CN111122806A - Quality control method of radix cudraniae medicinal material - Google Patents
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Abstract
The invention discloses a quality control method of a cudrania cochinchinensis medicinal material, and relates to the technical field of traditional Chinese medicinal materials. Comprises (1) microscopic identification of medicinal powder; (2) the ranges of water content, total ash content and extract content of the medicinal materials are as follows: the water content is not more than 13.0%, the total ash content is not more than 6.0%, and the extract is measured by hot dipping method under alcohol-soluble extract measuring method (2201 in the four-part general rule of the Chinese pharmacopoeia 2015 edition), and diluted ethanol is used as solvent, and is not less than 10.0%; (3) identifying by thin-layer chromatography; the positions of the chromatogram of the test sample, which correspond to the chromatogram of the kaempferide reference sample, show fluorescence spots with the same color. The invention establishes a scientific, complete, reliable and effective quality control method for the drug material of radix cudraniae, and the method has strong specificity and good reproducibility; meanwhile, the quality standard of the cudrania cochinchinensis medicinal material is established by adopting the method, and the internal quality and the medication quality of the medicinal material can be effectively evaluated and controlled.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicinal materials, in particular to a quality control method of a cudrania cochinchinensis medicinal material.
Background
The radix Cudraniae is fresh or dried root of Corner of Maclura tricuspidata (Carr.) Burr. or Maclura cochinchinensis (Lour.) of Moraceae. Collected all the year round, the rootlets are cut off, cleaned, used fresh or cut off, sliced and dried in the sun. According to the records of Chuanchuanshi, Bencao Shiyi, Kuo Gen (the prescription of Qianjin for emergency), Chuansha (the preparation of raw herb for medicinal property), Digossypii radix, Laiu Daishi Shi (the record of Lingnan vegetable medicine), 33896, and Zhi (Hunan). Is root of Cudrania tricuspidata or Brookra of Moraceae. Chuan Shi is named in Ling nan Cai Yao Bian (Ling nan Cai Yao Bian). The book "herbal shiyi" carries with "nu cudrania", which means: "Shengjiangnan mountain field. Cudrania tricuspidata, spiny thorn, irregular winter. "compendium of materia Medica": "the tree is small like a Chinese thorny. The leaves are also as small as tussah leaves and can be used for feeding silkworm, the above description is consistent with the case of brothera. The compendium of materia Medica also carries "Cudrania", cloud: "everywhere there is a mountain, which is like fasciculation, dry, loose and straight. The leaves are thick and thick, rounded and sharp. 'paper mulberry, Jiu-layer peel, false litchi, monkey joy, mountain litchi, gold thorn, bird's dead, rat thorn, rice ball , wild plum fruit. Collected all the year round, the rootlets are cut off, cleaned, used fresh or cut off, sliced and dried in the sun.
At present, the cudrania root is mainly used for dispelling wind, dredging collaterals, clearing heat, removing dampness, detoxifying and reducing swelling. The medicine has the functions of treating wind-damp arthralgia, jaundice, stranguria with turbid urine, furuncle, carbuncle and swelling, and the specific efficacy is widely accepted by people. At present, the market begins to develop the medicine containing the cudrania cochinchinensis as the effective component, but the quality of the cudrania cochinchinensis medicinal material is difficult to control due to the lack of a good quality control method, so that the normal production and operation are difficult, and the quality control method needs to be standardized to control the quality of the cudrania cochinchinensis medicinal material. At present, no relevant standard of the drug of radix cudraniae has been established. The prior art only relates to the examination of the properties of the Ningshao medicinal materials (quality standards of Chinese medicinal materials and national medicinal materials in Guizhou province), has low pertinence, and cannot achieve the aim of really controlling the quality of the medicinal materials by using the methods.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a quality control method of a cudrania cochinchinensis medicinal material, which can effectively evaluate and control the internal quality and the medication quality of the medicinal material.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a quality control method of radix Cudraniae comprises (1) identifying the powder of radix Cudraniae by microscopy; the powder is brown yellow, the stone cells are single or grouped, the stone cells are square-like, irregular or round-like, the diameter is about 20-80 mu m, the wall is thick, calcium oxalate square crystals are numerous, the diameter is about 5-30 mu m, the guide tube is mainly a conduit with fringe holes, occasionally appearing reticulate guide tubes and the cork cells are polygonal; (2) the ranges of water content, total ash content and extract content of the medicinal materials are as follows: the water content is not more than 13.0%, the total ash content is not more than 6.0%, and the extract is measured by hot dipping method under alcohol-soluble extract measuring method (2201 in the four-part general rule of the Chinese pharmacopoeia 2015 edition), and diluted ethanol is used as solvent, and is not less than 10.0%; (3) identifying by thin-layer chromatography; the positions of the chromatogram of the test sample, which correspond to the chromatogram of the kaempferide reference sample, show fluorescence spots with the same color.
