Method for identifying gardenia and processed product thereof

Abstract

The invention discloses a method for identifying gardenia and processed products thereof. The method comprises the following steps: step 1, respectively weighing equivalent gardenia sample powder and gardenia processed product sample powder; 2, respectively soaking the powder with an ethanol solution, then carrying out ultrasonic extraction and filtration, taking the filtrate, and evaporating to dryness to obtain a gardenia sample crude extract and a gardenia processed product sample crude extract; step 3, respectively adding water into the crude extracts for dissolving, then sequentially extracting twice by using petroleum ether and ethyl acetate, combining the two extracting solutions, evaporating to dryness to obtain an extract, and dissolving the extract by using methanol to obtain a gardenia sample test solution and a gardenia processed product sample test solution; and 4, respectively dispensing the test solutions on the same silica gel thin-layer plate, developing by using a developing solvent, airing, spraying a color developing agent to develop color, inspecting the thin-layer chromatography under an ultraviolet lamp, and identifying the sample type according to the number, position and color of fluorescent spots on the thin-layer chromatography. The method can effectively identify gardenia and processed products thereof.

Description

Technical Field

[0002] The present invention relates to the technical field of analysis and detection, and more specifically, to a method for identifying Gardenia jasminoides and its processed products. Background Art

[0003] Gardenia, also known as mountain gardenia and yellow gardenia, is an evergreen shrub of the Rubiaceae family. The mature fruit of Gardenia is used as medicine. It is bitter and cold in nature, and it is used in the heart, liver, lung, and stomach meridians. Gardenia has the effects of protecting the liver, promoting gallbladder function, lowering blood pressure, calming, stopping bleeding, and reducing swelling. It is commonly used for fever, restlessness, insomnia, jaundice, thirst, red eyes, sore throat, vomiting blood, bloody diarrhea, hematuria, heat toxicity, epidemic diseases, sprains, swelling and pain (Natural Product Research, 2001 (5); 57-59). The 2005 edition of the Chinese Pharmacopoeia contains not only raw gardenia, but also processed fried gardenia, scorched gardenia, and carbonized gardenia. The role of processing is to change the medicinal properties, enhance the efficacy, reduce adverse reactions, and meet the medication needs of different diseases in the clinic. The method for designing a method for identifying gardenia and its processed products is of great significance. Summary of the invention

[0004] An object of the present invention is to provide a method for identifying Gardenia jasminoides and its processed products to at least solve the above-mentioned problems.

[0005] In order to achieve the purpose and other advantages of the present invention, a method for identifying Gardenia jasminoides and its processed products is provided, comprising the following steps: Step 1, weigh equal amounts of Gardenia sample powder and Gardenia processed product sample powder respectively; Step 2, soaking the above powders in ethanol solution respectively, then performing ultrasonic extraction, filtering, and evaporating the filtrate to dryness to obtain a crude extract of a gardenia sample and a crude extract of a processed gardenia sample; Step 3, respectively dissolving the above crude extracts in water, then extracting twice with petroleum ether and ethyl acetate in sequence, combining the two extracts and evaporating to dryness to obtain an extract, dissolving the extract with methanol to obtain a test solution of a gardenia sample and a test solution of a processed gardenia sample; Step 4: Spot the above test solutions on the same silica gel thin layer plate, develop it with a developing agent, dry it, spray it with a color developer, and inspect the thin layer chromatogram under ultraviolet light. Identify the type of sample based on the number, position and color of the fluorescent spots on the thin layer chromatogram.

[0006] The gardenia in the present invention refers to raw gardenia, and the processed gardenia product is prepared by processing the raw gardenia.

[0007] Preferably, in the identification method of Gardenia jasminoides and its processed products, in step 2, the concentration of the ethanol solution is 95wt% and the soaking time is 8 to 12h.

[0008] Preferably, in the identification method of Gardenia jasminoides and its processed products, in step 2, the ultrasonic power of the ultrasonic extraction is 200w, the ultrasonic frequency is 40KHz, and the extraction time is 60min.

[0009] Preferably, in the method for identifying Gardenia jasminoides and its processed products, in step 4, the developing agent is a chloroform-acetone mixed solution with a volume ratio of 200:3.

[0010] Preferably, in the identification method of Gardenia jasminoides and its processed products, in step 4, the silica gel thin layer plate is a silica gel GF254 thin layer plate, the color developer is a 10wt% sulfuric acid ethanol solution, and the ultraviolet light wavelength of the ultraviolet lamp is one of 365nm, 302nm, and 254nm.

[0011] Preferably, in the method for identifying Gardenia jasminoides and its processed products, the wavelength of ultraviolet light is 302 nm or 254 nm.

