CN112903897A - Thin-layer chromatography identification method of Danweikang capsules - Google Patents
Thin-layer chromatography identification method of Danweikang capsules Download PDFInfo
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Abstract
The invention relates to the field of pharmaceutical analysis, and provides a thin-layer chromatography identification method of a Danweikang capsule, which is characterized in that 7 thin-layer chromatography qualitative identification indexes of swertiamarin, wogonin, naringin, neohesperidin, alisol B, 23-acetyl alisol B and pachymic acid which serve as reference substances are added, and identification objects respectively point to 'Danweikang capsule' formula main medicinal materials of swertia mileensis, Scutellaria baicalensis, fructus aurantii, rhizoma alismatis and poria cocos. Compared with the existing drug standard of the 'Danweikang capsule', the invention overcomes the technical defect that the existing standard of the 'Danweikang capsule' has fewer control points on the quality of the identification of the medicinal materials of the formula, provides more comprehensive identification project indexes, has strong specificity, is simple, convenient and quick to operate, has intuitive and clear judgment and objective and reliable conclusion, and provides a technical method for perfecting and improving the drug quality standard of the 'Danweikang capsule' of the national drug and better controlling the drug quality.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a thin-layer chromatography identification method of a gallbladder and stomach health capsule.
Background
The prescription of the national medicine 'Danweikang capsule' is from famous family of national medicine Mr. Hongguang in Baoyuan Tang of Yunnan, and has obvious curative effect on costalgia and jaundice caused by damp-heat in liver and gallbladder, bile reflux gastritis, cholecystitis and the like in clinical application for more than 40 years. The prescription comprises 10 medicinal materials of mile swertia herb, bitter orange, southwestern baical skullcap root, bamboo leaf bupleurum, white paeony root, oriental waterplantain rhizome, Indian buead, virgate wormwood herb, common lophatherum herb and rush, wherein the mile swertia herb, the southwestern baical skullcap root, the bamboo leaf bupleurum and the like are characteristic national medicinal materials in Yunnan. The prescription composition and the preparation method of the product are protected by the invention patent of 'a medicine for treating gallbladder and stomach diseases and a preparation method thereof' (ZL 200410022327.5).
According to the original prescription handed down by the family of the Setarian, the national medicine preparation 'Danweikang capsule' was developed by the original family at the end of the last century in Yunnan Baoyuan Tang, and the 'national medicine standard character Z20025134' batch was obtained. It has effects of dispersing stagnated liver qi, promoting bile flow, and clearing away damp-heat, and can be used for treating hypochondriac pain and jaundice due to damp-heat in liver and gallbladder, and bile reflux gastritis and cholecystitis with the above symptoms.
The 'Danweikang capsule' drug standard WS-10124 (ZD 0124) -2002-2012Z qualitative identification only uses 4 thin-layer chromatography identifications using oleanolic acid, white paeony root glycoside, baicalin and rhizoma alismatis as reference substances, the identification targets respectively point to the constituent drugs of swertia mileensis, white paeony root, southwestern radix scutellariae and rhizoma alismatis, and the other 6 drugs have no corresponding identification methods. In the existing identification method, oleanolic acid is a common component contained in various medicinal materials such as swertia mileensis, glossy privet fruit, anemone rhizome and the like, and the specificity of the identification method using oleanolic acid as the point swertia mileensis is not strong. The alisma orientale is taken as a reference substance, so that the problems that spots are more and difficult to correspond one to one and the result judgment is difficult exist.
The quality control of traditional Chinese medicine is an important measure for guaranteeing the safety of the medicine, and establishing objective, multidimensional and reliable quality control points by using the modern medicine analysis technology is an important way for improving the quality management level of the traditional Chinese medicine. The prescription of the product comprises 10 medicinal materials, the existing drug standard only points to qualitative identification items of 4 medicinal materials, and the difference between the qualitative identification items and the actual requirements of the quality control of the traditional Chinese medicine is large.
According to the representative components contained in the main medicine taste of the prescription of the 'Danweikang capsule', on the basis of the existing medicine standard, swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid which have strong specificity to the raw medicinal materials are selected as reference substances, more and more comprehensive thin-layer chromatography identification items are added, and a technical method is provided for perfecting and improving the medicine quality standard of the national medicine 'Danweikang capsule'.
Disclosure of Invention
The invention aims to provide a thin-layer chromatography identification method of a gallbladder and stomach health capsule.