Wherein, the thin-layer chromatography adopts a silica gel G thin-layer plate, toluene-ethyl acetate-formic acid is used as a developing agent, and 5% aluminum trichloride ethanol solution is used as a color developing agent.
In the invention, the thin-layer chromatography is carried out according to the following operations: respectively dropping 5-10 μ l of sample solution and 5-10 μ l of reference solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid solution at volume ratio of 12-8:5-3:1 as developing agent, taking out, and air drying; spraying 5% ethanol solution of aluminum trichloride, and inspecting under 365nm ultraviolet lamp; spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
Preferably, the volume ratio of the developing solvent toluene-ethyl acetate-formic acid is 10:4: 1.
In the invention, the test sample is prepared by the following method: placing the medicinal powder in a conical flask with a plug, adding methanol, heating and reflux-extracting, cooling, filtering, evaporating the filtrate, dissolving the residue in water, shaking with diethyl ether, removing the diethyl ether solution, adding diluted hydrochloric acid into the water solution, heating and reflux-extracting in water bath, taking out, rapidly cooling, shaking with ethyl acetate, mixing the ethyl acetate solutions, washing with water, collecting the ethyl acetate solution, evaporating to dryness, and dissolving the residue in methanol to obtain a sample solution.
Preferably, the test article is prepared by the following method: taking about 5g of medicinal powder, placing into a conical flask with a plug, adding 50ml of 80% methanol, heating and refluxing for 1 hour, cooling, filtering, evaporating the filtrate to dryness, adding 10ml of water into the residue to dissolve, shaking and extracting with diethyl ether for 2 times, 10ml each time, discarding the ethyl ether solution, adding 10ml of dilute hydrochloric acid into the water solution, heating and refluxing for 1 hour in a water bath, taking out, rapidly cooling, shaking and extracting with ethyl acetate for 2 times, 20ml each time, combining the ethyl acetate solutions, washing with 30ml of water, separately taking the ethyl acetate solution to dryness, and adding 1ml of methanol into the residue to dissolve to obtain a sample solution.
In the invention, the reference substance is prepared by the following method: taking kaempferide reference substance, adding methanol to make into solution containing 1mg per 1ml, and using as reference substance solution.
Compared with the prior art, the invention has the following beneficial effects: the method establishes a scientific, complete, reliable and effective quality control method for the radix cudramiae medicinal material by the microscopic identification of the medicinal material and combining the moisture, the total ash content, the extract and the thin-layer chromatography, and has strong specificity and good reproducibility; meanwhile, the quality standard of the cudrania cochinchinensis medicinal material is established by adopting the method, and the internal quality and the medication quality of the medicinal material can be effectively evaluated and controlled.
Drawings
FIG. 1: microscopic characteristic diagram of the cudrania cochinchinensis medicinal material powder, wherein: 1. stone cells 2, calcium oxalate cubic crystals 3, a conduit 4 with fringe holes, and cork cells;
FIG. 2: the cudrania cochinchinensis is used as a chromatogram in a thin-layer identification method by taking quercetin as a reference substance; in the figure: 1.2 samples (origin: Liuzhou), 3 samples (origin: Guangdong), 4 and a quercetin reference substance;
FIG. 3: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 25 ℃, humidity: when 54 percent of the total content is in the range, the chromatogram is used for thin layer identification; in the figure: 1. sample (producing area: Guangxi), 2, sample (producing area: Guangdong), 3, sample (producing area: Liuzhou), 4 kaempferide reference substance;
FIG. 4: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 5 ℃, humidity: when 63 percent of the total content is in the range of thin layer identification chromatogram; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 kaempferide reference substances;
FIG. 5: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 40 ℃, humidity: when the concentration is 40%, the chromatogram is used for a thin layer identification method chromatogram; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 kaempferide reference substances;
FIG. 6: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 25 ℃, humidity: when 72 percent of the total content is in the range, the chromatogram is used for thin layer identification; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 kaempferide reference substances;
FIG. 7: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 25 ℃, humidity: when 32%, using the chromatogram in thin layer identification method; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 kaempferide reference substances;
FIG. 8: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 25 ℃, humidity: when 54 percent of the total content is in the range, a Qingdao ocean silica gel G plate is used for a thin layer identification method chromatogram; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 kaempferide reference substances;
FIG. 9: the cudrania cochinchinensis uses kaempferol as a reference substance, and the temperature: 25 ℃, humidity: when 54 percent of the total content is in the range, a silica gel G plate is laid by hands to be used for a chromatogram in a thin layer identification method; in the figure: 1.2, 3 samples (producing area: Guangxi), 4 Kaempferide reference substances.
