CN103487546A - Identification method of flower of sunset abelmoschus - Google Patents
Identification method of flower of sunset abelmoschus Download PDFInfo
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- CN103487546A CN103487546A CN201310394319.2A CN201310394319A CN103487546A CN 103487546 A CN103487546 A CN 103487546A CN 201310394319 A CN201310394319 A CN 201310394319A CN 103487546 A CN103487546 A CN 103487546A
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- hyperin
- quercetin
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- 241001075517 Abelmoschus Species 0.000 title claims abstract description 19
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- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 claims abstract description 40
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Abstract
The invention relates to an identification method of flower of sunset abelmoschus, which comprises the following steps of: by taking rutin, hyperin and quercetin as contrast substances or taking rutin and hyperin as contrast substances, spotting test product solution and contrast drug solution on the same polyamide film, by taking 60-75% glacial acetic acid as the developing agent, developing through aluminium trichloride test solution, viewing under an ultraviolet lamp (365 nm), and developing fluorescent spots of the same colour at the position corresponding to a contrast substance chromatograph in a test product chromatograph. The identification method of flower of sunset abelmoschus provided by the invention has the advantages of being strong in specificity, few in use amounts of drugs and chemical reagents, simple and convenient for operation and good in reproducibility and is applied to identifying all flowers of sunset abelmoschus and identifying whether finished products containing flower of sunset abelmoschus contain flower of sunset abelmoschus.
Description
Technical Field
The invention relates to a method for qualitative and identification of medicinal materials, in particular to a method for identification of a flower of abelmoschus manihot medicinal material.
Background
Abelmoschus manihot is a dry corolla of Abelmoschus manihot of Malvaceae, and has medical records in Jiayou materia Medica and Ben Cao gang mu which have a long medicinal history in China. Sweet and cold in nature, entering kidney and bladder meridians, and used for damp-heat obstruction and stranguria with turbid urine and edema; it is indicated for abscess, deep-rooted carbuncle, swelling and toxin, scald due to hot water or fire.
The flos Abelmoschi Manihot flower mainly comprises hyperoside, isoquercitrin, quercetin, myricetin, rutin, etc. The hyperin has the highest content, has obvious local analgesic effect, can protect myocardial ischemia and cerebral ischemia, can protect liver and stomach mucosa, and has the effects of relieving spasm and pain, reducing blood fat, enhancing immunologic function and the like. Quercetin can be used as medicine, has effects of eliminating phlegm, relieving cough and asthma, lowering blood pressure, enhancing capillary resistance, reducing capillary fragility, and reducing blood lipid. Rutin has antiinflammatory, antiviral, blood vessel resistance maintaining, permeability reducing, and blood vessel fragility reducing effects.
The traditional Chinese medicine standard (2002 edition) of Shandong province collects flower of abelmoschus manihot medicinal materials, magnesium hydrochloride powder is selected for reaction in identification items, flavonoid glycoside in the flower of Shandong province is identified, red to purple red reaction is used as an index, operation is relatively simple, specificity is poor, and the flower of Shandong province can show positive and negative reactions only by different medicinal materials containing flavonoid glycoside components.
The flos Abelmoschi Manihot is newly collected in the pharmacopoeia of the people's republic of China (2010 edition), and the identification method of flos Abelmoschi Manihot is improved. The operation process is as follows: taking 1g of the product powder, adding 20ml of 0.18% hydrochloric acid ethanol solution, placing on a water bath, heating and refluxing for 1 hour, filtering while hot, and concentrating the filtrate to 5ml to be used as a test solution. Taking quercetin control, adding ethanol to make into solution containing 0.5mg per 1ml as control solution. Pipette 1. mu.l of each of the two solutions, drop each on the same silica gel G thin layer plate prepared with 0.5% sodium hydroxide solution, and mix with toluene-ethyl acetate-formic acid 5: 4: and 1, developing with a developing agent, taking out, drying in the air, spraying an aluminum trichloride test solution, and inspecting under an ultraviolet lamp at 365nm to obtain fluorescent spots with the same color at positions corresponding to the color spectrum of a reference substance. The method comprises the steps of removing substituents of hyperin, quercetin-3-glucoside, isoquercitrin and the like which are effective components in the flower of abelmoschus manihot through hydrochloric acid hydrolysis reaction, converting the effective components into quercetin, and identifying the authenticity of medicinal materials by taking a quercetin reference substance as a reference. The method has relatively strong specificity, but has the defects of complicated operation process, various types of used chemical reagents, long identification time and the like, and is not suitable for the requirement of quick inspection in the production process.
