CN113759066B - Thin-layer identification method for allium macrostemon test sample - Google Patents
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Abstract
The invention provides a thin-layer identification method of allium macrostemon test samples, which comprises the following steps: preparing allium macrostemon medicinal material, water extract or formula granules into a test solution; and (3) dropping the sample solution on a silica gel G thin layer plate, wherein the volume ratio is (5-6): (3.5-4): (1-1.2): (0.8-1) petroleum ether-ethyl acetate-dichloromethane-formic acid is used as a developing agent, and the mixture is developed, taken out, dried and inspected by an ultraviolet lamp. Compared with the thin layer chromatography information spots in the pharmacopoeia, the method of the invention can obtain more thin layer chromatography information spots, and the thin layer information is rich; and the method has the advantages of clear spots, good separation degree, good reproducibility and the like.
Description
Technical Field
The invention relates to the field of thin-layer identification, in particular to a thin-layer identification method for allium macrostemon samples.
Background
Bulbus Allii Macrostemi is dried bulb of Allium macrostemon Bge or Allium macrostemon G.Don of Liliaceae. The longstamen onion bulb is a traditional common Chinese medicinal material in China, and has warm property, pungent taste and bitter taste. It enters heart, lung, stomach and large intestine meridians. Has effects of resisting tumor, resisting oxidation, inhibiting platelet aggregation, reducing blood lipid, resisting bacteria, relieving spasm and relieving asthma, and can be used for treating coronary heart disease, angina pectoris, bronchial asthma, hyperlipemia and myocardial ischemia. The allium macrostemon medicinal material has the advantages of low toxicity, wide safety range, rich medicinal sources and low price, so the allium macrostemon medicinal preparation has good prospects in strengthening research and development of the allium macrostemon medicinal preparation.
The chemical components of the allium macrostemon are complex and comprise a plurality of components such as steroid saponin, volatile oil, nitrogen-containing compounds, acidic components, polysaccharide, inorganic elements and the like. The steroid saponin is one of the main active ingredients of the allium macrostemon, has various pharmacological effects of inhibiting blood coagulation, resisting tumor, relieving asthma and the like, and is also the material basis of the drug effect of the allium macrostemon. Because the allium macrostemon aqueous extract and the formula particles are prepared from allium macrostemon medicinal materials through a series of processes, wherein some processes can destroy the character characteristics of the original medicinal materials, and an identification method which has good distinguishing and identifying capabilities and is simpler and faster to operate is needed for identifying the traditional Chinese medicine aqueous extract and the formula particles with destroyed characters so as to better control the quality.
The thin-layer chromatography identification method has the advantages of simple and convenient operation and rapidness, and is a better identification method. For allium macrostemon, the current pharmacopoeia records a thin-layer identification method of allium macrostemon medicinal materials, specifically, n-hexane is used as a solvent, n-hexane-ethyl acetate (10.
However, in the thin layer identification method of allium macrostemon in the above pharmacopoeia, the thin layer obtained by inspection has the problems of fuzzy color spots and poor separation effect. Meanwhile, the obtained chromatographic information is less, and especially for allium macrostemon water extract and formula granules, the information is less. In addition, in the existing thin-layer chromatography identification method, a color developing agent needs to be adopted for treatment after development, so that the method is not friendly to operators and the environment.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of fuzzy color spots, poor separation effect and less chromatographic information in the thin-layer chromatography identification in the prior art; thereby providing a thin-layer identification method of the allium macrostemon test sample, which has more chromatographic information, good separation effect, clear color spots and is more friendly to operators.
A thin layer identification method of allium macrostemon test products comprises the following steps:
preparing allium macrostemon medicinal material, water extract or formula granules into a test solution;
and (3) dropping the sample solution on a silica gel G thin layer plate, wherein the volume ratio is (5-6): (3.5-4): (1-1.2): (0.8-1) using petroleum ether-ethyl acetate-dichloromethane-formic acid as a developing agent, developing, taking out, airing, and inspecting by an ultraviolet lamp.
The petroleum ether is medium-boiling point petroleum ether with the boiling point temperature of 60-90 ℃.
The preparation process of the test solution comprises the following steps:
taking the allium macrostemon medicinal material, the water extract or the formula particles, adding water and hydrochloric acid, extracting, cooling, shaking and extracting by using ethyl acetate, and concentrating to obtain a test solution.
