CN112168940A - Method for extracting water-soluble effective components of oral liquid for treating tetanus septicemia - Google Patents
Method for extracting water-soluble effective components of oral liquid for treating tetanus septicemia Download PDFInfo
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Abstract
The invention discloses a method for extracting water-soluble effective components of a Banlianbaidu oral liquid, which comprises the following steps: respectively placing the traditional Chinese medicine materials of isatis root, forsythia, rhizoma anemarrhenae, patchouli, rhizoma acori graminei, radix rehmanniae, gypsum, rhizoma phragmitis and radix curcumae which form the oral liquid for treating the continuous septicemia in a 50 ℃ oven to be dried to constant weight, and crushing the dried materials into powder; weighing the traditional Chinese medicine powder according to the content of each component in the Banlianbaidu oral liquid, placing the traditional Chinese medicine powder in an extraction tank, adding methanol, soaking for 30min, carrying out ultrasonic extraction for 2-4 h, repeatedly extracting for 3-4 times, and combining extracting solutions; evaporating and concentrating the extract, transferring to a freeze-drying tube for freeze-drying, and storing in a refrigerator at 4 ℃; the extraction method is simple to operate, high in extraction efficiency and good in repeatability, the separated substances have high stability, and the quality of the continuous-toxicity-eliminating oral liquid can be effectively controlled.
Description
Technical Field
The invention relates to the technical field of extraction of effective components of traditional Chinese medicines, in particular to a method for extracting water-soluble effective components of a Banlianbaidu oral liquid.
Background
The oral liquid is prepared by extracting effective components of the Chinese medicinal decoction, and adding additives such as correctant and bacteriostatic agent to obtain sterile or semi-sterile oral liquid preparation; is convenient to take and is suitable for the fast-paced life at present.
The oral liquid consists of 9 medicinal materials of isatis root, forsythia, anemarrhena, patchouli, grassleaf sweelflag rhizome, dried rehmannia root, gypsum, reed rhizome and turmeric root-tuber, and has the effects of clearing away heat and toxic materials, cooling blood and relieving sore throat. The oral liquid takes effective components of radix isatidis leyichun and fructus forsythiae, namely phillyrin, as main active ingredients, the leyichun is a monarch drug and the phillyrin is a ministerial drug, and the two drugs have the effects of clearing heat and removing toxicity, cooling blood and relieving sore throat and can be used as index ingredients to accurately indicate the quality of the oral liquid.
In the prior art, the extraction of effective components of the Banlianbaidu oral liquid generally adopts an immersion extraction method, and pure water is used as a water extracting agent, so that the problems of low extraction efficiency and poor stability of the extracted effective components exist.
It is seen that improvements and enhancements to the prior art are needed.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a method for extracting water-soluble effective components of a Banlian Baidu oral liquid, and aims to solve at least one technical problem in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting water-soluble effective components of a Banlianbaidu oral liquid comprises the following steps:
s01, respectively placing traditional Chinese medicine materials including radix isatidis, fructus forsythiae, rhizoma anemarrhenae, herba pogostemonis, rhizoma acori graminei, radix rehmanniae recen, gypsum, rhizoma phragmitis and radix curcumae which form the oral liquid for treating the continuous septicemia in a 50-DEG C oven to dry to constant weight, and crushing the dried traditional Chinese medicine materials into powder;
s02, weighing the traditional Chinese medicine powder according to the content of each component in the Banlianbaidu oral liquid, placing the powder into an extraction tank, adding methanol, soaking for 30min, carrying out ultrasonic extraction for 2-4 h, repeatedly extracting for 3-4 times, and combining the extracting solutions;
s03, evaporating and concentrating the extracting solution, then transferring the extracting solution to a freeze-drying tube for freeze-drying, and storing the extracting solution in a refrigerator at 4 ℃.
In the method for extracting the water-soluble effective components of the Banlianbaidu oral liquid, in the step S01, the traditional Chinese medicinal materials are crushed to be less than 200 meshes.
In the method for extracting the water-soluble effective components of the Banlianbaidu oral liquid, in the step S02, the weight-volume ratio of the traditional Chinese medicine to the methanol is 1: 8-12.
In the method for extracting the water-soluble effective components of the Banlianbaidu oral liquid, in the step S02, the weight-volume ratio of the traditional Chinese medicines to the methanol is 1: 10.