The purpose of the invention is realized as follows:
a thin-layer chromatography identification method of a gallbladder and stomach-recovering capsule comprises the thin-layer chromatography identification of representative chemical components of swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid contained in the main medicine of a gallbladder and stomach-recovering capsule prescription, and is carried out according to the following steps:
(1) preparation of a test solution:
adding methanol 45mL into 3g of the content of the gallbladder and stomach-recovering capsule, performing ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue with 3mL of methanol to obtain a sample solution;
(2) thin-layer chromatography identification of swertiamarin:
dissolving swertiamarin reference substance with methanol to obtain reference substance solution of 0.5 mg/mL; respectively sucking 3 μ L of each of the test solution and the reference solution, respectively dropping on the same thin layer chromatography plate, developing upwards with chloroform-methanol-water-formic acid solution as developing agent, taking out, and air drying; spraying sulfuric acid-ethanol solution on thin layer chromatography, air drying, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test sample shows blue-green fluorescence spots with the same color tone at the corresponding positions of the chromatogram of the swertiamarin reference substance;
(3) thin-layer chromatography identification of wogonin:
dissolving wogonin control with methanol to obtain 0.3mg/mL control solution; respectively sucking 3 μ L of test solution and control solution, respectively, spotting on the same thin layer chromatography plate, developing with n-butanol-ethyl acetate-water upper layer solution as developing agent, taking out, air drying, fumigating thin layer chromatography in iodine vapor cylinder for color development, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test solution shows dark brown fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference solution;
(4) identifying naringin and neohesperidin by thin-layer chromatography: respectively dissolving naringin and neohesperidin with methanol to obtain reference solutions of 0.3 mg/mL; respectively sucking 3 μ L of test solution, naringin and neohesperidin reference solution, respectively dropping on the same thin layer chromatography plate, spreading with chloroform-methanol-water lower layer solution as developing agent, taking out, and air drying; spraying 1% aluminum trichloride-ethanol solution by thin layer chromatography, air drying, and inspecting under ultraviolet lamp (365 nm); the chromatogram of the test sample shows bluish purple fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(5) carrying out thin-layer chromatography identification on alisol B and 23-acetyl alisol B: respectively dissolving alisol B and 23-acetyl alisol B reference substances with methanol to obtain 0.3mg/mL reference substance solutions; respectively sucking 3 μ L of test solution, alisol B and 23-acetyl alisol B reference solution, respectively, placing on the same thin layer chromatography plate, developing upwards with chloroform-methanol solution as developing agent, taking out, and air drying; spraying 2% vanillin-sulfuric acid-ethanol solution for color development, air drying, baking at 105 deg.C until color development is clear, and inspecting in sunlight; the chromatogram of the test sample shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(6) identifying pachymic acid by thin-layer chromatography: dissolving pachymic acid reference substance with methanol to obtain 0.5mg/mL reference substance solution; respectively sucking 3 μ L of test solution and control solution, respectively, placing on the same thin layer chromatography plate, developing with toluene-ethyl acetate-formic acid solution as developing agent, taking out, air drying, spraying sulfuric acid-ethanol solution to develop color, baking at 105 deg.C until spots are clear, and inspecting in sunlight; the chromatogram of the test solution shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the control solution.
The volume ratio of the developing agent trichloromethane-methanol-water-formic acid in the step (2) is 40: 10: 1: 1.
the volume ratio of the n-butyl alcohol-ethyl acetate-water as the developing agent in the step (3) is 4: 1: 1;
the volume ratio of the developing agent trichloromethane to the methanol to the water in the step (4) is 6: 3: 1.
the volume ratio of the developing solvent trichloromethane to the methanol in the step (5) is 20: 1.
the volume ratio of the developing solvent toluene-ethyl acetate-formic acid in the step (6) is 30: 10: 1.
the invention has the advantages that:
compared with the prior art, the invention has the advantages that:
(1) compared with the existing medicine standard of the gallbladder and stomach-recovering capsule, the thin-layer chromatography identification method of the gallbladder and stomach-recovering capsule establishes 7 thin-layer identification methods of representative chemical components of main medicinal materials of the prescription, namely swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid, and further perfects and improves the quality detection method of the national medicine of the gallbladder and stomach-recovering capsule.
(2) The sample pretreatment adopts ultrasonic treatment of samples to extract representative chemical components of the medicinal materials of each group, the dissolution of the detected components is sufficient, the experimental operation steps are simplified, the preparation time of the test solution is shortened, and the interference of other substances is eliminated.
(3) The screened developing agent system has good separation effect on corresponding detected components, clear thin-layer chromatography spots and clear result judgment, and can objectively and efficiently identify representative components in main formula medicinal materials of the national medicine 'Danweikang capsule'.
(4) The thin-layer chromatography identification detection indexes of 7 items such as swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, pachymic acid and the like are added, the existence condition of the chemical components in the 'gallbladder and stomach health capsule' can be more accurately detected, the capsule can be specially corresponding to corresponding prescription medicinal materials, and the better control of the medicine quality is facilitated.
Drawings
FIG. 1: identification of swertiamarin
In the chromatogram (identification of swertiamarin), spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is swertiamarin reference solution, and spot 5 is 'Danweikang capsule' preparation negative reference solution of swertia mileensis.
FIG. 2 is a drawing: identification of wogonin
In the chromatogram (identification of wogonin), spots 1, 2 and 3 are three batches of test solution of national medicine "Danweikang capsule", spot 4 is wogonin reference solution, and spot 5 is negative reference solution of "Danweikang capsule" preparation lacking Scutellaria baicalensis.
FIG. 3: identification of naringin
In the chromatogram (identification of naringin), spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is naringin reference solution, and spot 5 is 'Danweikang capsule' preparation negative reference solution lacking fructus Aurantii.
FIG. 4 is a drawing: identification of neohesperidin
In the chromatogram (identification of neohesperidin), spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is neohesperidin reference solution, and spot 5 is 'Danweikang capsule' preparation negative reference solution lacking fructus Aurantii.
FIG. 5: identification of alisol B
In the chromatogram (the identification of alisol B), spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is alisol B reference solution, and spot 5 is 'Danweikang capsule' preparation negative reference solution lacking alisma rhizome.