The volume ratio of the hydrochloric acid to the water is 3 (30-50).
The addition amount of the ethyl acetate is 1 to 1.5 times of the volume of the water;
the volume after concentration is 2-10% of the original volume.
The extraction mode is heating reflux; the extraction time is 30-90min.
Also comprises the identification of a reference medicinal material solution, and the preparation method of the reference medicinal material solution is the same as that of the test sample solution.
The wavelength viewed by the UV lamp was 365nm.
The Bulbus Allii Macrostemi sample is Bulbus Allii Macrostemi medicinal material, bulbus Allii Macrostemi decoction pieces, bulbus Allii Macrostemi water extract or Bulbus Allii Macrostemi formula granule.
The allium macrostemon aqueous extract is extracted by adopting water as an extraction solvent to obtain an extracting solution, a concentrated solution or dry powder.
The technical scheme of the invention has the following advantages:
1. the invention provides a thin-layer identification method of allium macrostemon samples, which comprises the following steps of: (3.5-4): (1-1.2): (0.8-1) petroleum ether-ethyl acetate-dichloromethane-formic acid is used as a developing agent, and after development and inspection, more thin-layer chromatographic information spots can be obtained compared with those in pharmacopoeia, and the thin-layer information is rich; moreover, the spots are clear, the resolution is good, and the reproducibility is good.
2. The thin-layer identification method provided by the invention is formulated according to the thin-layer identification method of steroid saponins in the allium macrostemon, so that the multi-information of water-soluble components in the allium macrostemon can be better kept, further more thin-layer information in an allium macrostemon water extract or allium macrostemon formula granules is ensured, the quality controllability in the process engineering of allium macrostemon medicinal materials, the water extract and the formula granules is ensured, and the clinical medication curative effect is ensured; meanwhile, a reference picture and a method for identifying the thin layer are provided for various preparations of longstamen onion bulb which is extracted into the medicament by water.
3. The method of the invention does not use color developing agent, and the clear spots can be displayed by direct inspection under the ultraviolet light (365 nm). Compared with the existing identification method, the inspection process is simple, convenient and quick, and the damage to the health of operators and the pollution to the environment are reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a thin-layer identification and inspection result chart of 18 batches of allium macrostemon aqueous extracts in example 1 of the present invention;
FIG. 2 is a diagram of the thin-layer identification and inspection results of three batches of allium macrostemon in example 1 of the present invention;
FIG. 3 is a diagram showing the results of thin-layer chromatography for different sample amounts of a sample solution in example 2 of the present invention;
FIG. 4 is a diagram showing the results of thin-layer identification and inspection of a sample solution under normal temperature and low humidity conditions in example 3 of the present invention;
FIG. 5 is a diagram showing the results of thin-layer identification and inspection under low-temperature and normal-humidity conditions of the sample solution in example 3 of the present invention;
FIG. 6 is a diagram showing the results of thin-layer identification and inspection under high-temperature and high-humidity conditions of the sample solution in example 3 of the present invention;
FIG. 7 is a diagram showing the results of thin-layer chromatography using Merck KGaA on a silica gel G plate according to example 3 of the present invention;
FIG. 8 is a diagram showing the thin-layer identification and inspection results of silica gel G plate of the yellow silica gel development test factory, taiwan Chizhi, 32600;
FIG. 9 is a graph showing the thin-layer discrimination and inspection results of a silica gel G plate obtained by the institute of chemical industry of the cigarette Taiwan city in example 3 of the present invention;
FIG. 10 is a diagram showing the results of thin-layer chromatography for 3 test solutions used in example 4 of the present invention;
FIG. 11 is a diagram showing the results of thin layer identification inspection in example 5 of the present invention;
FIG. 12 is a graph showing the results of thin layer identification inspection of comparative example 1 of the present invention;
FIG. 13 is a graph showing the results of thin layer identification inspection of comparative example 2 of the present invention.
Detailed Description
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The instrument comprises the following steps: CAMAG thin layer imaging system, ME104E electronic balance (Mettler Torlo), JY20002 electronic balance (Mettler Torlo), BSA124S electronic balance (Sidolisi scientific and technical instrument (Beijing) Co., ltd.), BT25S electronic balance (Sidolisi scientific and technical instrument (Beijing) Co., ltd.), DZKW-4 constant temperature water bath (Beijing Zhongxing Weiji apparatus Co., ltd.), KQ-500DB ultrasonic cleaner (Kunshan ultrasonic instrument Co., ltd.), silica gel G plate (Merck KGaA, nicoti institute of chemical industry, nicoti city, chi \32600yellowsilicone development test factory).