Detailed Description
In order to make the objects and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Examples
1. Experimental apparatus and medicinal materials
The medicinal materials are as follows:
the cudrania is provided by the Guizhou Shengshilongfang pharmaceutical Co. The producing area: (1) guangdong (2) Guangxi (3) Liuzhou; and identified as fresh or dried roots of Maclura tricuspidata (Carr.) Bur. or Maclura cochinchinensis (Lour.) Corner, a family Moraceae. The certificate specimen is stored in Guizhou Shengshi Longfang pharmaceutical products GmbH.
Instruments and reagents:
electronic balance type AUW-220D (Shimadzu, Japan); a numerical control ultrasonic cleaner model KQ-500DE (ultrasonic instruments Co., Ltd., Kunshan city, Jiangsu province); digital display constant temperature water bath HH-4 (national electric appliance Co., Ltd.); type 101-1 constant temperature drying oven (Shanghai Puhong instrument factory), dryer; WFH-201B ultraviolet transmission reflectometry (Shanghai Jingke industries, Ltd.), Oribasi MD-50 type biological microscope and matched imaging system, and conventional microscopic slide blade, slide glass, tweezers, chloral hydrate, diluted glycerol, distilled water, toluene (analytically pure, Chongqing Chundong chemical (group) Ltd.), formic acid (analytically pure, Chongqing Chundong chemical (group) Ltd.), hydrochloric acid (analytically pure, Chongqing Chundong chemical (group) Ltd.), ethanol (analytically pure, Chongqing Chundong chemical (group) Ltd.), ethyl acetate (analytically pure, Tianjin City Damao chemical reagent factory), etc.
Test standard substance:
kaempferide reference substance (content is 93.2%) (China institute for testing and testing food and drug, lot number: 110861-201310); quercetin reference (content is 99.1%) (China institute for food and drug testing, batch number: 10081-.
2. Authentication
2.1 microscopic identification:
the microscopic identification characteristics of the powders obtained by observing and measuring the 3 samples of medicinal materials (Guangdong, Guangxi, Liuzhou) are shown in FIG. 1 and summarized as follows:
the powder was brown-yellow. The stone cells are single or grouped, are square-like, irregular or round-like, have the diameter of about 20-80 mu m and are thicker. The calcium oxalate has a plurality of cubic crystals with a diameter of about 5 to 30 μm. The guide pipe is mainly a guide pipe with a fringe hole and occasionally a reticulate pattern guide pipe. The suberect cells are polygonal.
2.2 thin layer identification
2.2.1 exploratory Studies of control
(1) Thin layer chromatography with quercetin as control substance is performed by the following operation method, and the result is shown in figure 2.
Sampling about 5g of each powder of substances (Liuzhou and Guangdong), placing the powders in conical flasks with plugs, adding 50ml of 80% methanol into each powder, heating and refluxing for 1 hour, cooling, filtering, evaporating the filtrate to dryness, adding 10ml of water into the residues to dissolve the residues, shaking and extracting the residues with diethyl ether for 2 times, 10ml each time, discarding the ethyl ether solution, adding 10ml of diluted hydrochloric acid (the general concentration is 9.5% -10.5%, the same below) into the water solution, heating the water solution in a water bath for 1 hour, taking out the solution, rapidly cooling, shaking and extracting the residues with ethyl acetate for 2 times, 20ml each time, combining the ethyl acetate solutions, washing the ethyl acetate solutions with 30ml of water, discarding the water solution, evaporating the ethyl acetate to dryness, and adding 1ml of methanol into the residues to. Taking quercetin control, adding methanol to obtain solution containing 1mg per 1ml as control solution. Performing thin layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), sucking 5-10 μ l of each of the 3 solutions, respectively dropping on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid (10:8:1) as developing agent, taking out, air drying, spraying with 5% aluminum trichloride ethanol solution, heating at 105 deg.C for several minutes, and inspecting under ultraviolet lamp (365 nm). The spot of the sample is fuzzy and not obvious at the position corresponding to the chromatogram of the reference substance in the chromatogram of the test solution, and the thin-layer identification test is not ideal and needs further research. So the method is not included in the text of the new revised quality standards.
