CN112881583A - Detection method of gout paste for grid brushing - Google Patents
Detection method of gout paste for grid brushing Download PDFInfo
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- CN112881583A CN112881583A CN202110089042.7A CN202110089042A CN112881583A CN 112881583 A CN112881583 A CN 112881583A CN 202110089042 A CN202110089042 A CN 202110089042A CN 112881583 A CN112881583 A CN 112881583A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract
The invention provides a detection method of grid brushing gout ointment, which is characterized by comprising the following steps: the raw material medicines of the gout plaster comprise phellodendron, raw rhubarb, cyrtomium rhizome, angelica dahurica, clematis root, coptis and borneol; mainly comprises thin layer chromatography and HPLC detection. By adopting the method, various medicinal materials and main components in the grid brushing gout ointment can be detected, so that a foundation is provided for quality standard control of the grid brushing gout ointment, and positive significance is brought to popularization of the grid brushing gout ointment.
Description
Technical Field
The invention relates to the field of national medicines and quality detection thereof.
Background
Qiang doctor considers the grunt oh to be in the category of the basal (gout) diseases. The Tornado wunieri base (wind-blowing pain) is called gout, and the Mowa changli rhodea yuneyi base (burning stone blockage-like pain) belongs to the Qiang doctor 'dudi (blockage disease)'. In recent years, Qiang medicine is used for treating gout to obtain a better curative effect, and according to the pathology of the disease such as Zi (water), Mo (fire) and Muer (rainwater) Jinengzi, fire clearing, rainwater removing, thick taste food detoxification is mainly used, the disease is well developed in four limbs, particularly in the joints of the big toe and the sole of the foot, and is closely related to dysfunction of organs of the spleen, the stomach, the liver and the kidney in Saisaxi house. The fire toxin stones generated by the disordered functions of the Baishizi part, the Heishi part and the fire toxin stones are not normally run and excreted in vivo, but continuously circulate maliciously in vivo, and are continuously accumulated in blood vessels and internal organs to block normally running pipelines, so that blood, water and the like are abnormal, wherein abnormal venom such as abnormal black stone, fire toxin liquid crystals, black fire toxin liquid crystals and the like are main virus-causing body fluids. The life activities of a person are controlled by the quality and quantity of various nutrients, namely, Moss, Sa, Jina and Sumo. After people eat various nutrient substances such as high fat, high protein and the like, under the action of Moss (qi), Sa (blood), Jina (fine substances) and Sumo (body qi) of the body, the nutrient substances are conveyed to the whole body according to the requirements of various parts and pipelines of the human body under normal conditions. The spleen, stomach, liver and kidney are disordered, and the toxic stones are continuously accumulated in blood vessels and internal organs to block normally running pipelines, so that the face is red, dark and painful, the toes are painful, and the pain is not quick. Therefore, the patients with a doctor firstly judge the differentiation and the type, analyze the pathogenic factors, the distribution of the white stone nourishing part and the black stone nourishing part, the influencing factors and the syndrome symptoms related to different differentiation and type, and adopt comprehensive treatment such as diet dietetic restraint, moderate exercise therapy, use of fire-extinguishing agents and toxin-expelling agents, medicines, non-medicines and the like on the basis. The treatment method comprises the steps of firstly enabling a patient to live regularly, not to be fat, sweet, thick and greasy, properly exercise, regulating emotion, and prohibiting the patient from eating extremely icy, pyrogenic, indigestible, strong in irritation and capable of producing qi, drinking aspirin medicines, forbidding foods containing oxalic acid, forbidding drinking wine, forbidding drinking bean foods, avoiding alcoholism and the like. The disease is caused by the abnormal blood and water caused by the fire toxin stones generated after the function of the Baishizi part, the Heishi part and the functional disorder, and the fire toxin stones are continuously accumulated in blood vessels and internal organs; fire-clearing, toxicity-removing and coordination therapies should be used. The fire-extinguishing agent and the toxin-dispelling agent, the abnormal venom such as black stone liquid, fire toxin liquid crystal, black fire toxin liquid crystal and the like correct the unhealthy running embolism pipeline, promote the generation of normal spleen, stomach, liver, kidney, lung, body Moss (qi), Sa (blood), Zi (water), Jina (fine substances) and Sumo (intrinsic qi), and restore the functional state of each viscera organ. According to different differentiation analysis, the