In addition, the traditional Chinese medicine market is not countless due to adulteration and secondary and good phenomena. Traditional Chinese medicines are used for treating diseases, and if pseudo medicinal materials or inferior medicinal materials are used for treatment, the treatment effect cannot be achieved, but the condition of an illness can be delayed, even the life is damaged, so that the strengthening of quality management of traditional Chinese medicinal materials and traditional Chinese medicines becomes more and more important work. The traditional Chinese medicinal material identification is difficult, and the specificity of the method directly determines the value of the identification method. Although the identification by adopting a single reference substance has certain specificity, the phenomenon of misjudgment often occurs because the components of the traditional Chinese medicinal materials are complex and a plurality of traditional Chinese medicinal materials contain the same effective component. For example, the traditional Chinese medicinal materials containing quercetin recorded in the pharmacopoeia include herba orostachyos, humifuse euphorbia herb, sedum sarmentosum, perfoliate knotweed herb, desmodium, cacumen biotae, folium ginkgo, semen lepidii, abelmoschus manihot flower and the like, and when the identification method of the abelmoschus manihot medicinal materials is used for identifying the traditional Chinese medicinal materials, characteristic points of the quercetin can appear, so that a false positive result is caused.
Disclosure of Invention
The invention aims to provide a method for identifying a flower of abelmoschus manihot medicinal material, which is simple and convenient to operate, has stronger specificity and good reproducibility, and can quickly and accurately identify the flower of abelmoschus manihot medicinal material.
The identification method of the abelmoschus manihot medicinal material provided by the invention takes rutin, hyperin and quercetin as reference substances and adopts thin-layer chromatography for identification, and the specific method comprises the following steps:
1) preparation of test solution
Taking 0.1-0.5 g of abelmoschus manihot medicinal powder, and adding C1～410ml of monohydric alcohol is fully dissolved and filtered, and the filtrate is taken as a test solution;
2) preparation of control solutions
Taking rutin, hyperoside and quercetin as reference substances, respectively, and adding C1～4Preparing solution containing 0.05-0.1 mg of rutin, 0.1-0.3 mg of hyperin and 0.05-0.1 mg of quercetin in each 1ml by using monohydric alcohol as rutin reference solution, hyperin reference solution and quercetin reference solution;
or,
dissolving rutin, hyperoside and quercetin control in C1～4Preparing a solution containing 0.05-0.1 mg of rutin, 0.1-0.3 mg of hyperin and 0.05-0.1 mg of quercetin in 1ml of monohydric alcohol as a reference solution;
3) identification by thin layer chromatography
Respectively sucking the sample solution and the reference solution by 2-10 mu L, dripping the sample solution and the reference solution on the same polyamide film, taking 60-75% glacial acetic acid as a developing agent, spreading for 6cm, taking out, airing, spraying an aluminum trichloride test solution, drying by hot air, and inspecting under a 365nm ultraviolet lamp; in the chromatogram of the test sample, fluorescent spots of the same color appear at the positions corresponding to the chromatograms of the control samples.
The identification method of the sunset abelmoschus flower medicinal material provided by the invention can also use rutin and hyperin as reference substances and adopts thin-layer chromatography for identification, and the specific method comprises the following steps:
1) preparation of test solution
Taking 0.1-0.5 g of abelmoschus manihot medicinal material powder or finished product powder containing abelmoschus manihot medicinal material equivalent to 0.1-0.5 g of abelmoschus manihot medicinal material, and adding C1～410ml of monohydric alcohol is fully dissolved and filtered, and the filtrate is taken as a test solution;
2) preparation of control solutions
Taking rutin and hyperoside as reference substances, respectively, and adding C1～4Preparing a solution containing 0.05-0.1 mg of rutin and 0.1-0.3 mg of hyperin in each 1ml of monohydric alcohol, and taking the solution as a rutin reference substance solution and a hyperin reference substance solution;
or,
dissolving rutin and hyperoside control in C1～4Preparing a solution containing 0.05-0.1 mg of rutin and 0.1-0.3 mg of hyperin in 1ml of monohydric alcohol as a reference solution;
3) identification by thin layer chromatography
Respectively sucking the sample solution and the reference solution by 2-10 mu L, dripping the sample solution and the reference solution on the same polyamide film, taking 60-75% glacial acetic acid as a developing agent, spreading for 6cm, taking out, airing, spraying an aluminum trichloride test solution, drying by hot air, and inspecting under a 365nm ultraviolet lamp; in the chromatogram of the test sample, fluorescent spots of the same color appear at the positions corresponding to the chromatograms of the control samples.