FIG. 6: identification of 23-acetyl alisol B
In the identification of the chromatogram, spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is 23-acetyl alisol B reference solution, and spot 5 is 'Danweikang capsule' preparation negative reference solution lacking alisma rhizome.
FIG. 7: identification of pachymic acid
In the chromatogram (identification of pachymic acid), spots 1, 2 and 3 are three batches of national medicine 'Danweikang capsule' test solution, spot 4 is pachymic acid reference solution, and spot 5 is Poria-absent 'Danweikang capsule' preparation negative reference solution.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The specific embodiments described herein are merely illustrative of the invention and do not delimit the scope of the invention.
A thin-layer chromatography identification method of a gallbladder and stomach-recovering capsule comprises the thin-layer chromatography identification of representative chemical components of swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid contained in the main medicine of a gallbladder and stomach-recovering capsule prescription, and is carried out according to the following steps:
(1) preparation of a test solution:
adding methanol 45mL into 3g of the content of the gallbladder and stomach-recovering capsule, performing ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue with 3mL of methanol to obtain a sample solution;
(2) thin-layer chromatography identification of swertiamarin:
dissolving swertiamarin reference substance with methanol to obtain reference substance solution of 0.5 mg/mL; respectively sucking 3 μ L of each of the test solution and the reference solution, respectively dropping on the same thin layer chromatography plate, developing upwards with chloroform-methanol-water-formic acid solution as developing agent, taking out, and air drying; spraying sulfuric acid-ethanol solution on thin layer chromatography, air drying, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test sample shows blue-green fluorescence spots with the same color tone at the corresponding positions of the chromatogram of the swertiamarin reference substance;
(3) thin-layer chromatography identification of wogonin:
dissolving wogonin control with methanol to obtain 0.3mg/mL control solution; respectively sucking 3 μ L of test solution and control solution, respectively, spotting on the same thin layer chromatography plate, developing with n-butanol-ethyl acetate-water upper layer solution as developing agent, taking out, air drying, fumigating thin layer chromatography in iodine vapor cylinder for color development, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test solution shows dark brown fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference solution;
(4) identifying naringin and neohesperidin by thin-layer chromatography: respectively dissolving naringin and neohesperidin with methanol to obtain reference solutions of 0.3 mg/mL; respectively sucking 3 μ L of test solution, naringin and neohesperidin reference solution, respectively dropping on the same thin layer chromatography plate, spreading with chloroform-methanol-water lower layer solution as developing agent, taking out, and air drying; spraying 1% aluminum trichloride-ethanol solution by thin layer chromatography, air drying, and inspecting under ultraviolet lamp (365 nm); the chromatogram of the test sample shows bluish purple fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(5) carrying out thin-layer chromatography identification on alisol B and 23-acetyl alisol B: respectively dissolving alisol B and 23-acetyl alisol B reference substances with methanol to obtain 0.3mg/mL reference substance solutions; respectively sucking 3 μ L of test solution, alisol B and 23-acetyl alisol B reference solution, respectively, placing on the same thin layer chromatography plate, developing upwards with chloroform-methanol solution as developing agent, taking out, and air drying; spraying 2% vanillin-sulfuric acid-ethanol solution for color development, air drying, baking at 105 deg.C until color development is clear, and inspecting in sunlight; the chromatogram of the test sample shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(6) identifying pachymic acid by thin-layer chromatography: dissolving pachymic acid reference substance with methanol to obtain 0.5mg/mL reference substance solution; respectively sucking 3 μ L of test solution and control solution, respectively, placing on the same thin layer chromatography plate, developing with toluene-ethyl acetate-formic acid solution as developing agent, taking out, air drying, spraying sulfuric acid-ethanol solution to develop color, baking at 105 deg.C until spots are clear, and inspecting in sunlight; the chromatogram of the test solution shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the control solution.
The volume ratio of the developing agent trichloromethane-methanol-water-formic acid in the step (2) is 40: 10: 1: 1.
the volume ratio of the n-butyl alcohol-ethyl acetate-water as the developing agent in the step (3) is 4: 1: 1;
the volume ratio of the developing agent trichloromethane to the methanol to the water in the step (4) is 6: 3: 1.
the volume ratio of the developing solvent trichloromethane to the methanol in the step (5) is 20: 1.
the volume ratio of the developing solvent toluene-ethyl acetate-formic acid in the step (6) is 30: 10: 1.
the invention overcomes the technical defect that the existing medicine standard of the national medicine 'Danweikang capsule' has few quality control points for identifying the medicinal materials of the prescription, and provides a thin-layer chromatography identification method of the 'Danweikang capsule', which aims to increase more comprehensive qualitative analysis indexes to identify more medicinal materials of the prescription and improve the quality standard of the 'Danweikang capsule' medicine.
The technical route is a special identification method for researching formula medicinal materials by taking representative components contained in formula medicinal materials of the 'Danweikang capsule' as reference substances, and the identifiable quantity of the formula medicinal materials is increased. The provided method adds 7 thin-layer chromatography qualitative identification items with swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid as reference substances, and respectively points to the existence detection of the main medicinal materials of swertia mileensis, Scutellaria baicalensis, fructus Aurantii, alisma orientale and Poria in the preparation of the 'Danweikang capsule'.