elimination and recovery conditions of the syndrome symptoms related to the patient are analyzed, and special medicines and non-medicines are adopted for treatment. The commonly used medicines comprise an external dose of the Rou oh Yougui and an oral dose of the Rou oh Yougui: the grunts oh are scattered according to the ground. Has effects in relieving swelling and pain, softening and resolving hard mass, removing calculus, invigorating lung and spleen, invigorating kidney, promoting diuresis, and removing toxic materials; ziba red shell therapy, Su Xue lard therapy, Qiang ointment therapy applied to the affected part, Qiang medicine steaming therapy, Qiang medicine washing and Qiang medicine bath therapy, Qiang medicine tea beverage therapy, Sadeza washing therapy, acupuncture therapy, and diet regulation therapy. The Qiang medicine performs gout treatment by differentiation and calculation, has abundant clinical experience on gout diagnosis and treatment in different morbidity stages such as hyperuricemia, acute stage, intermission stage, chronic stage and the like, is particularly suitable for researching on moderate and severe gout, intractable gout, fever of unknown reason and tophus rehabilitation, effectively rehabilitates a plurality of gout patients who are ineffectively treated repeatedly, and lays a foundation for completion of the project. Qiang doctor treats the grunt oh according to the scheme of the base (gout) (English gout) (Tophus (plural number is Tophi)) accurately, and the curative effect is unique. Qiang medical practitioners and scholars write and compile Qiang medical treatment Roulu oh Yi-ji (gout) arthritis diagnosis and treatment routine together, and establish clinical diagnosis and comprehensive treatment research of gout and gout typing and individualized diagnosis and treatment technology in different periods.
The Shuge gout ointment is a proved formula of Qiang medicine for hundreds of years, and consists of 6 medicines of raw rhubarb, coptis chinensis, clematis root, phellodendron, cyrtomium rhizome and angelica dahurica root, wherein the clinical application of Qiang medicine hospital in Qiang autonomous county of Qiang of Beichuan is more than 5 years, the total effective rate is up to 98 percent by matching with the application of Shuge gout granules, and no obvious toxic or side effect is found. However, the medicine has no related quality research scheme so far, and may bring certain influence on the popularization of the product in the processes of production, sale and use.
Disclosure of Invention
Therefore, the invention aims to provide a detection method capable of effectively controlling the quality of the grid brushing gout ointment.
Specifically, the invention provides a detection method of gout paste with grids brushed thereon, and raw material medicines of the gout paste comprise 5-20 g of golden cypress, 5-20 g of raw rhubarb, 5-20 g of cyrtomium rhizome, 5-20 g of angelica dahurica, 5-20 g of radix clematidis, 5-20 g of coptis chinensis and 1-5 g of borneol; the method comprises the following thin-layer detection contents of coptis:
(1) extracting the paste with methanol or ethanol to obtain test solution;
(2) taking the coptis as a reference medicinal material, and extracting by the method (1) to obtain a coptis reference medicinal material solution;
(3) and adding a silica gel G thin layer plate to each solution, and detecting by using n-butyl alcohol-glacial acetic acid-water (7:1:2) as a developing agent.
The method for detecting the ointment can effectively develop the components in the ointment and has positive influence on the qualitative detection of the coptis chinensis.
In preliminary experiments, the inventors also used a developing reagent in the chinese pharmacopoeia: cyclohexane-ethyl acetate-isopropanol-methanol-water-triethylamine (3:3.5:1:1.5:0.5:1) but no obvious spots are generated after development, and the inventor also carried out various adjustments on the basis of the pharmacopeia developing agent, but the adjustment is not ideal. The inventor finally selects n-butyl alcohol-glacial acetic acid-water (7:1:2) as a developing agent, so that the corresponding spots of the coptis chinensis can be effectively detected, the spots are clear and visible, no tailing exists, and the developing effect is good.
And Zaoha (phellodendron amurense) for clearing heat. Dry dampness, purge fire, remove toxicity. Treating dysentery due to heat, diarrhea, diabetes, jaundice, flaccidity, 36484m, nocturnal emission, stranguria with turbid urine, hemorrhoid, hematochezia, leucorrhea, hectic fever due to yin-steaming, conjunctival congestion, sore of the mouth and tongue, and pyocutaneous disease and toxic swelling. The method of medication administration: it is indicated for sores with intolerable pain. Rihuazi Bencao: relieving fatigue, treating bone steaming, washing liver, improving eyesight, lacrimation, dry mouth, heart heat, killing infantile malnutrition worm, treating ascariasis and cardiodynia, scabies and tinea, treating rhinorrhea, intestinal wind, and bleeding, and then acute heat with swelling and pain.