In the above method of the present invention, the stepThe sufficient dissolution in step 1) is carried out by various conventional dissolution means such as stirring, shaking, heating and the like using C1～4The monohydric alcohol dissolves the effective components of flos Abelmoschi Manihot as much as possible. The simplest and most effective dissolving method is to treat the solution in ultrasonic waves for 20 min.
The identification method of the abelmoschus manihot medicinal material provided by the invention is a typical qualitative analysis method. The experimental results obtained may differ slightly under different experimental environments and conditions. In practice, the experimental conditions in the above-described identification method are allowed to be appropriately adjusted so as to obtain the best experimental results, thereby facilitating identification.
Generally, 70% glacial acetic acid is preferred as a developing agent. The concentration of the developing solvent can be appropriately adjusted according to the actual situation.
If the sample spots are not well developed due to the change of the experimental conditions or the influence of the experimental environment, the thin-layer plate can be properly heated to be beneficial to developing.
The percentage concentration of the invention is volume percentage concentration.
The method for identifying the flower of abelmoschus manihot is not only suitable for identifying single (including dry products, fresh products and different producing areas) flower of abelmoschus manihot medicinal materials from all sources, but also suitable for identifying whether the flower of abelmoschus manihot medicinal materials are contained in various finished products (including single-component and compound finished products) such as human medicines, foods, health care products, cosmetics, veterinary medicines and the like prepared from the flower of abelmoschus manihot medicinal materials from all sources.
The rutin, hyperin and quercetin standard substances used in the invention are prepared by the verification of Chinese medicinal biological products. The identification of the flower of abelmoschus manihot by thin layer chromatography is carried out according to the corresponding regulations of the pharmacopoeia of the people's republic of China (2010 version).
The identification method is mature, and through identification under different experimental conditions and identification comparison of a plurality of batches of abelmoschus manihot medicinal materials with different producing areas and different sources, the medicinal materials can be accurately identified, and the method has strong specificity and good reproducibility. The identification method is further applied to identification of the abelmoschus manihot flowers in the finished products containing the abelmoschus manihot flowers, such as compound abelmoschus manihot granules, and has the advantages of no interference in negative, good specificity and good identification effect.
Compared with the identification method of the sunset abelmoschus flower medicinal material in the existing pharmacopoeia, the identification method of the sunset abelmoschus flower medicinal material has the following advantages.
1. The specificity is stronger. The method simultaneously adopts two reference substances of rutin and hyperin or three reference substances of rutin, hyperin and quercetin as reference substances to identify the sunset abelmoschus flower medicinal material and the finished product containing the sunset abelmoschus flower medicinal material, can more comprehensively reflect the quality information of the medicinal materials, more effectively avoid false positive results and improve the specificity of identification. The quality of the product can be more comprehensively and rapidly checked and judged in the production process, the clinical safety of the abelmoschus manihot medicinal material and the preparation thereof can be better controlled, and the stable and reliable quality of the product is ensured.
2. The preparation method of the test solution is simple. Direct addition of C1～4The monohydric alcohol is obtained by extracting with ultrasonic wave or reflux, and compared with pharmacopeia method, the method needs to prepare ethanol solution of hydrochloric acid, and the ethanol solution of hydrochloric acid is heated and refluxed to make the hydrolysis reaction completely simple and convenient.
3. The identification time is shortened. The whole operation process can be completed within 1 hour, and the pharmacopoeia method requires at least more than 2 hours.
4. The usage amount of medicinal materials and reagents is small. The identification method only needs 0.1-0.5 g of medicinal materials, and the whole detection only needs C1～4A small number of reagents such as monohydric alcohol, glacial acetic acid and aluminum trichloride can be completed, at least 1g of medicinal materials is needed in a pharmacopoeia method, the whole detection relates to a plurality of reagents such as hydrochloric acid, ethanol, toluene, ethyl acetate, formic acid and aluminum trichloride, the use amount of the reagents is large, and the toxicity of an organic solvent is high.
5. The method has high sensitivity. The color development can be obvious only by a small amount of reference substances, and the sensitivity is high.
Drawings
FIG. 1 is a diagram showing the developing effect of thin layer chromatography in example 1.
FIG. 2 is a diagram showing the developing effect of thin layer chromatography in example 2.
FIG. 3 is a diagram showing the developing effect of thin layer chromatography in example 3.
FIG. 4 is a diagram showing the developing effect of thin layer chromatography in example 4.
Detailed Description
Example 1
The sunset abelmoschus flower medicinal material is originated from Bozhou of Anhui province.
