CN115372535A - Thin-layer chromatography detection method for two-day oil - Google Patents
Thin-layer chromatography detection method for two-day oil Download PDFInfo
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- 238000004809 thin layer chromatography Methods 0.000 title claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000009136 dragon's blood Substances 0.000 claims abstract description 18
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to the technical field of medicine quality control, and particularly discloses a thin-layer chromatography detection method for two-day oil. The method comprises the following steps: respectively dropping a test solution and a reference solution of the two-day oil on the same silica gel G plate, developing by using chloroform-ethyl acetate-methanol as a developing agent in a volume ratio of 5-10 to 1-5, taking out, airing, spraying a 5-15% sulfuric acid ethanol solution as a color developing agent, heating until the spots are clearly developed, and placing under an ultraviolet lamp 365nm for inspection. The method can carry out qualitative analysis on the content of the dragon's blood in the two-day oil, thereby carrying out quality control on the dragon's blood in the two-day oil and further effectively standardizing market competition.
Description
Technical Field
The invention belongs to the technical field of medicine quality control, and particularly relates to a thin-layer chromatography detection method of two-day oil.
Background
The two-day oil comprises Mentholum, oleum Menthae Dementholatum and Borneolum Syntheticum, is brownish red clear liquid, has peppermint fragrance, is a pathogenic wind expelling stimulant, and can be used for treating common cold, dizziness due to motion of boat, and abdominal pain due to heatstroke. The peppermint oil is light green liquid or light yellow clear liquid, a large number of colorless crystals are separated out at a low temperature, the peppermint oil has strong peppermint fragrance and cool slightly bitter taste, is spicy and cool, has strong permeability, can be stored for a long time, gradually becomes dark in color and gradually becomes sticky in quality, can be randomly mixed with ethanol, chloroform or ether, and is often used for expelling mosquitoes and relieving body fatigue. Menthol, also called menthol, is a terpenoid organic compound having the chemical formula C 10 H 20 O, menthol is extracted from leaf and stem of herba Menthae, is colorless needle-like or prism-like crystal or white crystalline powder, has special fragrance of herba Menthae, and has two isomers (D-type and L-type) after initial burning, natural menthol is mainly L-isomer (L-menthol), and can be used as flavoring agent for toothpaste, perfume, beverage and candy, and can be used as irritant in medicine, and has effects of refreshing and relieving itching, and can be used as wind-expelling medicine for oral administration for treating headache and inflammation of nose, throat, and larynx, and its ester can also be used in perfume and medicine. Borneolum, borneolum Syntheticum, and Borneolum Syntheticum is prepared from stem and leaf of blumea balsamifera of Compositae or branch and leaf of Cinnamomum camphora of Lauraceae by steam distillation and recrystallization, and has chemical composition of 2-arrowol 10 H 18 O, it can be used for block pattern of coma, conjunctival congestion with swelling and pain, sore throat, aphtha, sore and ulcer with swelling and pain, and unhealed ulcer. In addition, the two-day oil also comprises black oil, and the different colors of the two-day oil indicate that the addition amount of the black oil is obviously different. The black oil is prepared by refining dragon's blood, gardenia charcoal and mugwort leaf charcoal in tea oil, and because the black oil in the two-day oil has large consumption and contains the rare Chinese medicinal material dragon's blood, the quality control of the dragon's blood in the two-day oil is necessary, so that the black oil has the advantages of good quality control, low cost, high quality control, and good quality control effectThe effect standardizes market competition.
Patent CN02129687.1 provides a quality control method of a dragon's blood total flavone preparation, which comprises the following steps: taking the test solution and the reference solution, dropping on a silica gel G thin layer plate, developing by using 13-16. Patent CN200810049281.4 discloses a quality control method of Shaolin rheumatism traumatic injury paste, wherein the quality control method of dragon's blood is as follows: taking the test solution and the reference solution, spotting on a silica gel G thin-layer plate, developing with 95.
At present, no method for controlling the quality of the dragon's blood in the two-day oil exists.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a thin layer chromatography detection method of the two-day oil.
In order to achieve the above object, the present invention provides the following technical solutions:
in one aspect, the invention provides a two-day oil thin layer chromatography detection method, which uses chloroform-ethyl acetate-methanol as a developing agent and a silica gel G plate as a thin layer chromatography plate to perform the two-day oil thin layer chromatography detection.
Specifically, the developing solvent is a chloroform-ethyl acetate-methanol solution with the volume ratio of 5-10.
