Method for identifying gardenia and its processed products

Abstract

The application discloses a kind of gardenia and its processed product identification method, comprising: step one, respectively take equal amount of gardenia sample powder, gardenia processed product sample powder;Step two, the above-mentioned powder is respectively soaked with ethanol solution, then ultrasonic extraction is carried out, filtration, filter liquor is evaporated to dryness, obtain gardenia sample crude extract, gardenia processed product sample crude extract;Step three, the above-mentioned crude extract is respectively dissolved with water, then sequentially extracted with petroleum ether, ethyl acetate twice, and the two extraction liquids are combined and evaporated to dryness, obtain extract, the extract is dissolved with methanol, obtain gardenia sample test solution, gardenia processed product sample test solution;Step four, the above-mentioned test solution is respectively spotted on the same silica gel thin layer plate, with developing agent development, dry, with color developing agent color development, and under ultraviolet lamp, view thin layer chromatogram, according to the number, position, color of fluorescence spot on thin layer chromatogram, identify sample variety.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of analytical detection technology. More particularly, the present application relates to a method for identifying Gardenia and its processed products. BACKGROUND

[0002] Gardenia is also known as mountain Gardenia and yellow Gardenia. It is a evergreen shrub of Rubiaceae. The ripe fruits of Gardenia are used as medicine. It tastes bitter and is cold in nature, and is attributed to heart, liver, lung and stomach meridians. Gardenia has the effects of protecting liver, promoting bile secretion, lowering blood pressure, calming, stopping bleeding and reducing swelling, and is often used for treating symptoms such as feverish restlessness, insomnia, jaundice, diabetes, red eyes, sore throat, hematemesis, dysentery, hematuria, toxic diseases and sprain and swelling (Natural Products Research, 2001(5): 57-59). In addition to raw Gardenia, Gardenia that has been processed, such as fried Gardenia, charred Gardenia and carbonized Gardenia, are also recorded in Chinese Pharmacopoeia 2005 edition. The purpose of processing is to change the nature of the medicine, enhance the efficacy, reduce adverse reactions, and meet the needs of different clinical conditions. Therefore, it is of great significance to design a method for identifying Gardenia and its processed products. SUMMARY

[0003] An object of the present application is to provide a method for identifying Gardenia and its processed products, which at least solves the above problems.

[0004] In order to achieve the object and other advantages of the present application, a method for identifying Gardenia and its processed products is provided, which comprises the following steps:

[0005] Step one, respectively take equal amounts of Gardenia sample powder and Gardenia processed product sample powder;

[0006] Step two, respectively soak the powders with ethanol solution, then perform ultrasonic extraction, filter, and evaporate the filtrate to obtain Gardenia sample crude extract and Gardenia processed product sample crude extract;

[0007] Step three, respectively dissolve the crude extracts in water, then successively extract twice with petroleum ether and ethyl acetate, evaporate the combined extract to obtain extract, and dissolve the extract in methanol to obtain Gardenia sample test solution and Gardenia processed product sample test solution;

[0008] Step four, respectively point the test solutions on the same silica gel thin layer plate, develop with developing agent, dry, spray with color developing agent, develop color, and observe the thin layer chromatogram under ultraviolet light, and identify the sample types according to the number, position and color of fluorescent spots on the thin layer chromatogram.

[0009] In the present application, Gardenia refers to raw Gardenia, and Gardenia processed product is obtained by processing raw Gardenia.

[0010] Preferably, in step two of the method for identifying Gardenia and its processed products, the concentration of the ethanol solution is 95wt%, and the soaking time is 8-12h.

[0011] Preferably, in the step two of the identification method of Gardenia and its processed products, the ultrasonic power is 200w, the ultrasonic frequency is 40KHz, and the extraction time is 60min.

[0012] Preferably, in the step four of the identification method of Gardenia and its processed products, the developing agent is a chloroform-acetone mixed solution with a volume ratio of 200:3.

[0013] Preferably, in the step four of the identification method of Gardenia and its processed products, the silica gel thin layer plate is a silica gel GF254 thin layer plate, the color developing agent is a 10wt% sulfuric acid ethanol solution, and the ultraviolet light wavelength of the ultraviolet lamp is one of 365nm, 302nm and 254nm.

[0014] Preferably, in the identification method of Gardenia and its processed products, the ultraviolet light wavelength is 302nm or 254nm.

[0015] Preferably, in the identification method of Gardenia and its processed products, the Gardenia processed products include fried products Gardenia and roasted products Gardenia.