(2) The thin layer chromatography experiment using kaempferol as reference substance is carried out by the following operation method, and the result is shown in figure 3.
Sampling about 5g of each powder of substances (Liuzhou, Guangdong and Guangxi), placing the powders into conical flasks with stoppers, adding 50ml of 80% methanol into each powder, heating and refluxing for 1 hour, cooling, filtering, evaporating the filtrate to dryness, adding 10ml of water into residues to dissolve the residues, shaking and extracting for 2 times by using ether and 10ml each time, discarding the ether solution, adding 10ml of diluted hydrochloric acid into water solution, heating and refluxing for 1 hour in a water bath, taking out the solution, quickly cooling, shaking and extracting for 2 times by using ethyl acetate and 20ml each time, combining the ethyl acetate solutions, washing by using 30ml of water, discarding the water solution, evaporating the ethyl acetate to dryness, adding 1ml of methanol into the residues to dissolve the residues to obtain a sample solution. Adding methanol into kaempferide control to obtain 1mg solution per 1ml as control solution. Performing thin layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), sucking 5-10 μ l of each of the 4 solutions, respectively dropping on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid (10:4:1) as developing agent, taking out, air drying, spraying with 5% aluminum trichloride ethanol solution, heating at 105 deg.C for several minutes, and inspecting under ultraviolet lamp (365 nm). Spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution. The method is listed in the text of the new revision quality standard.
2.2.2 thin layer chromatography methodology durability examination.
① temperature examination of the temperature at room temperature (25 ℃), low temperature (5 ℃) and high temperature (40 ℃) were carried out, and the results were good (see FIGS. 3, 4 and 5)
② examination of humidity the results were good when both high humidity (72%) and low humidity (32%) were examined (see FIGS. 6 and 7)
③ investigation of different thin silica gel G plates two thin silica gel G plates were tested in total, Qingdao ocean chemical Co., Ltd. and hand-laid silica gel G plate (see FIGS. 8 and 9)
And (4) conclusion: under the test condition, spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the control solution. The results show that the separation is good and the spots are clearly developed, so the selection is put into the text of quality standard.
2.3 inspection of moisture
The method comprises selecting radix Cudraniae powder (sieved with No. 2 sieve) of 2.0g at different places, and measuring by the second method of water content determination (0832 in the fourth Productivity of 2015 pharmacopoeia). The sample measurement result is 9.7-10.4%, the highest measurement value is 10.4% according to the moisture measurement result, the limit is set as 120% of the highest measurement value and is 12.5%, and the moisture is determined to be less than 13.0% by combining the factors of medicinal material characteristics, harvesting and processing, storage processes and the like. The samples from different origins were determined as shown in Table 1.
2.4 inspection of Total Ash
The ash content of the powder of radix Cudraniae (sieved by No. 2 sieve) of different producing areas is measured by ash content measurement method (according to 2302 of the four-part general rule of 2015 edition in Chinese pharmacopoeia). The measurement result of the sample is 1.6-4.4%, the highest measurement value is 4.4% according to the measurement result of the total ash content, the limit is set to 120% of the highest measurement value and is 5.3%, and the total ash content is determined to be not more than 6.0% by combining the factors of the characteristics of medicinal materials, the harvesting and processing processes, the storage process and the like. The samples from different origins were determined as shown in Table 1.
2.5 examination of acid-insoluble Ash
The ash content obtained in the total ash content test was measured by an ash content measuring method (the general rule 2302 in the four departments of the edition of the Chinese pharmacopoeia 2015). The test result of the sample is 0.2-1.8%, and the experimental result shows that the ash content of acid incompatibility is low, so the method does not fall into the text of a standard draft. The samples from different origins were determined as shown in Table 1.