The provided thin-layer chromatography identification method can effectively eliminate interference of other substances in the aspect of sample pretreatment, and has the advantages of good thin-layer chromatography separation degree, simple and convenient operation and good reproducibility. Compared with the existing medicine standard of the 'Danweikang capsule', the qualitative identification indexes of 7 representative components are increased, the identification method is more comprehensive in comparison, strong in specificity, intuitive and clear in judgment, and objective and reliable in conclusion.
The purpose of the invention is realized by the following technical scheme
According to the existing medicine standard of 'Danweikang capsule' (2012) and the national medicine standard ZD-0334 (WS-10124 (ZD 0124) -2002-2012Z), the prescription and the preparation method of the medicine are as follows:
150g of swertia mileensis, 150g of Scutellaria baicalensis Georgi, 100g of fructus aurantii, 150g of Bupleurum falcatum, 150g of radix paeoniae alba, 100g of rhizoma alismatis, 100g of poria cocos, 100g of herba artemisiae capillaris, 50g of lophatherum gracile and 50g of rush. The 10 medicinal materials are prepared into decoction pieces, and the mile swertia herb is crushed into fine powder for standby; extracting volatile oil from fructus Aurantii and bupleuri radix, distilling to obtain water solution, soaking the residue and the rest 7 materials including Scutellariae radix in water for 12 hr, decocting for three times (2 hr each time), filtering, mixing filtrates, mixing the filtrate with the above water solution, and concentrating to obtain extract with relative density of 1.20 (50 deg.C); mixing the extract with the above fine powder, granulating, drying, spraying above volatile oil, and making into capsule (1000 granules).
The product is in the form of capsule, and the content is brown granule, light smell, bitter and astringent taste. Yi medicine with main functions is described as follows: chromelanchou, hi and Khatani, Dacroneau, le. The traditional Chinese medicine is described as follows: soothing liver, promoting bile flow, clearing heat and promoting diuresis. Can be used for treating costalgia, jaundice, bile reflux gastritis, and cholecystitis due to damp-heat in liver and gallbladder.
The 'Danweikang capsules' related to the technical research and development of the invention are all marketed medicines produced by drug industry Limited liability company of Paoyuan Tang in Yunnan; the reference substances including swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid are all purchased from Kjeldahl biotechnologies (purity is more than or equal to 98%).
The thin layer chromatography plate is a silica gel G common thin layer chromatography plate produced by Qingdao ocean chemical group, Nicoti Xin De Kezhi company and Merck company (Shanghai); the solvents (reagents) used for screening of the developing agent system are all ordinary chemically pure or analytically pure solvents (reagents).
The invention provides a thin-layer chromatography identification method of a 'Danweikang capsule', which comprises a series of thin-layer chromatography identifications by using swertiamarin (directing to formula medicinal material swertia mileensis), wogonin (directing to formula medicinal material southwestern baikal skullcap root), naringin, neohesperidin (directing to formula medicinal material bitter orange), 23-acetyl alisol B, alisol B (directing to formula medicinal material alisma rhizome) and pachymic acid (directing to formula medicinal material poria) as reference substances.
1. Thin-layer chromatography identification of swertiamarin
Swertiamarin is a representative component of monarch drug 'swertiamarin' of national drug 'Danweikang capsule' formula, and the swertiamarin is identified to have relatively exclusive characterization of swertiamarin in and judge the feeding condition of swertiamarin drug in the production process of the 'Danweikang capsule'.
Taking the content of the gallbladder and stomach-recovering capsule, adding methanol, performing ultrasonic treatment, filtering, evaporating the filtrate, and dissolving the residue with methanol to obtain a sample solution; dissolving swertiamarin in methanol as reference solution. And preparing a negative control sample without the swertia mileensis by taking the medicinal materials of the prescription of the 'Danweikang capsule' except the swertia mileensis according to the preparation method, and preparing a negative control solution of the swertia mileensis according to the method.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, taking chloroform-methanol-water-formic acid (40: 10: 1: 1) solution as developing agent, developing upwards, taking out, and air drying. Spraying 10% sulfuric acid-ethanol solution for color development, air drying, and inspecting under ultraviolet lamp (254 nm).
In the chromatogram of the test sample of the DANWEIKANG Capsule, fluorescent spots with the same color should be displayed at the corresponding positions of the chromatogram of the reference sample; in the chromatogram of the negative control solution of the elephantopus scaber, no corresponding fluorescent spot exists at the position corresponding to the chromatogram of the control product.
2. Thin-layer chromatography identification of wogonin
The wogonin is a representative component of the southwestern scutellaria baicalensis of the prescription medicinal material of the gallbladder and stomach health capsule, and the identification of the wogonin in the gallbladder and stomach health capsule has the indication and the directive significance for judging the feeding condition of the southwestern scutellaria baicalensis medicinal material in the production process of the gallbladder and stomach health capsule.
Taking the content of the gallbladder and stomach-recovering capsule, adding methanol, performing ultrasonic treatment, filtering, evaporating the filtrate, and dissolving the residue with methanol to obtain a sample solution; dissolving wogonin control in methanol to obtain control solution. And preparing negative control samples without the Scutellaria baicalensis in southwestern according to the preparation method, and preparing negative control solution without the Scutellaria baicalensis in southwestern according to the method.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, taking the upper layer solution of n-butanol-ethyl acetate-water (4: 1: 1) as a developing agent, performing upward development, taking out, and air drying. The thin layer chromatography was fumigated in iodine vapor tank for color development, and inspected under ultraviolet lamp (254 nm).