[0016] Preferably, in the identification method of Gardenia and its processed products, the preparation method of the sample powder is as follows:

[0017] Each sample is placed in a prepared mixed solution configured by bitter gourd juice, ginger juice and lemon juice, soaked at 50-70℃ for 3-5h, taken out, dried and ground into powder to obtain each sample powder.

[0018] Preferably, in the prepared mixed solution of the identification method of Gardenia and its processed products, the volume ratio of the bitter gourd juice, the ginger juice and the lemon juice is 6:5: (30-35).

[0019] The present application at least includes the following beneficial effects:

[0020] The present application can obtain the thin layer chromatogram of the sample on the silica gel thin layer plate under the ultraviolet lamp by the ethanol immersion, ultrasonic extraction, petroleum ether and ethyl acetate twice extraction, spotting, development and coloration of the sample powder, and can determine whether the sample to be identified is the Gardenia processed product or the Gardenia according to the color, quantity and position of the fluorescent spots in the thin layer chromatogram.

[0021] And by the pretreatment of the sample and the preparation of the powder, the thin layer chromatogram of the sample on the silica gel thin layer plate under the ultraviolet lamp can be obtained by the ethanol immersion, ultrasonic extraction, petroleum ether and ethyl acetate twice extraction, spotting, development and coloration of the sample powder, and the sample to be identified can be determined to be the fried products Gardenia, the roasted products Gardenia or the Gardenia according to the color, quantity and position of the fluorescent spots in the thin layer chromatogram.

[0022] The method of this invention is easy to operate, and the fluorescent spots in the thin-layer chromatogram are clearly separated. It can effectively identify the roasted gardenia, the charred gardenia, and the gardenia, which helps to improve the accuracy of medication use by medical personnel.

[0023] Other advantages, objectives and features of the present invention will become apparent in part from the following description, and in part from those skilled in the art through study and practice of the invention. Attached Figure Description

[0024] Figure 1 This is the thin-layer chromatogram of Comparative Example 3 of the present invention;

[0025] Figure 2 This is the thin-layer chromatogram of Comparative Example 2 of the present invention;

[0026] Figure 3 This is the thin-layer chromatogram of Comparative Example 1 of the present invention;

[0027] Figure 4 This is a thin-layer chromatogram of Example 3 of the present invention;

[0028] Figure 5 This is a thin-layer chromatogram of Example 1 of the present invention;

[0029] Figure 6 This is a thin-layer chromatogram of Example 4 of the present invention;

[0030] In each figure, 1-3 are test solutions of gardenia samples, 4-6 are test solutions of roasted gardenia samples, and 7-9 are test solutions of charred gardenia samples. Detailed Implementation

[0031] The present invention will now be described in further detail with reference to the embodiments and accompanying drawings, so that those skilled in the art can implement it based on the description.

[0032] It should be understood that terms such as “having,” “comprising,” and “including” as used herein do not exclude the presence or addition of one or more other elements or combinations thereof.

[0033] It should be noted that the experimental methods in the following embodiments are conventional methods, and the reagents and materials are commercially available unless otherwise specified. In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connection", "arrangement" should be understood broadly, for example, they can be fixedly connected, arranged, or detachably connected, arranged, or integrally connected, arranged. Those skilled in the art can understand the specific meanings of the above terms in the present application according to the specific circumstances. The orientations or positional relationships indicated by the terms "transverse", "longitudinal", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like are based on the orientations or positional relationships shown in the drawings, and are merely intended to facilitate the description of the present application and simplify the description, and are not intended to indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0034] Example 1

[0035] Step one, grind Gardenia, fried Gardenia and charred Gardenia, and take 5g of Gardenia sample powder, 5g of fried Gardenia sample powder and 5g of charred Gardenia sample powder respectively;

[0036] Step two, soak the above powders in 95wt% ethanol solution overnight (8-12h, about 10h) respectively, then ultrasonic extract for 60min, wherein the ultrasonic power is 200w and the ultrasonic frequency is 40KHz, filter, take the filtrate to dry, to obtain Gardenia sample crude extract, fried Gardenia sample crude extract and charred Gardenia sample crude extract;

[0037] Step three, dissolve the above crude extracts in 20mL water respectively, then extract with petroleum ether and ethyl acetate in turn twice, the addition amount of petroleum ether or ethyl acetate is 10mL each time, combine the two extraction solutions to dry, to obtain the extract, dissolve the extract in 5ml of methanol to obtain Gardenia sample test solution, fried Gardenia sample test solution and charred Gardenia sample test solution;

[0038] Step four, take 3μL of the above test solutions respectively, and point them on the same silica gel GF254 thin layer plate, use the 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 observe the thin layer chromatogram under ultraviolet light (302nm), the results are shown in Table 1. Figure 5

[0039] Figure 5 ​​It can be seen that in the thin-layer chromatography of the gardenia test solution (roasted and charred), fluorescent spots B and C of the same color are displayed at the corresponding positions as in the thin-layer chromatography of the gardenia test solution, and fluorescent spot A is added at other positions.