2.6 measurement of extract
2.6.1 measurement of Water-soluble extracts: the test sample for determination is pulverized, passed through a second sieve, and mixed uniformly.
(1) Cold soaking method: weighing about 2.0g of radix Cudraniae powder (sample origin: Liuzhou), precisely weighing, placing in a 100ml conical flask, precisely adding 50ml of water, sealing, cold soaking, shaking within the first 6 hours, standing for 18 hours, rapidly filtering with a drying filter, precisely weighing 20ml of subsequent filtrate, placing in an evaporation dish dried to constant weight, drying in a water bath, drying at 105 ℃ for 3 hours, cooling in a drier for 30 minutes, and rapidly precisely weighing. The content (%) of the water-soluble extract in the test sample was calculated from the dried product. The results are shown in Table 2.
(2) Hot dipping method: taking 2.0g of radix Cudraniae powder (sample production place: Liuzhou), precisely weighing, placing in a 100ml conical flask, precisely adding 50ml of water, tightly plugging, weighing, standing for 1 hour, connecting with a reflux condenser tube, heating to boil, and keeping slightly boiling for 1 hour. After cooling, the flask was removed, stoppered, weighed again, the lost weight was made up with water, shaken well and filtered through a dry filter. Precisely measuring 25ml of filtrate, placing the filtrate in an evaporating dish which is dried to constant weight, drying the filtrate by evaporation on a water bath for 3 hours at 105 ℃, placing the filtrate in a dryer for cooling for 30 minutes, rapidly and precisely weighing the filtrate, and calculating the content (%) of the water-soluble extract in the test sample according to the dry product. The results are shown in Table 2.
TABLE 2 Water soluble extract content (%)
| Producing area | Cold dipping method | Hot dipping method |
| Liuzhou tea | 10.9％ | 14.8％ |
And (3) test results: the extract content of radix Cudraniae is higher than that of cold soaking method, so hot soaking method is selected.
2.6.2. Alcohol-soluble extract determination: the measurement is carried out by hot dipping method under the alcohol-soluble extract measurement item. Ethanol, diluted ethanol and 70% ethanol are used as solvents. About 2.0g of cudrania cochinchinensis medicinal material powder (sample production place: Guangdong) to be tested is precisely weighed, 3 parts of cudrania cochinchinensis powder are respectively placed into 100ml conical bottles, 50ml of ethanol (95% ethanol, the same below), diluted ethanol (49.5% -50.5% ethanol, the same below) and 70% ethanol are precisely added, and the mixture is sealed and tested according to the method 2.6.1. The results are shown in Table 3.
TABLE 3 alcohol soluble extract content (%)
| Solvent(s) | Extract of plant |
| Ethanol | 10.4％ |
| 70% ethanol | 15.0％ |
| Dilute ethanol | 15.4％ |
The experimental results are as follows: according to the comparison of the determination results in Table 3, the extract contents of the cudrania root medicinal material in the dilute ethanol and the 70% ethanol are not greatly different, and the dilute ethanol is selected as the solvent in consideration of the cost. Therefore, the extract of Cudrania cochinchinensis (lour.) Merr is measured by hot dipping method in alcohol-soluble extract measuring method, and diluted ethanol is used as solvent.
And (3) determining the extract of the radix cudraniae medicinal material in different producing areas: weighing 2.0g of radix Cudraniae powder (sieved with No. two sieve) from different production places (1: Liuzhou 2: Guangdong 3: Guangxi), precisely weighing 2 parts of the powder, respectively placing the powder into 100ml conical bottles, precisely adding 50ml of diluted ethanol, tightly plugging, and testing according to a method 1.2. The results are shown in Table 1.
Combining with factors such as the origin, harvesting season and processing, the lowest value is 15.4%, the lowest value is 80% of the value and is 12.3%, and combining with factors such as the characteristics, harvesting and storage process, etc., the alcohol-soluble extract hot-dipping method is formulated with diluted ethanol as solvent, which is not less than 10.0%.