More specifically, the volume ratio of the developing solvent is 6-10.
Specifically, the method takes a sulfuric acid ethanol solution as a color developing agent.
More specifically, the concentration of the sulfuric acid ethanol solution is 5-15%, preferably 10%.
Specifically, the method comprises the following steps: respectively dropping a test solution and a reference solution of the two-day oil on the same silica gel G plate, developing by using chloroform-ethyl acetate-methanol as a developing agent at a volume ratio of 5-10 to 1-5, taking out, airing, spraying a 5-15% sulfuric acid ethanol solution as a color developing agent, heating until the spots are clearly developed, and placing under an ultraviolet lamp of 365nm for inspection.
Specifically, the preparation method of the test solution comprises the following steps: and (2) adding the two-day oil into a sodium hydroxide solution according to the volume ratio of the two-day oil to the 2% sodium hydroxide solution of 1.
Specifically, the preparation method of the reference solution comprises the following steps: taking a dragon's blood reference medicinal material, adding tea oil according to a material-liquid ratio of 1: the petroleum ether volume ratio is 1.
In some embodiments, the thin-layer chromatography detection method can be used for detecting and identifying the content of the dragon's blood in the two-day oil, so that the quality of the dragon's blood in the two-day oil is controlled.
In some embodiments, for the quality detection of the two-day oil, the quality detection and identification of the menthol crystal and the peppermint oil in the two-day oil are also required, which mainly comprises the following steps: (1) 0.5mL of the two-day oil was diluted to 5mL with ethyl acetate to obtain a test solution. (2) Separately adding ethyl acetate into Mentholum and oleum Menthae Dementholatum control to obtain solution containing 0.01mg per 1mL as control solution. (3) Performing thin layer chromatography (0502 in 2020 th edition of Chinese pharmacopoeia), sucking 1-2 μ L of the above three solutions, respectively dropping on the same silica gel G thin layer plate, developing with benzene-ethyl acetate (19).
Compared with the prior art, the invention has the advantages that:
the method can carry out qualitative analysis on the dragon's blood in the two-day oil, thereby carrying out quality control on the dragon's blood in the two-day oil and further effectively standardizing market competition.
Drawings
FIG. 1 is a diagram showing the results of two days of example 1 (T: 24.2 ℃ C., RH: 52.2%) in which 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 2 is a diagram of two-day oil thin layer chromatography detection results using German Merck thin layer plate (T: 24.6 ℃, RH: 69.2%), wherein 1 is sanguis Draxonis negative control, 2 is sanguis Draxonis control drug, 3 is sample SC80008,4 is sample SC80017,5 is sample SC80019,6 is sample SC80020.
FIG. 3 is a diagram of two-day oil thin-layer chromatography detection results (T: 24.6 ℃, RH: 69.2%) using Qingdao sea thin-layer plates, wherein 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 4 is a diagram of the results of two-day oil thin-layer chromatography detection under the conditions of T:25.1 ℃ and RH:33.6%, wherein 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 5 is a diagram of the results of two-day oil thin-layer chromatography detection under the conditions of T:24.4 ℃ and RH:87.7%, wherein 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 6 is a diagram of the results of two-day oil thin-layer chromatography detection under the conditions of T:8.9 ℃ and RH:70.7%, wherein 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 7 is a diagram of the results of two-day oil thin-layer chromatography detection under the conditions of T:37.1 ℃ and RH:44.6%, wherein 1 is a dragon's blood negative control, 2 is a dragon's blood control medicinal material, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 8 is a diagram of the results of two-day oil thin-layer chromatography detection under the conditions of T:21.6 ℃ and RH:64.7%, wherein 1 is a sanguis Draxonis negative control, 2 is a sanguis Draxonis control drug, 3 is a test sample SC80008,4 is a test sample SC80017,5 is a test sample SC80019,6 is a test sample SC80020.
FIG. 9 shows the results of some samples tested in Experimental example 1 (T: 21.6 ℃, RH: 64.7%), wherein 1. Star group SC80021,2. Star group SC80022,3. Star group SC80023,4. Star group SC80024,5. Star group SC80025,6. Sanguis Draxonis negative control, 7. Sanguis Draxonis control drug, 8. Star group SC80026,9. Star group RC80014, 10. Star group SC80007, 11. Star group PC80009, 12. Star group PC80014.