[0012] Preferably, the identification method of gardenia and its processed products, the processed gardenia products include stir-fried gardenia and burnt gardenia.

[0013] Preferably, the identification method of Gardenia jasminoides and its processed products, the preparation method of each sample powder is: Each sample was placed in a pre-prepared mixed solution of bitter melon juice, ginger juice and lemon juice, soaked at 50-70°C for 3-5 hours, fished out, dried in the sun, and ground into powder to obtain each sample.

[0014] Preferably, in the method for identifying gardenia and its processed products, the volume ratio of bitter melon juice, ginger juice and lemon juice in the pre-prepared mixed solution is 6:5:(30-35).

[0015] The present invention has at least the following beneficial effects: The present invention can obtain a thin layer chromatogram of the sample on a silica gel thin layer plate under ultraviolet light by soaking the sample powder in ethanol, ultrasonically extracting, extracting twice with petroleum ether and ethyl acetate, spotting, developing, and coloring. According to the color, quantity, and position of the fluorescent spots in the thin layer chromatogram, it can be judged whether the sample to be identified is a processed product of gardenia or gardenia. The sample is pretreated and then powder is prepared, and then the sample powder is soaked in ethanol, ultrasonically extracted, extracted twice with petroleum ether and ethyl acetate, spotted, developed, and colored, and a thin layer chromatogram of the sample on a silica gel thin layer plate is obtained under ultraviolet light, and the color, number, and position of the fluorescent spots in the thin layer chromatogram can be used to determine whether the sample to be identified is a fried gardenia, a burnt gardenia, a gardenia, or a gardenia; The method of the invention is easy to operate, and the fluorescent spots in the thin layer chromatogram are obviously separated. The method can effectively identify the fried gardenia, the burnt gardenia, and the gardenia, and is helpful to improve the accuracy of medical personnel in using medicines.

[0016] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is the thin layer chromatogram of comparative example 3 of the present invention; Figure 2 It is the thin layer chromatogram of comparative example 2 of the present invention; Figure 3 It is the thin layer chromatogram of comparative example 1 of the present invention; Figure 4 is the thin layer chromatogram of Example 3 of the present invention; Figure 5 is the thin layer chromatogram of Example 1 of the present invention; Figure 6 is the thin layer chromatogram of Example 4 of the present invention; In each figure, 1-3 are the test solutions of gardenia samples, 4-6 are the test solutions of stir-fried gardenia samples, and 7-9 are the test solutions of burnt gardenia samples. DETAILED DESCRIPTION

[0018] The present invention is further described in detail below in conjunction with embodiments and drawings so that those skilled in the art can implement the invention with reference to the description.

[0019] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0020] It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials can be obtained from commercial sources unless otherwise specified; in the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "set" should be understood in a broad sense, for example, they can be fixedly connected, set, or detachably connected, set, or connected and set in one piece. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood in specific circumstances. The orientation or position relationship indicated by the terms "lateral", "longitudinal", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc. is based on the orientation or position relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention.

[0021] Example 1 Step 1: Grind the gardenia, the fried gardenia and the charred gardenia to powder, and weigh 5g of the gardenia sample powder, 5g of the fried gardenia sample powder and 5g of the charred gardenia sample powder respectively; Step 2, soak the above powders in 95wt% ethanol solution overnight (8-12h, about 10h), then perform ultrasonic extraction for 60min, wherein the ultrasonic power is 200w and the ultrasonic frequency is 40KHz, filter, take the filtrate and evaporate to dryness to obtain the crude extract of gardenia sample, the crude extract of fried gardenia sample, and the crude extract of charred gardenia sample; Step 3, respectively add 20 mL of water to dissolve the above crude extracts, then extract twice with petroleum ether and ethyl acetate in sequence, each time adding 10 mL of petroleum ether or ethyl acetate, combine the two extracts and evaporate to dryness to obtain an extract, dissolve the extract with 5 mL of methanol to obtain a test solution of a gardenia sample, a test solution of a fried gardenia sample, and a test solution of a coked gardenia sample; Step 4: Take 3 μL of each of the above test solutions and spot them on the same silica gel GF254 thin layer plate. Use a chloroform-acetone mixed solution with a volume ratio of 200:3 as the developing agent, develop, take out, dry, spray with 10wt% sulfuric acid ethanol solution for color development, and examine the thin layer chromatography under ultraviolet light (302nm). The results are as follows: Figure 5 shown.

[0022] Depend on Figure 5 It can be seen that in the thin layer chromatograms of the stir-fried gardenia test solution and the burnt gardenia test solution, fluorescent spots B and C of the same color are displayed at the corresponding positions of the thin layer chromatogram of the gardenia test solution, and fluorescent spots A are added at other positions accordingly.