In the chromatogram of the test sample of the 'Danweikang capsule', fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the reference sample; in the chromatogram of the negative control solution of the scutellaria baicalensis in the south of the west, no corresponding fluorescent spot exists on the position corresponding to the chromatogram of the control product.
3. Thin-layer chromatography identification of naringin and neohesperidin
Naringin and neohesperidin are main representative components of fructus aurantii as a medicinal material of a 'Danweikang capsule', and the identification of naringin and neohesperidin in the 'Danweikang capsule' can be used for relatively exclusive characterization and judgment of the feeding condition of the fructus aurantii in the production process of the 'Danweikang capsule'.
Taking the content of the gallbladder and stomach-recovering capsule, adding methanol, performing ultrasonic treatment, filtering, evaporating the filtrate, and dissolving the residue with methanol to obtain a sample solution; naringin and neohesperidin as reference solutions were dissolved in methanol, respectively. And preparing a negative control sample without the fructus aurantii according to the preparation method, and preparing a negative control solution without the fructus aurantii according to the preparation method.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, taking the lower layer solution of chloroform-methanol-water (6: 3: 1) as developing agent, developing upwards, taking out, and air drying. Spraying 1% aluminum trichloride-ethanol solution, air drying, and inspecting under ultraviolet lamp (365 nm).
In the chromatogram of the test sample of the DANWEIKANG Capsule, fluorescent spots with the same color should be displayed at the corresponding positions of the chromatogram of the reference sample; in the chromatogram of the negative control solution without fructus aurantii, no corresponding fluorescent spot exists at the position corresponding to the chromatogram of the control substance.
4. Thin-layer chromatography identification of 23-acetyl alisol B and alisol B
The 23-acetyl alisol B and alisol B are representative chemical components of alisma rhizome which is a prescription medicinal material of the 'gallbladder and stomach-recovering capsule', and the 23-acetyl alisol B and alisol B which are present in the 'gallbladder and stomach-recovering capsule' can be identified to be specially characterized and judge the feeding condition of the alisma rhizome in the production process of the 'gallbladder and stomach-recovering capsule'.
Taking the content of the gallbladder and stomach-recovering capsule, adding methanol, performing ultrasonic treatment, filtering, evaporating the filtrate, and dissolving the residue with methanol to obtain a sample solution; respectively dissolving 23-acetyl alisol B and alisol B as reference substances with methanol to obtain reference substance solutions. And preparing a negative control sample without the rhizoma alismatis according to the preparation method and preparing a negative control solution without the rhizoma alismatis according to the method, wherein the medicinal materials except the rhizoma alismatis in the formula of the 'gallbladder-stomach-recovering capsule' are taken.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, developing with chloroform-methanol (20: 1) solution as developing agent, taking out, and air drying. Spraying 2% vanillin-sulfuric acid-ethanol solution for color development, air drying, baking at 105 deg.C until the color development is clear, and inspecting in sunlight.
Spots of the same color should appear on the chromatogram of the test solution of the DANWEIKANG Capsule at the positions corresponding to the chromatogram of the reference solution; in the chromatogram of the negative control solution without the Alisma orientale, no corresponding spot exists on the position corresponding to the chromatogram of the control product.
5. Thin layer chromatography identification of pachymic acid
The pachymic acid is a representative component of a formula medicinal material of the 'Danweikang capsule' and is used for identifying the specific characterization of the pachymic acid in the 'Danweikang capsule' and judging the feeding condition of the tuckahoe medicinal material in the production process of the 'Danweikang capsule'.
Taking the content of the gallbladder and stomach-recovering capsule, adding methanol, performing ultrasonic treatment, filtering, evaporating the filtrate, and dissolving the residue with methanol to obtain a sample solution; taking pachymic acid reference substance, dissolving with methanol to obtain reference substance solution. And preparing a negative control sample without the tuckahoe according to the preparation method, and preparing a negative control solution without the tuckahoe according to the method.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, developing with toluene-ethyl acetate-formic acid (30: 10: 1) solution as developing agent, taking out, air drying, developing with 10% sulfuric acid-ethanol solution by thin-layer chromatography, air drying, baking at 105 deg.C until the spots are clear, and inspecting in sunlight.
Spots of the same color should appear on the chromatogram of the test solution of the DANWEIKANG Capsule at the positions corresponding to the chromatogram of the reference solution; in the chromatogram of the negative control solution without Poria, there was no spot corresponding to the position of the chromatogram of the control.
Secondly, the invention carries out the following research on the provided thin-layer chromatography identification method
1. Preparation of test solution and negative control solution
Extracting the capsule contents with water, methanol and acetone as solvent under reflux and ultrasonic treatment. The results show that: the extracts of water, methanol and acetone can be detected by thin-layer chromatography to have swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid, but the spot of the methanol extract is clearer and has less interference; reflux and sonication extraction were not significantly different. Thus, the thin-layer chromatography identification test solution is prepared by using the methanol as a solvent and adopting an ultrasonic treatment method. Negative control solutions lacking each drug were also prepared in parallel as described above.
2. Screening of thin layer chromatography developer systems
According to the conventional technical method for identifying the traditional Chinese medicine quality standard by thin-layer chromatography, the most common silica gel G thin-layer chromatography plate is selected as a chromatographic stationary phase for research.