[0040] Example 2

[0041] Same as Example 1, except that the thin-layer chromatography was examined under a UV lamp (254nm), and the results were the same. Figure 5 same.

[0042] Example 3

[0043] Same as Example 1, except that the thin-layer chromatography was examined under a UV lamp (365nm), and the results are as follows. Figure 4 As shown.

[0044] Depend on Figure 4 It can be seen that in the thin-layer chromatography of the gardenia test solution (both roasted and charred), fluorescent spots B of the same color are displayed at the corresponding positions as in the thin-layer chromatography of the gardenia test solution, and fluorescent spots A are also added at other positions.

[0045] Example 4

[0046] Step 1: Place gardenia, roasted gardenia, and charred gardenia separately 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℃ for 4 hours, remove, dry, and grind into powder to obtain powder for each sample. Weigh out 5g of gardenia powder, 5g of roasted gardenia powder, and 5g of charred gardenia powder respectively.

[0047] Step 2: Soak the above powders in 95wt% ethanol solution overnight (8-12h, about 10h), then perform ultrasonic extraction for 60min, with ultrasonic power of 200w and ultrasonic frequency of 40KHz, filter, take the filtrate and evaporate to dryness to obtain crude extracts of gardenia sample, crude extracts of roasted gardenia sample, and crude extracts of charred gardenia sample.

[0048] Step 3: Dissolve the above crude extracts in 20 mL of water, then extract them twice with petroleum ether and ethyl acetate, with 10 mL of petroleum ether or ethyl acetate added each time. Combine the two extracts and evaporate to dryness to obtain an extract. Dissolve the extract in 5 mL of methanol to obtain gardenia sample test solutions, roasted gardenia sample test solutions, and charred gardenia sample test solutions.

[0049] Step four, 3 μL of each of the above test solutions was taken and spotted on the same silica gel GF254 thin layer plate, a mixture of chloroform-acetone with a volume ratio of 200:3 was used as the developing agent, developed, taken out, air dried, sprayed with 10 wt% sulfuric acid ethanol solution for color development, and the thin layer chromatography was observed under ultraviolet light (302 nm), and the results are shown in Figure 6 .

[0050] As can be seen from Figure 6 , the thin layer chromatography of the fried gardenia fruit test solution and the roasted gardenia fruit test solution shows the same color fluorescent spots B and C at the corresponding positions of the thin layer chromatography of the gardenia fruit test solution, and each corresponds to an additional fluorescent spot A at another position. The thin layer chromatography of the roasted gardenia fruit test solution corresponds to the thin layer chromatography of the fried gardenia fruit test solution, and an additional fluorescent spot D is added at another position.

[0051] Example 5

[0052] The same as example 4, except that: step one, the gardenia, fried gardenia, and roasted gardenia were respectively placed in a pre-prepared mixture liquid prepared from bitter gourd juice, ginger juice, and lemon juice with a volume ratio of 6:5:30, soaked at 50°C for 3h, taken out, dried, and ground into powder to obtain sample powders; 5g of gardenia sample powder, 5g of fried gardenia sample powder, and 5g of roasted gardenia sample powder were weighed respectively.

[0053] The thin layer chromatography showed the same results as Figure 6 .

[0054] Example 6

[0055] The same as example 4, except that: step one, the gardenia, fried gardenia, and roasted gardenia were respectively placed in a pre-prepared mixture liquid prepared from bitter gourd juice, ginger juice, and lemon juice with a volume ratio of 6:5:35, soaked at 70°C for 5h, taken out, dried, and ground into powder to obtain sample powders; 5g of gardenia sample powder, 5g of fried gardenia sample powder, and 5g of roasted gardenia sample powder were weighed respectively.

[0056] The thin layer chromatography showed the same results as Figure 6 .

[0057] Example 7

[0058] The same as example 4, except that: the thin layer chromatography was observed under ultraviolet light (254 nm), and the results were the same as Figure 6 .

[0059] Comparative Example 1

[0060] The same as example 1, except that: a mixture of petroleum ether-ethyl acetate with a volume ratio of 5:1 was used as the developing agent. The thin layer chromatography showed the results as Figure 3As shown.

[0061] Comparative Example 2

[0062] Same as Example 2, except that a petroleum ether-ethyl acetate mixture with a volume ratio of 5:1 was used as the developing solvent. The thin-layer chromatography results are as follows: Figure 2 As shown.