The efficacy of Shuge (raw rhubarb) attacks stagnation; clearing away damp-heat; purging fire; cooling the blood; removing blood stasis; the rhubarb from Ben Cao Xin Huo (materia Medica) for removing toxicity has very quick property, runs without guarding, is good at cleaning and accumulating food, harmonizing middle energizer and resolving food stagnation, promoting diuresis and removing food, causing novelty by pushing old people, guiding blood, treating rolling saliva, breaking symptom knots, dissipating hard mass and gathering, relieving pain, eliminating carbuncle, cellulitis and toxic heat, and relieving swelling, which are all contained in spirit.
The Mullergba plant (Cyrtomium fortunei) has the functions and main indications of clearing away heat and toxic materials, killing parasites and stopping bleeding. Can be used for treating pestilence, macula, hematemesis, epistaxis, intestinal wind, hematochezia, bloody dysentery, metrorrhagia, and leukorrhagia. [ FUNCTIONS AND INDICATIONS ] can clear away heat and toxic materials, kill parasites, and stop bleeding. Can be used for treating pestilence, macula, hematemesis, epistaxis, intestinal wind, hematochezia, bloody dysentery, metrorrhagia, and leukorrhagia.
Pi Shi Ji Bo Lu (powder of radix Angelicae Dahuricae and radix Puerariae) has the main functions of dispelling wind-damp, promoting blood circulation, expelling pus, promoting granulation and relieving pain. Can be used for treating headache, toothache, nasosinusitis, hemorrhoid, leucorrhea with red and white discharge, carbuncle, cellulitis, pyocutaneous disease, and skin pruritus,
zibasi (borneol) has the main function: unblocking orifices, dispelling stagnated fire, removing nebula, improving eyesight, relieving swelling and alleviating pain. It is indicated for wind stroke, vomiting, coma due to febrile disease, epilepsy due to convulsion, phlegm-phlegm, qi block, deafness, sore throat, aphtha, otitis media, carbuncle, swelling, hemorrhoid, nebula, and enterobiasis. Zhangjing: the flavor is slightly sweet and pungent, and the patient with the herb has a cool feeling like ice, while the qi and stamina are sharp. This is not hot, and yang is also yin-rich. Excels in dispersing qi, dissipating blood, dissipating fire, dissipating stagnation, inducing resuscitation, repelling nausea, and expelling pathogenic factors from the heart and abdomen. "(" the materia Medica)
Gu Shi Gu Si Bai (Chinese medicine) (Latin Wen name Clematischennsis) has the main functions of dispelling wind and eliminating dampness, dredging collaterals and relieving pain, eliminating phlegm and water and dispersing nodules. The medicine is mainly used for treating gout stubborn arthralgia, rheumatic arthralgia, numbness of limbs, psychroalgia of waist and knees, spasm of muscles and tendons, difficulty in stretching and bending, dermatophytosis, malaria, abdominal mass accumulation, tetanus, tonsillitis and bone sticking pharynx.
What Si Ge Bu (Huang Lian) is drunk to clear heat and dry dampness, purge fire and remove toxicity. Can be used for treating damp-heat distention, fullness, emesis, dysentery, jaundice, hyperpyrexia, coma, excessive heart-fire, vexation, insomnia, hematemesis, epistaxis, conjunctival congestion, acid regurgitation, toothache, diabetes, carbuncle, and furuncle; it is used externally to treat eczema, eczema and purulent ear canal. Huang Lian (Chinese goldthread) processed with wine is good at clearing heat in upper energizer. For conjunctival congestion and aphtha
Beeswax as an auxiliary material in the ointment of the invention can be used as an excipient, and simultaneously has certain pharmacodynamic activity, and the efficacy of the beeswax is mainly as follows: it can be orally administered for relieving asthenia, eliminating turbid pathogen and reducing thirst; the external use can detoxify and detumescence, and the internal use can be used for body deficiency, senilism, hyperlipemia and diabetes; it can be used for external treatment of chapped skin, burn and scald.
In addition, the method also comprises the thin layer detection content of the cyrtomium fortunei:
(1) extracting the paste with methanol or ethanol to obtain test solution;
(2) taking rhizoma Osmundae as reference medicinal material, and extracting by the same method as (1) to obtain rhizoma Osmundae reference medicinal material solution;
(3) each solution was spotted on a silica gel G thin layer plate and examined with cyclohexane-ethyl acetate-formic acid at 12: 2: 0.2 as developing agent.