(1) Thin-layer chromatography identification of swertiamarin: different proportions of trichloromethane-methanol and trichloromethane-acetone in a binary solvent system are investigated; the different proportions of trichloromethane-methanol-water, normal butanol-ethyl acetate-water in the ternary solvent system are different; and an improved method for adjusting pH by adding formic acid into the solvent system to carry out a system comparison test. The results show that the separation effect of upward development is best by using the chloroform-methanol-water-formic acid (40: 10: 1: 1) solution of the improved quaternary solvent system as the developing agent.
(2) Thin-layer chromatography identification of wogonin: different proportions of trichloromethane-methanol and trichloromethane-acetone in a binary solvent system are investigated; the different proportions of the ternary solvent system trichloromethane-methanol-water, normal butanol-ethyl acetate-water are compared and tested. Research results show that the separation effect of upward development is best by taking the upper solution of n-butyl alcohol-ethyl acetate-water (4: 1: 1) of a ternary solvent system as a developing agent.
(3) Identifying naringin and neohesperidin by thin-layer chromatography: different proportions of a binary solvent system trichloromethane-methanol, a ternary solvent system trichloromethane-methanol-water and n-butyl alcohol-ethyl acetate-water are investigated for carrying out a system comparison test. Research results show that the separation effect of upward development is best by taking the lower layer solution of trichloromethane-methanol-water (6: 3: 1) of a ternary solvent system as a developing agent.
(4) The thin-layer chromatography identification of alisol B and 23-acetyl alisol B comprises the following steps: different proportions of cyclohexane-acetone, cyclohexane-ethyl acetate, trichloromethane-methanol and trichloromethane-acetone in a binary solvent system are examined for comparative tests. Research results show that the separation effect of upward development is best when chloroform-methanol (20: 1) solution is used as a developing agent.
(5) Identifying pachymic acid by thin-layer chromatography: a binary solvent system of trichloromethane-methanol and trichloromethane-acetone is investigated; the ternary solvent system trichloromethane-methanol-water, n-butyl alcohol-ethyl acetate-water, toluene-ethyl acetate-formic acid and trichloromethane-ethyl acetate-methanol in different ratios are subjected to system comparison tests. The research result shows that the separation effect of the upward development is the best when the toluene-ethyl acetate-formic acid (30: 10: 1) solution is used as the developing agent.
3. Comparison of silica gel G TLC plates
According to the above-identified various thin-layer chromatography conditions, the separation effects of silica gel G thin-layer chromatography plates produced by Qingdao ocean chemical group desiccant factories, Futai Xin DET technology corporation and Merck corporation (Shanghai) were compared. The results show that the silica gel G thin-layer chromatography plates of all manufacturers have good separation effect under the thin-layer chromatography parts, and the silica gel G thin-layer chromatography plates of different manufacturers can be selected in practical application.
4. Influence of developed ambient temperature and humidity on thin layer chromatography
The influence of different development temperature and humidity conditions on the thin-layer chromatography identification of the swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid serving as reference substances is examined, and the thin-layer chromatography has a good separation effect under the conditions of the development temperature of 10-30 ℃ and the relative humidity of 35-80%. The result shows that the thin-layer chromatography identification method has no special requirements on specific development temperature and humidity, and can finish the thin-layer chromatography identification work under the conventional conditions of a common laboratory.
5. Effect of developer steam saturation time on thin layer chromatography
The influence of the developing solvent on the thin-layer chromatography identification of the swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid which are used as reference substances under different saturation time conditions is examined. The results show that the thin-layer chromatography is not obviously affected by the unsaturated and saturated developing agent for 10 minutes and 20 minutes, and the chromatographic development operation of thin-layer chromatography identification can be carried out without presaturation of the developing agent in practical working application.
6. The specificity of the thin layer chromatography identification method
Preparing test solution and reference solution by thin layer chromatography identification method using swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid as reference; and preparing a negative control solution without a certain medicinal material by the same method of the test solution.
According to the determined development method, respectively sucking corresponding test solution, reference solution and negative reference solution, spotting on silica gel G thin layer chromatography plate, developing with determined developer, and developing. Spots with the same color appear in the thin-layer chromatography of the test sample at the corresponding positions of the chromatogram of the reference sample; the negative control solution had no corresponding spots, and the other components were not interfered with. The result shows that the thin-layer chromatography identification method has specificity on the identified representative components.
Example 1: thin-layer chromatography identification of swertiamarin in Danweikang capsules
Taking 3g of the content of the 'Danweikang capsule', adding 45mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue in 3mL of methanol to obtain a test solution. Dissolving swertiamarin control with methanol to obtain control solution of 0.5 mg/mL.
And taking 9 medicinal materials of the 'gallbladder and stomach-recovering capsule' except the mile swertia herb, preparing a negative control sample without the mile swertia herb according to a preparation method specified by the 'gallbladder and stomach-recovering capsule' standard, and preparing a negative control solution without the mile swertia herb according to the method.
Respectively sucking 3 μ L of test solution, control solution and negative control solution, respectively dropping on the same silica gel G thin layer chromatography plate, developing with chloroform-methanol-water-formic acid (40: 10: 1: 1) solution as developing agent, taking out, and air drying. Spraying 10% sulfuric acid-ethanol solution for color development, air drying, and inspecting under ultraviolet lamp (254 nm).
