria into culture medium (bacteria are inoculated into beef extract peptone water culture medium, molds and yeasts are inoculated into potato culture medium), culture at 37°C and 30°C respectively, and adjust the bacterial and spore concentrations to 5×10e5cFu / ml with sterile water [Wang Hao. Experimental study on the antibacterial effect of ten Chinese herbal medicines including Danshen on pathogenic superficial fungi [J], Ningxia Medical Journal, 1997, 19(4): 193-195].

[0319] Preparation of drug base: Each test tube is filled with 5.0 ml of culture medium, and the test drug samples are added into the culture medium tubes respectively, with the final mass concentrations being 20% ​​(ml / ml), 15%, 10%, 5%, and 2.5%, respectively.

[0320] Control setting: Ordinary culture medium inoculated with bacteria as positive control, ordinary culture medium without bacteria as blank control. Sterilization: Sterilize the drug-based tube and control tube at 0.56kg / cm2 for 30 minutes before inoculation. Inoculation: Inoculate 0.1ml per drug-based tube. Culture: Place the inoculated drug-based tube and control tube in an electric constant temperature incubator for culture (bacteria at 37℃ for 2 days, yeast and mold at 30℃ for 6 days).

[0321] Result determination: Culture bacteria for 3 days and molds for 6 days, and observe the growth results.

[0322] 3. Results

[0323] The experimental results are shown in Table 1, which show that the antibacterial effect of the washing liquid of Example 5 is significantly better than that of the washing liquids of Example 2 and Example 14. Both the positive control and the blank control are normal.

[0324] Table 1: Antibacterial effect results of each test drug (concentration ml / 100ml)

[0325]

[0326] Note: + indicates bacterial growth and the more + the stronger the bacterial growth; - indicates sterile growth.

[0327] The above results show that the biological effect of the washing liquid of Example 5 of the present invention is obviously better than that of other washing liquids.

[0328] The above examples are only preferred embodiments for fully illustrating the present application, and the protection scope of the present application is not limited thereto. Any equivalent substitution or change made by a person skilled in the art based on the present application is within the protection scope of the present application. The protection scope of the present application shall be subject to the claims.

Claims

1. A Rishuan lotion, characterized in that: The invention is prepared from eight medicinal materials including sophora flavescens, verbena, dandelion, cnidium monnieri, gallnut, stemona radix, Chinese prickly ash and alum, and pharmaceutical excipients; the eight medicinal materials and the pharmaceutical excipients are fed in the following proportions by weight: 38-58 parts of sophora flavescens, 18-38 parts of verbena, 5-25 parts of dandelion, 5-25 parts of cnidium monnieri, 5-15 parts of gallnut, 25-45 parts of stemona radix, 5-15 parts of Chinese prickly ash, 5-15 parts of alum, 5-15 parts of benzoic acid and 0.1-0.5 parts of ethyl hydroxybenzoate; the Rishuan lotion is prepared in the following amount to prepare 1000 ml: Add 550-650ml of water to the above eight herbs except alum and verbena and boil for 1 hour, filter and set aside the filtrate; Add 350-450 ml of water to the residue and alum for the first time, boil for 1 hour, filter, then add 250-350 ml of water and boil for 1 hour, filter, and the combined filtrate is used for later use; Verbena was boiled with 80-120ml, 40-80ml and 30-50ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was used for later use; Combine the three groups of filtrates and let stand for 24 hours; Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

2. The Rishuan lotion according to claim 1, characterized in that The proportions of the eight medicinal materials and pharmaceutical excipients are as follows by weight: 45-51 parts of Sophora flavescens, 25-31 parts of Herba Cynanchifoliae, 13-17 parts of Herba Taraxaci, 13-17 parts of Fructus Cnidium, 8-12 parts of Galla chinensis, 30-40 parts of Radix Stemonae, 8-12 parts of Zanthoxylum bungeanum, 8-12 parts of Alum, 7.5-12.5 parts of benzoic acid, and 0.2-0.4 parts of ethylparaben.

3. The Rishuan lotion according to claim 1, characterized in that The proportions of the eight medicinal materials and pharmaceutical excipients in parts by weight are: 48 parts of Sophora flavescens, 28 parts of Herba Lycopodii, 15 parts of Herba Taraxaci, 15 parts of Fructus Cnidium, 10 parts of Galla chinensis, 35 parts of Radix Stemonae, 10 parts of Zanthoxylum bungeanum, 10 parts of Alum, 10 parts of Benzoic acid, and 0.3 parts of Ethylparaben.

4. The Rishuan lotion according to claim 1, characterized in that According to the amount of 1000 ml, it is made by the following formula and preparation method: Prescription: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona 35g, Zanthoxylum bungeanum 10g, Alum 10g, Benzoic acid 10g, Ethylparaben 0.3g; Preparation method: Add 650ml of water to the above eight herbs, except alum and verbena, and boil for 1 hour, filter and set aside the filtrate; The residue and alum were first boiled with 390 ml of water for 1 hour, filtered, then boiled with 280 ml of water for 1 hour, filtered, and the combined filtrate was used for later use; Verbena was boiled with 100ml, 50ml and 30ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use; Combine the three groups of filtrates and let stand for 24 hours; Filter, adjust the pH value to 4.5-5.5 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

5. The Rishuan lotion according to claim 1, characterized in that: According to the amount of 1000 ml, it is made by the following formula and preparation method: Prescription: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona 35g, Zanthoxylum bungeanum 10g, Alum 10g, Benzoic acid 10g, Ethylparaben 0.3g; Preparation method: Add 600ml of water to the above eight herbs except alum and verbena and boil for 1 hour, filter and set aside the filtrate; The residue and alum were first boiled with 400 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use; Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use; Combine the three groups of filtrates and let stand for 24 hours; Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

6. The Rishuan lotion according to claim 1, characterized in that: According to the amount of 1000 ml, it is made by the following formula and preparation method: Prescription: Sophora flavescens 48g, Verbena officinalis 28g, Taraxacum officinale 15g, Cnidium monnieri 15g, Galla chinensis 10g, Stemona 35g, Zanthoxylum bungeanum 10g, Alum 10g, Benzoic acid 10g, Ethylparaben 0.3g; Preparation method: Add 550ml of water to the above eight herbs, except alum and verbena, and boil for 1 hour, filter, and set aside the filtrate; The residue and alum were first boiled with 450 ml of water for 1 hour, filtered, then boiled with 300 ml of water for 1 hour, filtered, and the combined filtrate was used for later use; Verbena was boiled with 100ml, 60ml and 40ml of water respectively for 3 times, each time for 1 hour, filtered and the combined filtrate was reserved for later use; Combine the three groups of filtrates and let stand for 24 hours; Filter, adjust the pH to 4.7-5.3 with hydrochloric acid or sodium hydroxide, add benzoic acid and ethylparaben and dissolve them, add water to 1000 ml to obtain Rishuan lotion.

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