Taking 0.1g flos Abelmoschi Manihot powder, adding 10ml methanol, treating in ultrasonic wave for 20min for dissolving, filtering, and collecting filtrate as sample solution; taking rutin, hyperoside and quercetin reference substances, respectively, adding methanol to obtain solutions containing rutin 0.05mg, hyperoside 0.1mg and quercetin 0.05mg per 1ml as reference substance solutions.
Sucking 10 μ L of each of the four solutions, respectively dropping on the same polyamide film, spreading with 60% glacial acetic acid as developing agent at a spreading distance of 6cm, taking out, air drying, spraying aluminum trichloride solution, drying with hot air, and inspecting under 365nm ultraviolet lamp. The chromatogram is shown in FIG. 1, and fluorescent spots of the same color appear at the corresponding positions of the chromatogram of the test solution and the chromatogram of the reference solution, so that the identified medicinal material is flos Abelmoschi Manihot flower.
Example 2
The sunset abelmoschus flower medicinal material comes from Jiangsu xing.
Taking 0.5g flos Abelmoschi Manihot powder, adding 10ml ethanol, treating in ultrasonic wave for 20min for dissolving, filtering, and collecting filtrate as sample solution; adding rutin, hyperoside and quercetin reference substances into ethanol to obtain solution containing rutin 0.05mg, hyperoside 0.1mg and quercetin 0.05mg per 1ml as reference substance solution; another control solution was prepared from Abelmoschus manihot (L.) medic of example 1, Bozhou, Anhui, by the same method.
Sucking the three solutions, respectively dropping the solutions on the same polyamide film at a distance of 6cm with 75% glacial acetic acid as developing agent, taking out, air drying, spraying aluminum trichloride solution, drying with hot air, and inspecting under ultraviolet lamp (365 nm). The chromatogram is shown in FIG. 2, and in the chromatogram of the test solution, fluorescent spots with the same color are displayed at the corresponding positions of the chromatogram of the reference solution, and have no obvious difference from the chromatogram of the reference solution, so that the identified solution is flos Abelmoschi Manihot flower.
Example 3
The sunset abelmoschus flower medicinal material is sourced from Hebei criminal terrace.
Taking 0.5g of flos Abelmoschi Manihot powder, adding 10ml of n-butanol, treating in ultrasonic wave for 20min for dissolving, filtering, and collecting filtrate as sample solution; taking rutin and hyperoside control substances, respectively, and adding n-butanol to obtain solution containing rutin 0.1mg and hyperoside 0.3mg per 1ml as control solution.
Sucking 2 μ L of each of the three solutions, respectively dropping on the same polyamide film, spreading with 75% glacial acetic acid as developing agent at a spreading distance of 6cm, taking out, air drying, spraying aluminum trichloride solution, drying with hot air, and inspecting under ultraviolet lamp (365 nm). The chromatogram is shown in FIG. 3, and fluorescent spots of the same color appear at the corresponding positions of the chromatogram of the test solution and the chromatogram of the reference solution, so that the identified medicinal material is flos Abelmoschi Manihot flower.
Example 4
In this example, the sunset abelmoschus flower medicinal material in the compound sunset abelmoschus granule is identified, and the sunset abelmoschus flower medicinal material is originated from Jiangsu Xinghua.
Prescription: 1000g of sunset abelmoschus flower, 500g of herba patriniae, Hu 240g of rhizoma dioscoreae hypoglaucae, 400g of giant knotweed rhizome, 350g of diverse wormwood herb, 250g of turmeric, 250g of radix bupleuri, 250g of wine-processed rhubarb, 250g of bighead atractylodes rhizome and 200g of prepared polygonum multiflorum.
The preparation method comprises the following steps: extracting flos Abelmoschi Manihot and Curcuma rhizome with ethanol under reflux for 1 hr, filtering, recovering ethanol from filtrate, and concentrating to obtain soft extract; decocting herba Patriniae, rhizoma Dioscoreae Septemlobae, rhizoma Polygoni Cuspidati, herba Artemisiae Anomalae, bupleuri radix, radix et rhizoma Rhei, Atractylodis rhizoma, and radix Polygoni Multiflori Preparata with water twice (1 hr each time), mixing decoctions, adding ethanol, cold precipitating for 24 hr, filtering, recovering ethanol from filtrate, and concentrating; mixing the above two extracts, adding lactose 100g and dextrin 400g, mixing, drying, and making into 1000 g.
Taking 5g of compound abelmoschus manihot granules, adding 10ml of methanol, treating in ultrasonic waves for 20min for full dissolution, and filtering to obtain filtrate as a test solution; adding rutin and hyperoside reference substances into methanol to obtain solution containing rutin 0.1mg and hyperoside 0.3mg per 1ml as reference substance solution; taking 5g of compound abelmoschus manihot granule negative sample except the abelmoschus manihot medicinal material, adding 10mL of methanol, treating in ultrasonic waves for 20min for full dissolution, and filtering to obtain filtrate as a negative control solution.