In preliminary experiments, the inventors also used the developing agent in the literature for Cyrtomium fortunei: chloroform-ethyl acetate-concentrated ammonia test solution (10: 1: 0.1), but has serious tailing phenomenon after development, and spots can not be clearly identified (Zhaoli, et al. Cyrtomium fortunei medicinal material rapid multi-information thin-layer identification method research. Chinese veterinary medicine J. 2020,54(04): 52-55.). After a plurality of attempts, the inventor finally selects cyclohexane-ethyl acetate-formic acid (12: 2: 0.2) as the developing agent, so that the corresponding spots of the cyrtomium fortunei can be clearly seen, no tailing exists, and the developing effect is good.
In addition, the method also comprises the following steps of measuring the content of berberine hydrochloride by HPLC:
(1) extracting the paste with ethanol or acidified methanol in the presence of acid to obtain a test solution;
(2) taking berberine hydrochloride, and preparing a reference substance solution;
(3) HPLC detection conditions:
a chromatographic column: octadecyl bond and silica gel are used as stationary phase;
mobile phase: acetonitrile: phosphoric acid aqueous solution 28: 72.
In the HPLC content detection of berberine hydrochloride, acetonitrile described in the pharmacopoeia method was initially used: the phosphoric acid 32:68 is detected, but the chromatographic peak of the berberine hydrochloride is not separated from the former peak, and the content measurement result has errors. After screening, acetonitrile is selected: the phosphoric acid aqueous solution (28: 72) is used as a mobile phase, has good separation effect on target peaks, and can be used for measuring the content of berberine hydrochloride in the product.
Wherein the acid in item (1) is hydrochloric acid.
Wherein the dosage ratio of the hydrochloric acid to the alcohol is 0.5-2: 100.
Wherein the concentration of the phosphoric acid aqueous solution in the item (2) is 0.01-2%.
Wherein the detection column temperature is selected from 20-30 ℃; the detection wavelength is selected from 265 +/-5 nm.
The preparation method of the grid brushing gout ointment comprises the following steps:
(1) pulverizing the above materials except Borneolum Syntheticum to obtain medicinal powder;
(2) melting Cera flava in hot oil, adding the medicinal powder, and stirring; cooling to below 30 deg.C, adding Borneolum Syntheticum, and cooling.
Wherein the oil is selected from vegetable oils.
By adopting the method, various medicinal materials and main components in the grid brushing gout ointment can be detected, so that a foundation is provided for quality standard control of the grid brushing gout ointment, and positive significance is brought to popularization of the grid brushing gout ointment.
Drawings
FIG. 1 is a thin-layer chromatogram of Coptidis rhizoma, from left to right, comprising test sample, negative control, and control medicinal materials
FIG. 2 is a thin-layer chromatogram of rhizoma Osmundae, 1 sample, 2 negative control, 3 reference materials
FIG. 3 pharmacopoeia method HPLC chromatogram
FIG. 4 HPLC chromatogram of the present invention
Detailed Description
The raw materials used in the examples were as follows:
phellodendron bark: the product is dried bark of Pheliodendron chinensis Schncid of Rutaceae. It is commonly called Chuan Huang Bai. Peeling the bark, removing the coarse bark, and drying in the sun. Standard is recorded in the Chinese pharmacopoeia 2020 edition, part I, page 318. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Raw rhubarb: the product is dried root and rhizome of Rheum palmatum L, Rheum tanguticum Maxim. ex Balf. or Rheum officinale of Polygonaceae. Collecting and digging stems and leaves at late autumn or before germination in spring, removing thin roots, scraping outer skin, cutting into sections or segments, stringing, and drying or directly drying. Standard is recorded in the first part of the "Chinese pharmacopoeia" 2020, page 24. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Clematis root: the product is dried root and rhizome of Clematis chinensis Osbeck, Clematis hexapetala pall or Clematis manshurica Rupr of Ranunculaceae. Collected in autumn, removed silt and dried in the sun. Standard is recorded in the Chinese pharmacopoeia 2020 edition on page 262. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Coptis chinensis: the product is dried rhizome of Coptis chinensis Franch, Coptis deltoidea C.Y.Cheng et Hsiao or Coptis Teeta wall. The three are called Weilian, Yalian and Yunlian respectively. Collected in autumn, removed fibrous root and silt, dried, and knocked to remove dry fibrous root. Standard is recorded in the Chinese pharmacopoeia 2020 edition part I, page 316. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Radix angelicae: the product is dried root of Angelica dahurica (Fisch. ex Hoffm.) Benth.et Hook, f. or Angelica dahurica (Fisch. ex Hoffm.) Benth.et hook.f. var.Formosana (Boiss.) ShanetYuan of Umbelliferae. Standard is recorded in the Chinese pharmacopoeia 2020 edition, page 109. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Rhizoma Osmundae: the product is the dried rhizome and petiole residue of Dryopteris crassirhizophila Nakai of Dryopteridaceae. Collected in autumn, leaf stalks and fibrous roots are cut off, silt is removed, and the tea is dried in the sun. Standard is recorded in the Chinese pharmacopoeia 2020 edition on page 344. The quality standard of the raw materials (medicinal materials) for research and medication is met through inspection.