In the method for extracting the water-soluble effective components of the Banlianbaidu oral liquid, the ultrasonic extraction time in the step S02 is 3 hours, and the extraction times are 3 times.
In the method for extracting the water-soluble effective components of the Banlian Baidu oral liquid, in the step S03, the extracting solution is evaporated and concentrated at 80 ℃ until the original drug concentration is 1 g/mL.
Has the advantages that:
the invention provides a method for extracting water-soluble effective components of a copaia chinensis Baidu oral liquid, which is simple to operate, strong in process controllability, high in efficiency, good in separation effect and good in repeatability, and the separated substances have higher stability and can effectively control the quality of the copaia chinensis Baidu oral liquid.
Drawings
FIG. 1 is a thin layer chromatogram of the effective components of the oral liquid and a reference substance;
wherein, A picture is radix Isatidis, 1 in A picture represents standard solution, 2 represents negative control solution, 3 represents control solution, and 4 and 5 represent test solution;
the B picture is forsythia, wherein 1 in the B picture represents a negative control solution, 2 represents a control medicinal material solution, 3 represents a standard substance solution, and 4 and 5 represent test substance solutions;
the C picture is rhizoma anemarrhenae, wherein 1 in the C picture represents a negative control solution, 2 represents a control medicinal material solution, 3 represents a standard substance solution, and 4 and 5 represent test substance solutions;
the D picture is rhizoma Acori Graminei, wherein 1 represents negative control solution, 2 and 3 represent control medicinal material solution, and 4 and 5 represent test sample solution.
Detailed Description
The invention provides a method for extracting water-soluble effective components of a Banlianbaidu oral liquid, which is further described in detail below by referring to the attached drawings and embodiments in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following embodiments relate to the main apparatus including:
shimadzu model LC-20A high performance liquid chromatograph, Shimadzu corporation, Japan;
DHG-9075A electric heating air-blast drying oven, Shanghai-Heng scientific instruments Co., Ltd;
the alliance JP-100 ultrasonic cleaning instrument, Shenzhen alliance cleaning equipment Limited;
a aviation FTS-100 split type medicine decocting pot, one pot and one hundred drink electric appliance industry Co., Ltd, Chaozhou city;
BSA124S ten thousandth electronic balance, sedolis scientific instruments background ltd;
JCS-6102C one hundredth electronic balance, cinnabar electronics ltd;
FreeZone2.5 lyophilizer, Labconco, USA.
The main reagents and drugs involved include:
the goitrin standard (lot No. 170154) and the phillyrin standard (lot No. 161271) were purchased from the institute of food and drug testing, china; radix Isatidis, fructus forsythiae, rhizoma anemarrhenae, herba Agastaches, rhizoma Acori Graminei, radix rehmanniae, Gypsum Fibrosum, rhizoma Phragmitis, and radix Curcumae all from Beijing Tongrentang national medicine Co., Ltd; silica gel G thin-layer plate, silica gel GF254 thin-layer plate, purchased from Qingdao ocean chemical Co.Ltd; phosphoric acid, acetonitrile and methanol are used as chromatographic purities, and water is ultrapure water. Other reagents and drugs not specifically mentioned are commercially available as usual analytical reagents and drugs.
The invention provides a method for extracting water-soluble effective components of a Chinese medicinal oral liquid for treating the toxin of Chinese medicinal material coptidis, which comprises the following steps:
respectively placing the traditional Chinese medicine materials of isatis root, forsythia, rhizoma anemarrhenae, patchouli, rhizoma acori graminei, radix rehmanniae, gypsum, rhizoma phragmitis and radix curcumae which form the oral liquid for treating the continuous septicemia in a baking oven at 50 ℃ to constant weight, and crushing the powder to powder of less than 200 meshes;
due to the difference of water absorption and the difference of sun drying degree of different types of medicinal materials, the water content of the medicinal materials may have larger difference. The traditional Chinese medicine raw materials are dried to constant weight, and the content of each component can be more accurately quantified during subsequent weighing and balancing, so that the proportion of the obtained product is closer to the original formula. Drying at 50 deg.C will not damage the effective components of Chinese medicinal materials, and can rapidly volatilize water and improve efficiency.