[0023] Example 2 Same as Example 1, except that the thin layer chromatography was examined under ultraviolet light (254 nm). Figure 5 same.

[0024] Example 3 Same as Example 1, except that the thin layer chromatography was examined under ultraviolet light (365 nm). Figure 4 shown.

[0025] Depend on Figure 4 It can be seen that in the thin layer chromatograms of the fried gardenia test solution and the burnt gardenia test solution, fluorescent spots B of the same color are displayed at the corresponding positions of the thin layer chromatograms of the gardenia test solution, and fluorescent spots A are added correspondingly at other positions.

[0026] Example 4 Step 1: Place gardenia, stir-fried gardenia, and charred gardenia in a pre-prepared mixture of bitter melon juice, ginger juice, and lemon juice in a volume ratio of 6:5:33, soak at 60°C for 4 hours, remove, dry in the sun, and grind to obtain each sample powder; weigh 5g of gardenia sample powder, 5g of stir-fried gardenia sample powder, and 5g of charred gardenia sample powder respectively; Step 2, soak the above powders in 95wt% ethanol solution overnight (8-12h, about 10h), then perform ultrasonic extraction for 60min, wherein the ultrasonic power is 200w and the ultrasonic frequency is 40KHz, filter, take the filtrate and evaporate to dryness to obtain the crude extract of gardenia sample, the crude extract of fried gardenia sample, and the crude extract of charred gardenia sample; Step 3, respectively add 20 mL of water to dissolve the above crude extracts, then extract twice with petroleum ether and ethyl acetate in sequence, each time adding 10 mL of petroleum ether or ethyl acetate, combine the two extracts and evaporate to dryness to obtain an extract, dissolve the extract with 5 mL of methanol to obtain a test solution of a gardenia sample, a test solution of a fried gardenia sample, and a test solution of a coked gardenia sample; Step 4: Take 3 μL of each of the above test solutions and spot them on the same silica gel GF254 thin layer plate. Use a chloroform-acetone mixed solution with a volume ratio of 200:3 as the developing agent, develop, take out, dry, spray with 10wt% sulfuric acid ethanol solution for color development, and examine the thin layer chromatography under ultraviolet light (302nm). The results are as follows: Figure 6 shown.

[0027] Depend on Figure 6 It can be seen that in the thin layer chromatograms of the stir-fried gardenia test solution and the burnt gardenia test solution, fluorescent spots B and C of the same color are displayed at the corresponding positions of the thin layer chromatogram of the gardenia test solution, and a fluorescent spot A is added at another position. The thin layer chromatogram of the burnt gardenia test solution has an additional fluorescent spot D at another position corresponding to that of the stir-fried gardenia test solution.

[0028] Example 5 Same as Example 4, except that: Step 1, place gardenia, stir-fried gardenia, and charred gardenia in a pre-prepared mixture of bitter melon juice, ginger juice, and lemon juice in a volume ratio of 6:5:30, soak at 50°C for 3h, remove, dry, and grind to obtain each sample powder; weigh 5g of gardenia sample powder, 5g of stir-fried gardenia sample powder, and 5g of charred gardenia sample powder, respectively.

[0029] Thin layer chromatography results showed Figure 6 same.

[0030] Example 6 Same as Example 4, except that: Step 1, place gardenia, stir-fried gardenia, and charred gardenia in a pre-prepared mixture of bitter melon juice, ginger juice, and lemon juice in a volume ratio of 6:5:35, soak at 70°C for 5 hours, remove, dry, and grind to obtain each sample powder; weigh 5g of gardenia sample powder, 5g of stir-fried gardenia sample powder, and 5g of charred gardenia sample powder, respectively.

[0031] Thin layer chromatography results showed Figure 6 same.

[0032] Example 7 Same as Example 4, except that the thin layer chromatogram was examined under ultraviolet light (254 nm). Figure 6 same.

[0033] Comparative Example 1 Same as Example 1, except that a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 5:1 was used as the developing solvent. The results of thin layer chromatography were as follows Figure 3 shown.

[0034] Comparative Example 2 Same as Example 2, except that a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 5:1 was used as the developing solvent. The results of thin layer chromatography were as follows Figure 2 shown.

[0035] Comparative Example 3 Same as Example 3, except that a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 5:1 was used as the developing solvent. The results of thin layer chromatography were as follows Figure 1 shown.