Example 1 preparation of a paste according to the invention
The following medicines in the formula are prepared: 5-15 g of phellodendron, 5-15 g of raw rhubarb, 5-15 g of cyrtomium rhizome, 5-15 g of angelica dahurica, 5-15 g of clematis root and 5-15 g of coptis root, and are weighed according to the amount. Grinding into fine powder, and sieving with 120 mesh sieve. Note: 1-5 g of borneol is separately ground and stored.
Heating oleum Sesami at I00 deg.C, adding Cera flava, melting, cooling, adding the above medicinal powder, stirring, cooling to 30 deg.C, adding Borneolum Syntheticum, mixing, and packaging.
Example 2 thin layer identification of Coptis chinensis Franch
Removing the back lining layer and the covering, weighing 0.25g of ointment, adding 25ml of methanol, performing ultrasonic treatment for 30 minutes, and filtering to obtain filtrate as a test solution. Taking 0.25g of rhizoma Coptidis as reference material, and making into reference material solution by the same method. Taking berberine hydrochloride reference substance, adding methanol to make solution containing 1ml each as reference substance solution. According to the test of 2020 version Chinese pharmacopoeia thin layer chromatography (general rule 0502), sucking 1ul of each of the three solutions, respectively dropping on the same high performance silica gel G thin layer plate, pre-saturating with concentrated ammonia solution for 20 minutes in an expansion cylinder with n-butanol-glacial acetic acid-water (7:1:2) as developing agent, expanding, taking out, drying, and inspecting under ultraviolet lamp (365 nm). In the chromatogram of the test solution, 3 fluorescence spots are displayed at the positions corresponding to those of the chromatogram of the control solution. The chromatogram is shown in FIG. 1.
Example 3 thin layer identification of Cyrtomium fortunei
Removing the back lining layer and the covering, weighing paste 3g, adding 15ml methanol, ultrasonic treating for 30min, evaporating the filtrate, and dissolving with 2ml methanol to obtain the final product. Weighing 3g of rhizoma Osmundae-free paste, and preparing negative control solution by the same method. Weighing rhizoma Osmundae 0.5g, and making into control solution by the same method. Respectively dropping 6 μ l of test solution, negative control solution and control solution on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate-formic acid (12: 2: 0.2) as developing agent, taking out, air drying, and inspecting under 254nm ultraviolet lamp; the main spots with the same color appear on the chromatogram of the test solution at the corresponding positions of the reference medicinal materials. The chromatogram is shown in FIG. 2.
EXAMPLE 4 Berberine hydrochloride content determination (HPLC)
Measuring by high performance liquid chromatography, and calculating berberine hydrochloride content by external standard method.
Chromatographic conditions
Inertsil ODS-3 Column (4.6X 250mm Column, 5 μm); performing isocratic elution with acetonitrile-0.1% phosphoric acid water solution (28: 72) as mobile phase at 25 deg.C, flow rate of 1mL/min, sample amount of 2 μ L, detection wavelength of 265nm, and theoretical plate number not less than 4000 calculated according to berberine hydrochloride peak.
Preparation of test solution
Precisely weighing 2.5g of paste, placing the paste in a conical flask with a plug, precisely adding 25ml of a mixed solution of methanol-hydrochloric acid (100:1), sealing the plug, weighing, carrying out ultrasonic treatment (power of 250W and frequency of 40kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, and filtering to obtain the ointment.
Preparation of control solutions
Precisely weighing 10mg of berberine hydrochloride standard, placing in a 100ml volumetric flask, adding methanol to scale, and making into 0.1mg/ml berberine hydrochloride standard solution for use.