The surface area of the crushed Chinese medicinal materials is increased, so that the effective components in the Chinese medicinal materials are more easily dissolved in the extracting solution; and the components are mixed more uniformly after being crushed, so that the extraction effect is more balanced. The 200-mesh specification is easy to realize, and a common traditional Chinese medicine grinder can realize.
Weighing the traditional Chinese medicine powder according to the content of each component in the Banlianbaidu oral liquid, placing the traditional Chinese medicine powder into an extraction tank, adding methanol with the weight ratio of the traditional Chinese medicine powder to the traditional Chinese medicine powder being 1: 8-12, soaking for 30min, carrying out ultrasonic extraction for 2-4 h, repeatedly extracting for 3-4 times, and combining extracting solutions; in the preferred embodiment, the weight volume ratio of the Chinese medicinal materials to methanol is 1: 10, the ultrasonic extraction time is 3h, and the extraction times are 3 times.
The material-liquid ratio, the extraction time and the extraction times are all important factors influencing the extraction rate, and when the parameters of the material-liquid ratio, the extraction time and the extraction times fall within the ranges, the extraction rate of the crushed Chinese medicinal materials reaches the best range. Especially, when the weight-volume ratio of the traditional Chinese medicine to the methanol is 1: 10, the ultrasonic extraction time is 3h, and the extraction times are 3 times, the extraction efficiency is highest. The incomplete extraction can be caused by too high feed-liquid ratio, too short extraction time and too few extraction times, and the extraction rate is reduced; the ratio of the feed liquid is too high, the solvent is wasted, and the time of subsequent concentration is prolonged; after the single extraction time exceeds 4 hours, the improvement of the extraction is basically not contributed, after the extraction times exceed 4 times, the improvement of the extraction rate is not obvious, the working efficiency is reduced, and the solvent is wasted.
The extract was concentrated by evaporation at 80 ℃ to a crude drug concentration of 1g/mL, transferred to a lyophilization tube, lyophilized, and stored in a refrigerator at 4 ℃. The extract is concentrated and freeze-dried and then preserved, and the stability of the extract is higher, thus being more beneficial to preservation.
The extraction rate of the effective components of the oral liquid for treating the continuous septicemia is equal to the mass of the freeze-dried powder/the dosage multiplied by 100 percent; the following 6 examples are provided to further illustrate the extraction effect of the present invention, and the specific parameters of each example are shown in the following table:
| process parameter | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Ratio of material to |
1∶10 | 1∶10 | 1∶8 | 1∶8 | 1∶9 | 1∶9 |
| Extraction time/ |
3 | 2 | 4 | 3 | 4 | 2 |
| Number of times of |
3 | 4 | 3 | 4 | 4 | 3 |
| Extraction ratio/% | 5.6 | 5.6 | 5.4 | 5.5 | 5.6 | 5.4 |
As shown in the table, the extraction rate of the effective components of the oral liquid for treating septicemia in the examples 1-6 is above 5%, and the extraction efficiency is high.
The test solutions of the following examples were prepared from the final products of example 1.
Example 6 determination of precision and repeatability
Radix isatidis is used as a monarch drug and fructus forsythiae is used as a ministerial drug, so that the effective components of radix isatidis, goivy and fructus forsythiae, namely phillyrin, are main effective components of the oral liquid, and the precision and repeatability of the extract obtained in example 1 are determined by taking goivy and phillyrin as indexes.
6.1 precision
6.1.1 preparation of control solutions:
accurately weighing 10mg of goitrin standard product and 2mg of phillyrin reference product, placing in a 10mL volumetric flask, and adding methanol to obtain 0.2mg/mL solution as reference mother liquor. And (5) diluting 6 gradients of the reference mother liquor in a precise multiple ratio to obtain a standard curve working solution.
6.1.2 preparation of test solutions
Precisely weighing 20g of the freeze-dried powder prepared in the embodiment 1, extracting with ethyl acetate for 6 times, each time with 25mL, combining, evaporating to dryness, dissolving residues with methanol, and fixing the volume to a 10mL volumetric flask to be used as a test solution.
6.1.3 chromatographic conditions:
the chromatographic column is an Agilent Hypersil ODS column (250 mm. times.4.0 mm, 5 μm);
mobile phase: gradient elution with acetonitrile-0.01% phosphoric acid solution: 20/80(0-16mim) → 25/75(16-25min) → 60/40(25-30min) → 100/0(30-33min) → 20/80; flow rate: 1 mL/min; the detection wavelength is 277 nm; the amount of the sample was 20. mu.L.