FIG. 10 shows the results of testing some samples in Experimental example 1 (T: 21.5 ℃, RH: 64.7%), wherein 1. Star group PC80016,2. Star group RC80001,3. Star group RC80007,4. Other companies X2002102, 5. Other companies X2109016. Sanguis Draxonis negative control, 7. Sanguis Draxonis control drug, 8. Other companies X2010110, 9. Other companies X210401, 10. Other companies Y201201, 11. Other companies Y200701, 12. Other companies Y200301.
FIG. 11 shows the results of testing some samples in Experimental example 1 (T: 21.6 ℃, RH: 65.3%), wherein 1 is SC80004,2 is QC80014,3 is QC80021,4 is X210301,5 is X210802, 6 is sanguis Draxonis negative control, 7 is sanguis Draxonis control drug, 8 is X211001, 9 is X21080110 is X210902, 11 is X2009108, 12 is X1911109 is other company.
FIG. 12 shows the results of testing a part of samples in Experimental example 1 (T: 21.6 ℃, RH: 65.3%), wherein 1 is constellation QC80007,2 is constellation SC80012,3 is constellation SC80013,4 is other company X210101, 5 is other company X2005105, 6 is sanguis Draxonis negative control, 7 is sanguis Draxonis control drug, 8 is other company X210701, 9 is other company X21020110 is other company X1906105, 11 is other company X2012112, 12 is other company X210402.
Detailed Description
The present invention will be further illustrated in detail with reference to the following specific examples, which are not intended to limit the present invention but are merely illustrative thereof. The experimental methods used in the following examples are not specifically described, and the materials, reagents and the like used in the following examples are generally commercially available under the usual conditions without specific descriptions.
Experimental Material
1. Experimental reagent: silica gel G precast slabs (Qingdao oceanographic plant, lot # 20210406) (Qingdao oceanographic plant, lot # 20210202), silica gel G precast slabs (German Merck, lot # HX 14868326), petroleum ether (60-90 deg.C) (analytical grade, guangzhou chemical reagent plant, lot # 20200803 20), toluene (analytical grade, guangzhou chemical reagent plant, lot # 20190101), acetone (analytical grade, guangzhou chemical reagent plant, lot # 20210301).
2. An experimental instrument: electronic balance model ME5002T/02 (mettler-toledo (shanghai)), electronic balance model BP-221D (cydocis germany) CAMAG reprostar3 digital imaging system (switzerland camma).
3. Reference medicinal materials: sanguis Draxonis reference medicinal material (batch No. 120906-201611), fructus Gardeniae reference medicinal material (batch No. 120906-201611), folium Artemisiae Argyi reference medicinal material (batch No. 121345-201804), mentholum reference (batch No. 110728-201707), mentholum reference extract (batch No. 111551-201704), and Borneolum Syntheticum reference medicinal material (batch No. 110743-201706) are all purchased from China food and drug testing institute.
4. And (3) testing the sample:
a total of 44 batches of two-day oil samples were collected, 23 from Guangzhou white cloud mountain constellation (pharmaceutical) GmbH, other X18, and other Y3. The batch is listed in Table 1, wherein ^ 1-4 is the batch used for the methodology study.
TABLE 1 two day oil batch List and corresponding manufacturers
5. And (3) a dragon's blood negative control substance: taking fructus Gardeniae, folium Artemisiae Argyi, mentholum oil, mentholum, and Borneolum Syntheticum except sanguis Draxonis according to the standard prescription, and making into sanguis Draxonis negative control sample according to standard process.
Example 1. Two-day oil thin layer chromatography detection method
By examining the extraction solvent and extraction method of the preparation method of the sample solution, preferably the preparation method of the sample solution, and examining the chromatographic conditions such as developing agent, inspection method and sample application amount of the developing conditions, the thin layer identification method finally determined is as follows:
preparing a test solution: extracting 2mL of the product with 2% sodium hydroxide solution 10mL by shaking, adjusting pH of the extractive solution to 3-5 with dilute hydrochloric acid, extracting with chloroform 10mL by shaking, evaporating the extractive solution, and dissolving the residue with ethyl acetate 2mL to obtain a sample solution.
Preparation of reference drug solution: soaking sanguis Draxonis control material 0.4g, oleum Camelliae 4g in crucible for 48 hr, heating to 200 deg.C, refining for 4 hr, filtering, collecting filtrate 200 μ L, dissolving with petroleum ether 10mL, and making into control solution by the same method.
Preparation of negative control solution: taking the negative control sample of sanguis Draxonis with the same amount as the sample, and preparing the negative control solution by the same method.
Thin-layer plate: silica gel G thin layer plate.