Methodology investigation
Investigation of linear relationships
Precisely sucking berberine hydrochloride reference substance, and sequentially diluting with methanol to obtain reference substance solutions of 0.05mg/mL, 0.02mg/mL, 0.01mg/mL, 0.008mg/mL, 0.005mg/mL, and 0.002mg/mL as reference substance solutions with different concentrations. And precisely sucking 2 mu L of each reference substance solution respectively for determination, and drawing a standard curve by taking the sample injection mass concentration as an abscissa (X) and the corresponding peak area as an ordinate (Y). The regression equation y of berberine hydrochloride is 55900278.40x-27861.07, and R2 is 0.9996, which shows good linear relation.
And (3) precision test: the sample solution to be tested is precisely absorbed and repeatedly injected for 6 times, each injection is 2 mu L, the RSD of the berberine hydrochloride peak area is 0.30 percent, and the instrument precision is good.
And (3) repeatability test: 6 parts are prepared according to the preparation method of the test solution, and sample injection is carried out according to the chromatographic conditions, so that the RSD of the berberine hydrochloride mass fraction is 1.87 percent, which shows that the method has good repeatability.
And (3) stability test: and (3) taking the test sample solution, and performing sample injection determination for 0, 2, 4, 8, 16 and 24 hours after preparation respectively, wherein the RSD of the berberine hydrochloride peak area is 1.74%, which indicates that the gout granule test sample solution with the grids brushed is stable within 24 hours.
Sample recovery rate test: precisely weighing 6 parts of test sample with known content, each part is about 1.25g, precisely weighing, adding 2ml of 0.1mg/ml berberine hydrochloride reference solution, preparing test solution according to the test sample preparation method, and measuring. Results the recovery rates of berberine hydrochloride in 6 parts of Shuge gout ointment are 85.55%, 86.58%, 83.17%, 83.26%, 83.72%, 85.55% and RSD is 1.70% respectively.
Determination of content
The measurement results of the content of berberine hydrochloride in the Shuge gout ointment are shown in table 1.
TABLE 1 Berberine hydrochloride content determination in Shuge gout granules Table (n ═ 6)
Claims (9)
1. The detection method of the gout plaster for brushing grids is characterized by comprising the following steps: the raw material medicines of the gout plaster comprise phellodendron, raw rhubarb, cyrtomium rhizome, angelica dahurica, clematis root, coptis and borneol; the method comprises the following thin-layer detection contents of coptis:
(1) extracting the paste with methanol or ethanol to obtain test solution;
(2) taking the coptis as a reference medicinal material, and extracting by the method (1) to obtain a coptis reference medicinal material solution;
(3) and adding a silica gel G thin layer plate to each solution, and detecting by using n-butyl alcohol-glacial acetic acid-water (7:1:2) as a developing agent.
2. The detection method according to claim 1, characterized in that: it also includes the thin layer detection content of the basket fern:
(1) extracting the paste with methanol or ethanol to obtain test solution;
(2) taking rhizoma Osmundae as reference medicinal material, and extracting by the same method as (1) to obtain rhizoma Osmundae reference medicinal material solution;
(3) each solution was spotted on a silica gel G thin layer plate and examined with cyclohexane-ethyl acetate-formic acid at 12: 2: 0.2 as developing agent.
3. The detection method according to claim 1, characterized in that: it also comprises the content determination of berberine hydrochloride by HPLC:
(1) extracting the paste with ethanol or acidified methanol in the presence of acid to obtain a test solution;
(2) taking berberine hydrochloride, and preparing a reference substance solution;
(3) HPLC detection conditions:
a chromatographic column: octadecyl bond and silica gel are used as stationary phase;
mobile phase: acetonitrile: phosphoric acid aqueous solution 28: 72.
4. The detection method according to claim 3, characterized in that: (1) in item (1) the acid is hydrochloric acid.
5. The detection method according to claim 4, characterized in that: the dosage ratio of the hydrochloric acid to the alcohol is 0.5-2: 100.
6. The detection method according to claim 3, characterized in that: (2) in the item, the concentration of the phosphoric acid aqueous solution is 0.01-2%.
7. The detection method according to claim 3, characterized in that: the detection column temperature is selected from 20-30 ℃; the detection wavelength is selected from 265 +/-5 nm.
8. The detection method according to claim 1, characterized in that: the preparation method of the gout ointment for brushing grids comprises the following steps:
(1) pulverizing the above materials except Borneolum Syntheticum to obtain medicinal powder;
(2) melting Cera flava in hot oil, adding the medicinal powder, and stirring; cooling to below 30 deg.C, adding Borneolum Syntheticum, and cooling.
9. The detection method according to claim 8, characterized in that: the oil is selected from vegetable oils.
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