In the chromatogram of the test sample of DANWEIKANG Capsule, blue-green fluorescence spots with the same color tone are displayed at the positions corresponding to the chromatogram of the swertiamarin reference sample. In the chromatogram of the negative control solution of the elephantopus scaber, no corresponding fluorescent spot exists at the position corresponding to the chromatogram of the control product.
According to the thin-layer chromatography result, whether the detected national medicine preparation 'Danweikang capsule' contains the main medicinal material 'Qingyedan' can be objectively and accurately judged.
Example 2: thin-layer chromatography identification of wogonin in' Danweikang capsule
Taking 3g of the content of the 'Danweikang capsule', adding 45mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue in 3mL of methanol to obtain a test solution. Dissolving wogonin control with methanol to obtain control solution of 0.3 mg/mL.
And taking 9 medicinal materials of the 'Danweikang capsule' except the southwest scutellaria baicalensis, preparing a negative control sample without the southwest scutellaria baicalensis according to a preparation method specified by the 'Danweikang capsule' standard, and preparing a negative control solution without the southwest scutellaria baicalensis according to the method.
Respectively sucking 3 μ L of test solution, control solution and negative control solution, respectively dropping on the same silica gel G thin layer chromatography plate, developing with upper layer solution of n-butanol-ethyl acetate-water (4: 1: 1) as developing agent, taking out, and air drying. The thin layer chromatography was fumigated in iodine vapor tank for color development, and inspected under ultraviolet lamp (254 nm).
In the chromatogram of a test sample of the Danweikang capsule, dark brown fluorescent spots with the same color are displayed at the corresponding positions of the chromatogram of a reference sample; in the chromatogram of the negative control solution of the scutellaria baicalensis in the south of the west, no corresponding fluorescent spot exists on the position corresponding to the chromatogram of the control product.
According to the thin-layer chromatography result, whether the detected national medicine preparation 'Danweikang capsule' contains the main medicinal material 'southwest Baikal skullcap root' or not can be objectively and accurately judged.
Example 3: thin-layer chromatography identification of naringin and neohesperidin in' Danweikang capsule
Taking 3g of the content of the 'Danweikang capsule', adding 45mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue in 3mL of methanol to obtain a test solution. Collecting naringin and neohesperidin as control, and adding methanol to obtain solutions containing 0.3mg per 1mL respectively as control solutions.
And taking 9 medicinal materials of the 'Danweikang capsule' except the fructus aurantii, preparing a negative control sample without the fructus aurantii according to a preparation method specified by the 'Danweikang capsule' standard, and preparing a negative control solution without the fructus aurantii according to the method.
Respectively sucking the test solution, naringin and neohesperidin control solution, and negative control solution, respectively dropping on the same silica gel G thin layer chromatography plate, taking the lower layer solution of chloroform-methanol-water (6: 3: 1) as developing agent, spreading in the upward direction, taking out, and air drying. Spraying 1% aluminum trichloride-ethanol solution, air drying, and inspecting under ultraviolet lamp (365 nm).
In the chromatogram of the test sample of the DANWEIKANG Capsule, blue-purple fluorescent spots with the same color are respectively displayed at the corresponding positions of the chromatogram of the reference sample; in the chromatogram of the negative control solution without fructus aurantii, no corresponding fluorescent spot exists at the position corresponding to the chromatogram of the control substance.
According to the results of the thin-layer chromatography, whether the detected national medicine preparation, namely the gallbladder and stomach health capsule, contains the main medicinal material, namely the bitter orange, can be objectively and accurately judged.
Example 4: thin-layer chromatography identification of 23-acetyl alisol B and alisol B in' Danweikang capsule
Taking 3g of the content of the 'Danweikang capsule', adding 45mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue in 3mL of methanol to obtain a test solution. Respectively taking 23-acetyl alisol B and alisol B as reference substances, and respectively adding methanol to prepare solutions containing 0.3mg per 1mL as reference substance solutions.
And taking 9 medicinal materials of the 'Danweikang capsule' except the rhizoma alismatis, preparing a negative control sample without the rhizoma alismatis according to a preparation method specified by the 'Danweikang capsule' standard, and preparing a negative control solution without the rhizoma alismatis according to the method.
Respectively sucking the test solution, 23-acetyl alisol B, alisol B reference solution, and negative reference solution, respectively dropping on the same silica gel G thin layer chromatography plate, developing with chloroform-methanol (20: 1) solution as developing agent, taking out, and air drying. Spraying 2% vanillin-sulfuric acid-ethanol solution for color development, air drying, baking at 105 deg.C until the color development is clear, and inspecting in sunlight.
In the chromatogram of the test sample of the DANWEIKANG Capsule, gray yellow spots with the same color are respectively displayed at the corresponding positions of the chromatogram of the reference sample; in the chromatogram of the negative control solution without the Alisma orientale, no corresponding spot exists on the position corresponding to the chromatogram of the control product.
According to the thin-layer chromatography result, whether the detected national medicine preparation 'Danweikang capsule' contains the main medicine material 'Alisma orientale' or not can be objectively and accurately judged.
Example 5: thin-layer chromatography identification of pachymic acid in' Danweikang capsule
Taking 3g of the content of the 'Danweikang capsule', adding 45mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue in 3mL of methanol to obtain a test solution. Taking pachymic acid control, adding methanol to obtain solution containing 0.5mg per 1mL as control solution.