Reagent testing: bulbus Allii Macrostemi reference medicinal material (batch No. 121130-201906, china food and drug testing research institute);
the allium macrostemon water extract comprises the following components: placing allium macrostemon decoction pieces with the batch numbers of 200618-725800-01, 200529-724400-02, 200610-713800-03, 200703-725800-04, 200703-725800-05, 200703-043100-06, 200703-043100-07, 200703-725800-08, 200703-043100-093-725800-10, 200703-043100-11, 200703-727000-12, 200703-710000-13, 200703-718-14, 200703-712000-15, 200703-710000-16, 200703-714100-17 and 200703-724400-18 in a marmite, soaking for 30 minutes, adding water with the amount being 6 times of the decoction pieces once the decoction pieces is boiled with strong fire, decocting for 30 minutes with slow fire, filtering while hot, rapidly cooling for standby; adding water with the amount 4 times that of the decoction pieces into the second decoction, boiling the second decoction with strong fire, decocting the second decoction with slow fire for 20 minutes, filtering the second decoction while the second decoction is hot, and quickly cooling the second decoction for later use; the filtrates were combined and concentrated (65 ℃ C.) to a liquor to solids ratio of about 1:1 (relative density of 1.05-1.10), and freeze-drying to obtain the water extract of the corresponding batch.
Allium macrostemon medicinal materials: YC200618-725800-01, YC200529-724400-02 and YC200610-713800-03.
Reagent: petroleum ether (60-90 deg.c), ethyl acetate, dichloromethane, hydrochloric acid and formic acid are analytically pure and water is distilled water.
Example 1
A thin layer identification method for allium macrostemon test products comprises the following specific steps:
1. preparing a test solution:
preparation of a test solution: taking 0.5g of allium macrostemon aqueous extract, grinding, adding 30ml of water and 3ml of hydrochloric acid, heating and refluxing for 1 hour, cooling, extracting with ethyl acetate for 2 times by shaking and 30ml each time, combining ethyl acetate solutions, and concentrating to 5ml to obtain a test solution.
Preparation of a test solution: taking 1.5g of allium macrostemon as a medicinal material, grinding, adding 50ml of water and 3ml of hydrochloric acid, heating and refluxing for 1 hour, cooling, shaking and extracting for 2 times by using ethyl acetate, 30ml of each time, combining ethyl acetate solutions, and concentrating to 5ml to be used as a test solution.
Preparation of a reference medicinal material solution: collecting Bulbus Allii Macrostemi control material 1.5g, grinding, adding water 50ml and hydrochloric acid 3ml, heating and refluxing for 1 hr, cooling, extracting with ethyl acetate shaking for 2 times, 30ml each time, mixing ethyl acetate solutions, and concentrating to 5ml to obtain control solution.
2. Thin layer identification process:
sucking 2 mul of test solution and 1 mul of reference drug, respectively dropping on the same silica gel G thin layer plate, and mixing the solution with 5:3.5:1:0.8 petroleum ether (60-90 ℃) -ethyl acetate-dichloromethane-formic acid as a developing agent, developing, taking out, airing, and inspecting under a 365nm ultraviolet lamp.
In this embodiment, the test solution and the reference solution prepared from the 18 batches of the allium macrostemon water extract and the 3 batches of allium macrostemon medicinal material are respectively inspected, and the inspection results are shown in fig. 1 and fig. 2. In FIG. 1, numbers 1-18 correspond to the 18 batches of the allium macrostemon water extract, and DY corresponds to allium macrostemon control medicinal material; in FIG. 2, numbers 1-3 correspond to the 3 batches of Bulbus Allii Macrostemi in sequence, and DY corresponds to Bulbus Allii Macrostemi control drug.
Example 2
The difference between this embodiment and embodiment 1 is that the allium macrostemon aqueous extract, of which the sample solution is the one obtained in the same manner as in embodiment 1, of which the sample solution is 200618-725800-01, 200529-724400-02 and 200610-713800-03, is prepared, and the sample application amounts of the sample solution and the reference drug solution are different, specifically set as follows: the amounts of spots were 1. Mu.l, 2. Mu.l and 3. Mu.l, respectively, and the results are shown in FIG. 3.