6.1.4 Standard Curve
And (3) sequentially carrying out sample injection measurement on the 6-gradient reference substance solutions according to the sequence of concentration from low to high, and obtaining a regression equation by taking the peak area as a horizontal coordinate (X) and the concentration as a vertical coordinate (Y).
6.1.5 determination of precision
And (3) sucking 20 mu L of the same reference substance solution, repeatedly injecting samples for 6 times, measuring peak areas, and calculating the RSD value of the goitrin and the phillyrin.
6.1.6 determination of stability
Sampling the test solution for 24h, injecting 20 μ L of the sample for 0, 4, 8, 12 and 24h respectively, and measuring the peak areas of goitrin and phillyrin to obtain the RSD value.
The RSD of the goitrin obtained by 5 times of measurement in different time is 2.7 percent and the RSD of the phillyrin is 2.1 percent by calculation; the effective components of the oral liquid for treating septicemia in example 1 are proved to have good stability within 24 h.
6.1.7 repeatability determination
6 groups of products are respectively extracted according to the scheme of example 1, 3 parts of test solution is prepared for each group of products, the content of goitrin and phillyrin is respectively measured, and RSD values are respectively calculated.
The RSD of the goitrin obtained by measuring 18 parts of the test sample is 2.5 percent and the RSD of the phillyrin is 2.2 percent; the extraction method has good repeatability, and can produce the continuous detoxifying oral liquid with stable quality.
EXAMPLE 7 identification of extract Components
The sample solution in this example was prepared from the concentrated extract of the effective ingredient of the oral liquid of Banlianbaidu extracted in example 1.
7.1 radix Isatidis
Precisely measuring 2mL of the above extract, dissolving in 10mL volumetric flask with methanol, ultrasonically extracting for 30min, filtering, collecting filtrate, evaporating to dryness to obtain residue, dissolving completely in methanol, and making into sample solution. Preparing another radix Isatidis control solution 1g and radix Isatidis-lacking oral liquid 2mL, and preparing the control solution and negative control solution in the same way. Another 1mg of the Yiyichun standard substance is taken and added into a 10mL volumetric flask for constant volume to serve as a standard substance solution. According to thin layer chromatography (general rule 0502), 3. mu.L of each of the above solutions was pipetted onto the same silica gel GF254Spreading petroleum ether (60-90 deg.C) -ethyl acetate (1: 1) as developing agent on the thin layer plate, taking out, air drying, and inspecting under 254nm ultraviolet lamp.
7.2 Forsythia suspensa
Precisely measuring the above extract 20mL, adding ethyl acetate 20mL, ultrasonically extracting for 6 times, collecting ethyl acetate layer, mixing extractive solutions, evaporating in water bath to obtain residue, dissolving with methanol 5mL, and making into sample solution. Another 1g of fructus forsythiae control medicinal material and 20mL of the oral liquid containing fructus forsythiae and having no toxicity are prepared into control medicinal material solution and negative control solution by the same method. Taking forsythin reference substance 1mg, and diluting to 10mL volumetric flask as standard solution. According to thin layer chromatography (general rule 0502), sucking 3 μ L of the above solutions with capillary, respectively dropping on the same silica gel G thin layer plate, developing with chloroform-methanol (8: 1) as developer, taking out, air drying, heating with 10% sulphuric acid ethanol solution as developer, and developing at 105 deg.C until the spots are clear.
7.3 rhizoma anemarrhenae
Precisely measuring 2mL of the above extract, diluting with 30% acetone to a constant volume in a 10mL volumetric flask, performing ultrasonic treatment for 20min, collecting the supernatant as a test solution, and collecting rhizoma anemarrhenae control solution and rhizoma anemarrhenae-deficient Banlianchou oral liquid solution. Taking 1mg of timosaponin BII reference substance, and diluting to a 10mL volumetric flask to obtain the reference substance. According to thin layer chromatography (general rule 0502), 3. mu.L of each of the above solutions was pipetted by capillary and spotted on the same silica gel G thin layer plate. Developing with n-butanol-glacial acetic acid-water (4:1:5), air drying, and heating at 105 deg.C to obtain obvious spot color.