Sucking the three solutions, respectively dropping the solutions on the same polyamide film at a distance of 6cm with 70% glacial acetic acid as developing agent, taking out, air drying, spraying aluminum trichloride solution, drying with hot air, and inspecting under ultraviolet lamp (365 nm). The chromatogram is shown in FIG. 4, and in the chromatogram of the test solution, fluorescent spots with the same color are displayed at the corresponding positions of the chromatogram of the reference solution, and the negative control sample has no corresponding spots, so that the identified medicinal product contains flos Abelmoschi Manihot.
Claims (4)
1. An identification method of flos Abelmoschi Manihot medicinal material comprises identifying with rutin, hyperoside and quercetin as reference substances by thin layer chromatography, and comprises:
taking 0.1-0.5 g of abelmoschus manihot medicinal powder, and adding C1～410ml of monohydric alcohol is fully dissolved and filtered, and the filtrate is taken as a test solution;
taking rutin, hyperoside and quercetin as reference substances, respectively, and adding C1～4The monohydric alcohol is prepared into a solution containing 0.05-0.1 mg of rutin, 0.1-0.3 mg of hyperin and 0.05-0.1 mg of quercetin per 1ml, and the solution is used as the solutionRutin reference substance solution, hyperin reference substance solution and quercetin reference substance solution; or dissolving rutin, hyperoside and quercetin control in C1～4Preparing a solution containing 0.05-0.1 mg of rutin, 0.1-0.3 mg of hyperin and 0.05-0.1 mg of quercetin in 1ml of monohydric alcohol as a reference solution;
respectively sucking the sample solution and the reference solution by 2-10 mu L, dripping the sample solution and the reference solution on the same polyamide film, taking 60-75% glacial acetic acid as a developing agent, spreading for 6cm, taking out, airing, spraying an aluminum trichloride test solution, drying by hot air, and inspecting under a 365nm ultraviolet lamp; in the chromatogram of the test sample, fluorescent spots of the same color appear at the positions corresponding to the chromatograms of the control samples.
2. An identification method of flos Abelmoschi Manihot medicinal material comprises identifying with rutin and hyperoside as reference by thin layer chromatography, and comprises:
taking 0.1-0.5 g of abelmoschus manihot medicinal material powder or finished product powder containing abelmoschus manihot medicinal material equivalent to 0.1-0.5 g of abelmoschus manihot medicinal material, and adding C1～410ml of monohydric alcohol is fully dissolved and filtered, and the filtrate is taken as a test solution;
taking rutin and hyperoside as reference substances, respectively, and adding C1～4Preparing a solution containing 0.05-0.1 mg of rutin and 0.1-0.3 mg of hyperin in each 1ml of monohydric alcohol, and taking the solution as a rutin reference substance solution and a hyperin reference substance solution; or dissolving rutin and hyperoside control in C1～4Preparing a solution containing 0.05-0.1 mg of rutin and 0.1-0.3 mg of hyperin in 1ml of monohydric alcohol as a reference solution;
respectively sucking the sample solution and the reference solution by 2-10 mu L, dripping the sample solution and the reference solution on the same polyamide film, taking 60-75% glacial acetic acid as a developing agent, spreading for 6cm, taking out, airing, spraying an aluminum trichloride test solution, drying by hot air, and inspecting under a 365nm ultraviolet lamp; in the chromatogram of the test sample, fluorescent spots of the same color appear at the positions corresponding to the chromatograms of the control samples.
3. The method for identifying sunset abelmoschus flower as claimed in claim 1 or 2, wherein the sufficient dissolution is carried out by subjecting the solution to ultrasonic treatment for 20 min.
4. The method for identifying abelmoschus manihot medic material according to claim 1 or 2, wherein the developing solvent is 70% glacial acetic acid.
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| CN104459012A (en) * | 2014-12-26 | 2015-03-25 | 吉林化工学院 | Thin-layer identification method of effective part of flavones of fruit of rosa davurica pall |
| CN113391019A (en) * | 2021-05-08 | 2021-09-14 | 江苏苏中药业集团股份有限公司 | Thin-layer chromatography detection method for abelmoschus manihot medicinal material, extract or preparation |
| CN113391019B (en) * | 2021-05-08 | 2022-11-15 | 苏中药业集团股份有限公司 | Thin-layer chromatography detection method for flos abelmoschi manihot medicinal material, extract or preparation |
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