In the figure 3, the numbers 1-3 correspond to 1 mul, 2 mul and 3 mul of the allium macrostemon water extract 200618-725800-01 in sequence, the numbers 4-6 correspond to 1 mul, 2 mul and 3 mul of the allium macrostemon water extract 200618-725800-02 in sequence, the numbers 7-9 correspond to 1 mul, 2 mul and 3 mul of the allium macrostemon water extract 200618-725800-03 in sequence, and the numbers 10-12 correspond to 1 mul, 2 mul and 3 mul of allium macrostemon contrast medicine in sequence.
By examining the sample application amount, when the sample application amount of the allium macrostemon water extract and the allium macrostemon contrast medicinal material are respectively 2 mu l and 1 mu l, the thin-layer chromatography has clear spots and good separation degree. Therefore, the optimal sampling amount of the test solution and the reference solution is 2 mul and 1 mul.
Example 3
This example performed durability verification of the thin layer authentication in example 1, specifically including:
1. investigation of different humiture
The test solutions (allium macrostemon aqueous extract: 200618-725800-01, 200529-724400-02 and 200610-713800-03) prepared in example 1 and the control solutions were developed by the same method as in example 1 under the conditions of normal temperature and low humidity (T: 29 ℃, RH: 10%), low temperature and normal humidity (T: 4 ℃, RH: 60%) and high temperature and high humidity (T: 29 ℃, RH: 80%), and then were dried in the air and placed under an ultraviolet lamp (365 nm) to obtain the results shown in FIGS. 4-6. Numbers 1-3 in the figures 4-6 correspond to water extract 200618-725800-01 of Bulbus Allii Macrostemi, water extract 200529-724400-02 of Bulbus Allii Macrostemi, and water extract 200610-713800-03 of Bulbus Allii Macrostemi, respectively, and number 4 corresponds to reference drug of Bulbus Allii Macrostemi.
2. Investigation of different lamella plates
The test solution (allium macrostemon aqueous extract: 200618-725800-01, 200529-724400-02, 200610-713800-03) prepared in example 1 and the reference drug solution were applied to silica gel G plates from Merck KGaA, nicoti Seisaku Kogyo No. 32600600, and Nicoti Seisaku Kogyo research institute, respectively, and developed under the same conditions as in example 1, taken out, air-dried, and inspected under an ultraviolet lamp (365 nm), and the results are shown in FIGS. 7-9. Numbers 1-3 in the figures 7-9 correspond to water extract 200618-725800-01 of Bulbus Allii Macrostemi, water extract 200529-724400-02 of Bulbus Allii Macrostemi, water extract 200610-713800-03 of Bulbus Allii Macrostemi, and number 4 corresponds to reference drug of Bulbus Allii Macrostemi.
Example 4
The difference between this example and example 1 is that the present invention adopts the same conditions as example 1 to perform the detection of 3 batches of allium macrostemon formula granules; the preparation method of the allium macrostemon formula particle comprises the following steps: decocting Bulbus Allii Macrostemi decoction pieces in water, filtering, concentrating the filtrate to obtain fluid extract, drying (or drying, pulverizing), adding appropriate amount of adjuvant, mixing, and granulating. The process of preparing the test solution by adopting the allium macrostemon formula particles is completely the same as the preparation method of the allium macrostemon aqueous extract in the embodiment 1; the other conditions were the same as in example 1, and the results of testing 3 batches of allium macrostemon granules are shown in fig. 10.
The numbers 1-3 in the figure 10 correspond to the Allium macrostemon formula particle KL200618-725800-01, the Allium macrostemon formula particle KL200529-724400-02 and the Allium macrostemon formula particle KL200610-713800-03 in sequence, and the number 4 corresponds to the Allium macrostemon control drug material.
Example 5
The present example is different from example 4 in the ratio of developing agent, the sample and the amount of spotting thereof in the present example, and the other examples are the same as example 4. The method specifically comprises the following steps: the volume ratio of the developing solvent is 6:4:1.2:1, adopting allium macrostemon formula particles KL200618-725800-01 as a test sample, wherein the sample application amount of the test sample solution is respectively 5 mu l and 10 mu l, and the detection result is shown in figure 11.