7.4 Acorus tatarinowii Schott
Accurately weighing 2mL of the above extract and 20mL of petroleum ether, performing ultrasonic treatment for 30min, filtering, removing the filter residue, evaporating the filtrate to dryness, and dissolving the residue in 1mL of petroleum ether to obtain a sample. Taking another 1g rhizoma Acori Graminei control medicinal material and rhizoma Acori Graminei-deficient herba Patriniae oral liquid to make into control medicinal material solution and negative control solution. According to thin layer chromatography (general rule 0502), sucking 3 μ L of the above solutions with capillary, respectively dropping on the same silica gel G thin layer plate, spreading with petroleum ether-ethyl acetate (4:1) as developing agent, air drying, standing for 1h, and fumigating with iodine vapor until spots are clear.
The above color development results are shown in FIG. 1, where the thin layer chromatography of each sample and the control show the same color spots at the corresponding positions, and the negative control has no interference.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (6)
1. A method for extracting water-soluble effective components of a Banlianbaidu oral liquid is characterized by comprising the following steps:
s01, respectively placing traditional Chinese medicine materials including radix isatidis, fructus forsythiae, rhizoma anemarrhenae, herba pogostemonis, rhizoma acori graminei, radix rehmanniae recen, gypsum, rhizoma phragmitis and radix curcumae which form the oral liquid for treating the continuous septicemia in a 50-DEG C oven to dry to constant weight, and crushing the dried traditional Chinese medicine materials into powder;
s02, weighing the traditional Chinese medicine powder according to the content of each component in the Banlianbaidu oral liquid, placing the powder into an extraction tank, adding methanol, soaking for 30min, carrying out ultrasonic extraction for 2-4 h, repeatedly extracting for 3-4 times, and combining the extracting solutions;
s03, evaporating and concentrating the extracting solution, then transferring the extracting solution to a freeze-drying tube for freeze-drying, and storing the extracting solution in a refrigerator at 4 ℃.
2. The method of claim 1, wherein in step S01, the herbs are pulverized to a size of 200 meshes or less.
3. The method for extracting water-soluble effective components of Banlianbaidu oral liquid according to claim 1, wherein in step S02, the weight-to-volume ratio of Chinese herbs to methanol is 1: 8-12.
4. The method for extracting water-soluble effective components of Banlianbaidu oral liquid according to claim 2, wherein in step S02, the weight-to-volume ratio of Chinese herbs to methanol is 1: 10.
5. The method for extracting water-soluble effective components of Banlianbaidu oral liquid according to claim 1, wherein the ultrasonic extraction time in step S02 is 3 hours, and the number of extraction times is 3.
6. The method of claim 1, wherein the extraction solution is evaporated and concentrated at 80 ℃ to a crude drug concentration of 1g/mL in step S03.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872325A (en) * | 2006-04-27 | 2006-12-06 | 徐新盛 | Composition of Chinese traditional medicine for treating cold in virulence, and preparation method |
| CN101843884A (en) * | 2010-05-20 | 2010-09-29 | 广州市香雪制药股份有限公司 | Method for testing quality of antiviral oral liquid for treating hand-foot-and-mouth disease |
| CN103245737A (en) * | 2013-04-17 | 2013-08-14 | 杭州老桐君制药有限公司 | Detection method of anti-viral oral liquid |
| CN109432361A (en) * | 2018-12-21 | 2019-03-08 | 安徽东盛友邦制药有限公司 | A kind of preparation method improving antiviral oral liquor effective component |
-
2020
- 2020-10-22 CN CN202011141696.1A patent/CN112168940A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872325A (en) * | 2006-04-27 | 2006-12-06 | 徐新盛 | Composition of Chinese traditional medicine for treating cold in virulence, and preparation method |
| CN101843884A (en) * | 2010-05-20 | 2010-09-29 | 广州市香雪制药股份有限公司 | Method for testing quality of antiviral oral liquid for treating hand-foot-and-mouth disease |
| CN103245737A (en) * | 2013-04-17 | 2013-08-14 | 杭州老桐君制药有限公司 | Detection method of anti-viral oral liquid |
| CN109432361A (en) * | 2018-12-21 | 2019-03-08 | 安徽东盛友邦制药有限公司 | A kind of preparation method improving antiviral oral liquor effective component |
Non-Patent Citations (1)
| Title |
|---|
| 李青山等: "《现代药学实验技术》", 31 August 2006, 中国医药科技出版社 * |
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