And preparing a negative control sample without the poria cocos according to a preparation method specified by the standard of the gallbladder-stomach-recovering capsule and preparing a negative control solution without the poria cocos according to the method, wherein 9 medicinal materials of the gallbladder-stomach-recovering capsule except the poria cocos are taken.
Respectively sucking the test solution, the reference solution and the negative reference solution, respectively dropping on the same silica gel G thin-layer chromatography plate, developing with toluene-ethyl acetate-formic acid (30: 10: 1) solution as developing agent, taking out, air drying, developing with 10% sulfuric acid-ethanol solution by thin-layer chromatography, air drying, baking at 105 deg.C until the spots are clear, and inspecting in sunlight.
In the chromatogram of the test sample, the positions corresponding to those of the chromatogram of the reference sample show gray yellow spots with the same color; in the chromatogram of the negative control solution without Poria, there was no spot corresponding to the position of the chromatogram of the control.
Claims (6)
1. A thin-layer chromatography identification method of a gallbladder and stomach-recovering capsule is characterized by comprising the thin-layer chromatography identification of representative chemical components of swertiamarin, wogonin, naringin, neohesperidin, 23-acetyl alisol B, alisol B and pachymic acid contained in the main medicine of a gallbladder and stomach-recovering capsule prescription, and the thin-layer chromatography identification method is carried out according to the following steps:
(1) preparation of a test solution:
adding methanol 45mL into 3g of the content of the gallbladder and stomach-recovering capsule, performing ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and dissolving the residue with 3mL of methanol to obtain a sample solution;
(2) thin-layer chromatography identification of swertiamarin:
dissolving swertiamarin reference substance with methanol to obtain reference substance solution of 0.5 mg/mL; respectively sucking 3 μ L of each of the test solution and the reference solution, respectively dropping on the same thin layer chromatography plate, developing upwards with chloroform-methanol-water-formic acid solution as developing agent, taking out, and air drying; spraying sulfuric acid-ethanol solution on thin layer chromatography, air drying, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test sample shows blue-green fluorescence spots with the same color tone at the corresponding positions of the chromatogram of the swertiamarin reference substance;
(3) thin-layer chromatography identification of wogonin:
dissolving wogonin control with methanol to obtain 0.3mg/mL control solution; respectively sucking 3 μ L of test solution and control solution, respectively, spotting on the same thin layer chromatography plate, developing with n-butanol-ethyl acetate-water upper layer solution as developing agent, taking out, air drying, fumigating thin layer chromatography in iodine vapor cylinder for color development, and inspecting under ultraviolet lamp (254 nm); the chromatogram of the test solution shows dark brown fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference solution;
(4) identifying naringin and neohesperidin by thin-layer chromatography: respectively dissolving naringin and neohesperidin with methanol to obtain reference solutions of 0.3 mg/mL; respectively sucking 3 μ L of test solution, naringin and neohesperidin reference solution, respectively dropping on the same thin layer chromatography plate, spreading with chloroform-methanol-water lower layer solution as developing agent, taking out, and air drying; spraying 1% aluminum trichloride-ethanol solution by thin layer chromatography, air drying, and inspecting under ultraviolet lamp (365 nm); the chromatogram of the test sample shows bluish purple fluorescent spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(5) carrying out thin-layer chromatography identification on alisol B and 23-acetyl alisol B: respectively dissolving alisol B and 23-acetyl alisol B reference substances with methanol to obtain 0.3mg/mL reference substance solutions; respectively sucking 3 μ L of test solution, alisol B and 23-acetyl alisol B reference solution, respectively, placing on the same thin layer chromatography plate, developing upwards with chloroform-methanol solution as developing agent, taking out, and air drying; spraying 2% vanillin-sulfuric acid-ethanol solution for color development, air drying, baking at 105 deg.C until color development is clear, and inspecting in sunlight; the chromatogram of the test sample shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the reference sample;
(6) identifying pachymic acid by thin-layer chromatography: dissolving pachymic acid reference substance with methanol to obtain 0.5mg/mL reference substance solution; respectively sucking 3 μ L of test solution and control solution, respectively, placing on the same thin layer chromatography plate, developing with toluene-ethyl acetate-formic acid solution as developing agent, taking out, air drying, spraying sulfuric acid-ethanol solution to develop color, baking at 105 deg.C until spots are clear, and inspecting in sunlight; the chromatogram of the test solution shows gray yellow spots with the same color at the corresponding positions of the chromatogram of the control solution.
2. The thin layer chromatography identification method of claim 1, wherein the volume ratio of the developing solvent chloroform-methanol-water-formic acid in the step (2) is 40: 10: 1: 1.
3. the thin layer chromatography identification method according to claim 1, wherein the volume ratio of n-butanol-ethyl acetate-water as the developing solvent in step (3) is 4: 1: 1.
4. the thin layer chromatography identification method of claim 1, wherein the volume ratio of the developing solvent chloroform-methanol-water in step (4) is 6: 3: 1.
5. the thin layer chromatography identification method of claim 1, wherein the volume ratio of the developing solvent chloroform-methanol in step (5) is 20: 1.
6. the thin layer chromatography identification method of claim 1, wherein the volume ratio of the developing solvent toluene-ethyl acetate-formic acid in step (6) is 30: 10: 1.
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