The numbers 1-2 in the figure 11 correspond to 5 μ l and 10 μ l of Bulbus Allii Macrostemi formula granule KL200618-725800-01, and the number 3 corresponds to Bulbus Allii Macrostemi control medicinal material.
Comparative example 1
In this embodiment, a method of the first part of the "chinese pharmacopoeia" 2015 edition is adopted to perform thin layer chromatography detection on the allium macrostemon aqueous extract and allium macrostemon control medicinal materials, and the specific process is as follows:
preparation of a test solution: taking 4g of allium macrostemon aqueous extract, adding 20ml of n-hexane, carrying out ultrasonic treatment for 20 minutes, filtering, volatilizing the filtrate, adding 1ml of n-hexane into residues for dissolving, and taking the residues as a test solution.
Preparation of reference drug solution: taking Bulbus Allii Macrostemi control material 4g, adding n-hexane 20ml, ultrasonic treating for 20 min, filtering, volatilizing filtrate, and dissolving residue with n-hexane 1ml to obtain control solution.
Thin-layer chromatography conditions: sucking 10 μ l of each of the test solution and the control solution, respectively dropping on the same silica gel G thin layer plate, developing with n-hexane-ethyl acetate (10). In FIG. 12, number 1 corresponds to the allium macrostemon water extract 200618-725800-01; number 2 corresponds to allium macrostemon control drug.
Comparative example 2
The difference between the present example and comparative example 1 is that the thin layer chromatography detection process is different, and the specific process is as follows:
preparation of a test solution: taking 4g of allium macrostemon aqueous extract, adding 20ml of n-hexane, carrying out ultrasonic treatment for 20 minutes, filtering, volatilizing the filtrate, adding 1ml of n-hexane into residues for dissolving, and taking the residues as a test solution.
Preparation of reference drug solution: taking Bulbus Allii Macrostemi control material 4g, adding n-hexane 20ml, ultrasonic treating for 20 min, filtering, volatilizing filtrate, and dissolving residue with n-hexane 1ml to obtain control solution.
Thin-layer chromatography conditions: sucking 10 μ l of each of the two solutions of the test sample and the control drug, respectively dropping on the same silica gel H thin layer plate, developing with n-hexane-ethyl acetate (10. In FIG. 13, number 1 corresponds to Allium macrostemon aqueous extract 200618-725800-01; number 2 corresponds to allium macrostemon control drug.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A thin layer identification method of allium macrostemon test products is characterized by comprising the following steps:
preparing a test sample of allium macrostemon into a test sample solution;
and (3) spotting the test solution on a silica gel G thin-layer plate, wherein the volume ratio of the silica gel G thin-layer plate to the test solution is (5-6): (3.5-4): (1-1.2): (0.8-1) using petroleum ether-ethyl acetate-dichloromethane-formic acid as a developing agent, developing, taking out, airing, and inspecting by using an ultraviolet lamp;
the preparation process of the test solution comprises the following steps:
taking Bulbus Allii Macrostemi, water extract or formula granule, adding water and hydrochloric acid, extracting, cooling, extracting with ethyl acetate under shaking, and concentrating to obtain test solution.
2. The thin-layer identification method for allium macrostemon samples as claimed in claim 1, characterized in that the petroleum ether is medium-boiling point petroleum ether with a boiling point temperature of 60-90 ℃.
3. The thin-layer identification method for allium macrostemon samples as claimed in claim 1, wherein the volume ratio of the hydrochloric acid to the water is 3 (30-50).
4. The thin-layer identification method for allium macrostemon samples as claimed in claim 1, wherein the addition amount of the ethyl acetate is 1-1.5 times of the volume of water;
the volume after concentration is 2-10% of the original volume.
5. The thin-layer identification method for allium macrostemon samples as claimed in any one of claims 1 to 4, wherein the extraction method is heating reflux; the extraction time is 30-90min.
6. The thin-layer identification method of allium macrostemon samples as claimed in any one of claims 1 to 4, further comprising identification of a reference medicinal material solution, wherein the preparation method of the reference medicinal material solution is the same as that of the sample solution.
7. The method of claim 6, wherein the wavelength of the UV light is 365nm.
8. The thin-layer identification method for allium macrostemon test samples as claimed in claim 1, wherein the allium macrostemon aqueous extract is obtained by extracting allium macrostemon medicinal materials by using water as an extraction solvent to obtain an extracting solution, a concentrated solution or dry powder.
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