TABLE 1 determination results of water, total ash, acid-insoluble ash, and extract of cudrania littoralis
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. A quality control method of radix cudraniae medicinal materials is characterized by comprising the following steps: comprises (1) microscopic identification of medicinal powder; the powder is brown yellow, the stone cells are single or grouped, the stone cells are square-like, irregular or round-like, the diameter is about 20-80 mu m, the wall is thick, calcium oxalate square crystals are numerous, the diameter is about 5-30 mu m, the guide tube is mainly a conduit with fringe holes, occasionally appearing reticulate guide tubes and the cork cells are polygonal; (2) the ranges of water content, total ash content and extract content of the medicinal materials are as follows: the water content is not more than 13.0%, the total ash content is not more than 6.0%, and the extract is measured by hot dipping method under alcohol-soluble extract measuring method (2201 in the four-part general rule of the Chinese pharmacopoeia 2015 edition), and diluted ethanol is used as solvent, and is not less than 10.0%; (3) identifying by thin-layer chromatography; the positions of the chromatogram of the test sample, which correspond to the chromatogram of the kaempferide reference sample, show fluorescence spots with the same color.
2. The quality control method of the radix cudraniae medicinal material according to claim 1, characterized in that: the thin-layer chromatography adopts a silica gel G thin-layer plate, toluene-ethyl acetate-formic acid is used as a developing agent, and 5% aluminum trichloride ethanol solution is used as a color developing agent.
3. The quality control method of the radix cudraniae medicinal material according to claim 2, characterized in that: the thin layer chromatography was performed as follows: respectively dropping 5-10 μ l of sample solution and 5-10 μ l of reference solution on the same silica gel G thin layer plate, developing with toluene-ethyl acetate-formic acid solution at volume ratio of 12-8:5-3:1 as developing agent, taking out, and air drying; spraying 5% ethanol solution of aluminum trichloride, and inspecting under 365nm ultraviolet lamp; spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
4. The quality control method of the radix cudraniae medicinal material according to claim 3, characterized in that: the volume ratio of the developing agent toluene to ethyl acetate to formic acid is 10:4: 1.
5. The quality control method of the radix cudraniae medicinal material according to claim 3, characterized in that: the test sample is prepared by the following method: placing the medicinal powder in a conical flask with a plug, adding methanol, heating and reflux-extracting, cooling, filtering, evaporating the filtrate, dissolving the residue in water, shaking with diethyl ether, removing the diethyl ether solution, adding diluted hydrochloric acid into the water solution, heating and reflux-extracting in water bath, taking out, rapidly cooling, shaking with ethyl acetate, mixing the ethyl acetate solutions, washing with water, collecting the ethyl acetate solution, evaporating to dryness, and dissolving the residue in methanol to obtain a sample solution.
6. The quality control method of the radix cudraniae medicinal material according to claim 5, characterized in that: the test sample is prepared by the following method: taking 5g of medicinal powder, placing in a conical flask with a plug, adding 50ml of 80% methanol, heating and refluxing for 1 hour, cooling, filtering, evaporating the filtrate to dryness, adding 10ml of water into the residue to dissolve, shaking and extracting with diethyl ether for 2 times, 10ml each time, discarding the ethyl ether solution, adding 10ml of dilute hydrochloric acid into the water solution, heating and refluxing for 1 hour in a water bath, taking out, rapidly cooling, shaking and extracting with ethyl acetate for 2 times, 20ml each time, combining the ethyl acetate solutions, washing with 30ml of water, separating the ethyl acetate solutions to dryness, and adding 1ml of methanol into the residue to dissolve to obtain a sample solution.
7. The quality control method of the radix cudraniae medicinal material according to claim 3, characterized in that: the reference substance is prepared by the following method: taking kaempferide reference substance, adding methanol to make into solution containing 1mg per 1ml, and using as reference substance solution.
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Citations (2)
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|---|---|---|---|---|
| CN102707006A (en) * | 2012-05-30 | 2012-10-03 | 涂瑶生 | Quality detection method of cudrania tricuspidata formula granules |
| CN108562683A (en) * | 2018-04-18 | 2018-09-21 | 贵州景诚制药有限公司 | A kind of leek roots drug quality detection method |
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|---|---|---|---|---|
| CN102707006A (en) * | 2012-05-30 | 2012-10-03 | 涂瑶生 | Quality detection method of cudrania tricuspidata formula granules |
| CN108562683A (en) * | 2018-04-18 | 2018-09-21 | 贵州景诚制药有限公司 | A kind of leek roots drug quality detection method |
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