[0036] Depend on Figures 1 to 3 It can be seen that in the thin layer chromatography of the stir-fried gardenia test solution, the burnt gardenia test solution, and the gardenia test solution, the corresponding positions all show fluorescent spots A, B, and C of the same color. It can be seen that the methods of Comparative Examples 1 to 3 cannot identify the three samples of gardenia, stir-fried gardenia, and burnt gardenia based on the color, position, and number of fluorescent spots.

[0037] Comparative Example 4 Same as Example 4, except that the pre-mixed solution contained no bitter melon juice. Figure 5 same.

[0038] Comparative Example 5 Same as Example 4, except that the pre-mixed solution does not contain ginger juice. Figure 5 same.

[0039] Comparative Example 6 Same as Example 4, except that the pre-mixed solution does not contain citric acid. Figure 5 same.

[0040] Comparative Example 7 Same as Example 4, except that the pre-prepared mixed solution contained no bitter melon juice or ginger juice. Figure 5 same.

[0041] Comparative Example 8 Same as Example 4, except that the pre-prepared mixed solution contained no bitter melon juice or citric acid. Figure 5 same.

[0042] Comparative Example 9 Same as Example 4, except that the pre-mixed solution contains no ginger juice or citric acid. Figure 5 same.

[0043] In summary, from the results of thin layer chromatography of Examples 1 to 4, it can be seen that there are significant differences in the number, position and color of fluorescent spots on thin layer chromatography between processed Gardenia and Gardenia, and the methods of Examples 1 to 4 can be used to identify processed Gardenia and Gardenia, and from the results of thin layer chromatography of Example 4, it can be seen that there are significant differences in the number, position and color of fluorescent spots on thin layer chromatography between stir-fried Gardenia, charred Gardenia and Gardenia, and the method of Example 4 can be used to identify stir-fried Gardenia, charred Gardenia and Gardenia. That is, the methods of Examples 1 to 4 of the present application can effectively determine whether the sample to be identified is Gardenia or processed Gardenia, and the method of Example 4 can also effectively determine whether the sample to be identified is stir-fried Gardenia or charred Gardenia.

[0044] The number of equipment and processing scale described here are used to simplify the description of the present invention. The application, modification and variation of the identification method of Gardenia jasminoides and its processed products of the present invention are obvious to those skilled in the art.

[0045] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the embodiments shown and described herein.

Claims

1. A method for identifying Gardenia jasminoides and its processed products, characterized in that: The following steps are involved: Step 1, weigh equal amounts of Gardenia sample powder and Gardenia processed product sample powder respectively; Step 2, soaking the above powders in ethanol solution respectively, then performing ultrasonic extraction, filtering, and evaporating the filtrate to dryness to obtain a crude extract of a gardenia sample and a crude extract of a processed gardenia sample; Step 3, respectively dissolving the above crude extracts in water, then extracting twice with petroleum ether and ethyl acetate in sequence, combining the two extracts and evaporating to dryness to obtain an extract, dissolving the extract with methanol to obtain a test solution of a gardenia sample and a test solution of a processed gardenia sample; Step 4: Spot the above test solutions on the same silica gel thin layer plate, develop it with a developing agent, dry it, spray it with a color developer, and inspect the thin layer chromatogram under ultraviolet light. Identify the type of sample based on the number, position and color of the fluorescent spots on the thin layer chromatogram.

2. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 1, characterized in that: In step 2, the concentration of the ethanol solution is 95wt% and the soaking time is 8-12h.

3. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 1, characterized in that: In step 2, the ultrasonic power of the ultrasonic extraction is 200w, the ultrasonic frequency is 40KHz, and the extraction time is 60min.

4. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 1, characterized in that: In step 4, the developing agent is a chloroform-acetone mixed solution with a volume ratio of 200:

3.

5. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 1, characterized in that: In step 4, the silica gel thin layer plate is a silica gel GF254 thin layer plate, the developer is a 10wt% sulfuric acid ethanol solution, and the ultraviolet light wavelength of the ultraviolet lamp is one of 365nm, 302nm, and 254nm.

6. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 5, characterized in that: The wavelength of the ultraviolet light is 302nm or 254nm.

7. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 1, characterized in that: The processed gardenia products include stir-fried gardenia and burnt gardenia.

8. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 7, characterized in that: The preparation method of each sample powder is as follows: Place each sample in a pre-prepared mixed solution of bitter melon juice, ginger juice and lemon juice, soak at 50-70°C for 3-5 hours, fish out, dry in the sun, and grind to obtain powder of each sample.

9. The method for identifying Gardenia jasminoides and its processed products as claimed in claim 8, characterized in that: In the prefabricated mixed solution, the volume ratio of bitter melon juice, ginger juice and lemon juice is 6:5:(30-35).

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