Sample application: each 10. Mu.L of the above solution was prepared.
Developing agent: chloroform-ethyl acetate-methanol (8.
The unfolding mode is as follows: and (4) unfolding the upper row.
And (6) inspection: spraying 10% ethanol sulfate solution, slightly heating, and inspecting under ultraviolet lamp (365 nm).
As a result: four batches of the test articles are taken and tested according to the conditions. In the chromatogram of the test solution, the same blue spot appears at the position corresponding to the chromatogram of the control solution. The results were reproducible and the negative control was not significantly interfered, and the results are shown in FIG. 1.
Example 2 methodology examination
1. Comparison of different lamella plates: taking prefabricated silica gel G thin-layer plates of two brands of Germany Merck and Qingdao ocean, and respectively testing according to a proposed method. The results are shown in FIGS. 2-3, and 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, and no interference is observed in the negative control.
2. Comparison of different humidities: the relative humidity of the incubator was adjusted using calcium chloride and distilled water, and the sampled thin-layer plates were developed in incubators with low relative humidity (33.6%) and high relative humidity (87.7%), respectively. The results are shown in FIGS. 4-5, and when tested under the condition of 33.6-87.7% relative humidity, the test sample chromatogram shows spots with the same color at the corresponding positions of the control material chromatogram, and the negative control has no obvious interference.
3. Comparison of different temperatures: the spotted thin layer plates were taken and developed at low temperature (8.9 ℃ in a refrigerator) and high temperature (37.1 ℃ in an incubator), respectively. The results are shown in fig. 6-7, when tested at the temperature of 8.9-37.1 ℃, spots with the same color appear on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference material, and the negative control has no obvious interference.
Comparative example 1.
This comparative example differs from example 1 in that: the developing solvent used was petroleum ether: ethyl acetate (2.
The result is shown in fig. 8, no spot exists on the corresponding position of the chromatogram, and the detection of the dragon's blood can not be carried out.
EXAMPLE 1 sample determination
The 44 test samples were tested as described in example 1 above, and it was found that the oil samples from the individual batches of two days were not acceptable and the spots corresponding to the control spots were not clear enough. The rest batches are in accordance with the regulations, the spots are clear, the separation effect of the method is good, the results are shown in the figures 9-12, and the results are summarized in the table 2.
TABLE 2 thin layer identification results of two-day oil batches
The above are merely embodiments of the present invention, which are described in detail and with particularity, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the present invention, and these changes and modifications are within the scope of the present invention.
Claims (10)
1. A thin layer chromatography detection method of two-day oil is characterized in that: the method takes chloroform-ethyl acetate-methanol as a developing agent and takes a silica gel G plate as a thin layer chromatography plate to carry out thin layer chromatography detection of oil for two days.
2. The method of claim 1, wherein: the developing agent is a chloroform-ethyl acetate-methanol solution with the volume ratio of 5-10.
3. The method of claim 2, wherein: the volume ratio of the developing solvent is 6-10.
4. The method of claim 3, wherein: the volume ratio of the developing solvent is 8.
5. The method of claim 1, wherein: the method takes sulfuric acid ethanol solution as a color developing agent.
6. The method of claim 5, wherein: the concentration of the sulfuric acid ethanol solution is 5-15%.
7. The method of claim 6, wherein: the concentration of the sulfuric acid ethanol solution is 10%.
8. The method according to any one of claims 1 to 7, wherein: the method comprises the following steps: respectively dropping a test solution and a reference solution of the two-day oil on the same silica gel G plate, developing by using chloroform-ethyl acetate-methanol as a developing agent in a volume ratio of 5-10 to 1-5, taking out, airing, spraying a 5-15% sulfuric acid ethanol solution as a color developing agent, heating until the spots are clearly developed, and placing under an ultraviolet lamp 365nm for inspection.
9. The method of claim 8, wherein: the preparation method of the test solution comprises the following steps: and (2) adding sodium hydroxide solution into the two-day oil according to a volume ratio of the two-day oil to the 2% sodium hydroxide solution of 1.
10. The method of claim 8, wherein: the preparation method of the reference substance solution comprises the following steps: taking a dragon's blood reference medicinal material, adding tea oil according to a material-liquid ratio of 1: the petroleum ether volume ratio is 1.
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| CN116173099B (en) * | 2023-04-19 | 2023-09-08 | 广州白云山星群(药业)股份有限公司 | Application of Ertian oil in preparation of product for treating respiratory tract virus infection |
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