[0063] Comparative Example 3

[0064] Same as Example 3, except that a petroleum ether-ethyl acetate mixture with a volume ratio of 5:1 was used as the developing solvent. The thin-layer chromatography results are as follows: Figure 1 As shown.

[0065] Depend on Figures 1-3 It can be seen that in the thin-layer chromatography of the test solutions of roasted gardenia, charred gardenia, and gardenia, fluorescent spots of the same color A, B, and C are all displayed at the corresponding positions. Therefore, the method of comparative examples 1-3 cannot distinguish between the three samples of gardenia—roasted gardenia and charred gardenia—based on the color, position, and number of fluorescent spots.

[0066] Comparative Example 4

[0067] Same as Example 4, except that the pre-prepared mixed solution did not contain bitter melon juice. Thin-layer chromatography results are the same as... Figure 5 same.

[0068] Comparative Example 5

[0069] Same as Example 4, except that the pre-mixed solution did not contain ginger juice. Thin-layer chromatography results are the same as... Figure 5 same.

[0070] Comparative Example 6

[0071] Same as Example 4, except that the pre-prepared mixed solution did not contain citric acid. Thin-layer chromatography results showed the same... Figure 5 same.

[0072] Comparative Example 7

[0073] Same as Example 4, except that the pre-prepared mixed solution contained no bitter melon juice or ginger juice. Thin-layer chromatography results were similar to... Figure 5 same.

[0074] Comparative Example 8

[0075] Same as Example 4, except that the pre-prepared mixed solution contained no bitter melon juice or citric acid. Thin-layer chromatography results were similar to... Figure 5 same.

[0076] Comparative Example 9

[0077] The same as example 4, except that no ginger juice and no citric acid were added to the pre-prepared mixed solution. The results of the thin layer chromatography showed the same results as Figure 5

[0078] In summary, the results of the thin layer chromatography of examples 1-4 show that there are significant differences in the number, position, and color of the fluorescent spots on the thin layer chromatography of processed gardenia fruit, gardenia fruit, and that the methods of examples 1-4 can be used to identify processed gardenia fruit and gardenia fruit, and that the results of the thin layer chromatography of example 4 show that there are significant differences in the number, position, and color of the fluorescent spots on the thin layer chromatography of fried gardenia fruit, charred gardenia fruit, and gardenia fruit, and that the method of example 4 can be used to identify fried gardenia fruit, charred gardenia fruit, and gardenia fruit. That is, the methods of examples 1-4 of the present application can be used to effectively determine whether the sample to be identified is gardenia fruit or a processed product of gardenia fruit, and the method of example 4 can also be used to effectively determine whether the sample to be identified is fried gardenia fruit or charred gardenia fruit.

[0079] The number of devices and the scale of the process described here are used to simplify the description of the present application. It is obvious to those skilled in the art that the application, modification, and variation of the method for identifying gardenia fruit and its processed products of the present application are obvious.

[0080] Although the embodiments of the present application have been disclosed as above, it is not limited to the application and the embodiments listed in the specification, and it can be fully applied to various fields suitable for the present application, and additional modifications can be easily realized by those skilled in the art, and therefore the present application is not limited to specific details and the examples shown and described here, without departing from the general concept defined by the claims and the equivalent scope.​

Claims

1. A method for identifying Gardenia and its processed products, characterized in that, The method comprises the following steps: Step one, respectively take equal amounts of gardenia sample powder, gardenia processed product sample powder; Step two, the above powders are respectively soaked with ethanol solution, then ultrasonic extraction, filtration, dry the filtrate, get gardenia sample crude extract, gardenia processed product sample crude extract; Step three, the above crude extract is respectively dissolved in water, then extracted with petroleum ether and ethyl acetate twice, dry the combined extract, get the extract, dissolve the extract with methanol, get gardenia sample test solution, gardenia processed product sample test solution; Step four, the above test solution is respectively spotted on the same silica gel thin layer plate, developed with developing agent, dried, sprayed with color developing agent, and observed under ultraviolet light, according to the number, position and color of fluorescent spots on the thin layer chromatogram, the sample type is identified; wherein, the developing agent is a chloroform-acetone mixed solution with a volume ratio of 200:3, and the color developing agent is a 10wt% sulfuric acid ethanol solution.

2. The method for identifying Gardenia and its processed products according to claim 1, characterized in that, In step two, the concentration of the ethanol solution is 95wt%, and the soaking time is 8~12h.

3. The method for identifying Gardenia and its processed products according to claim 1, wherein, In step two, the ultrasonic extraction power is 200w, the ultrasonic frequency is 40KHz, and the extraction time is 60min.

4. The method for identifying Gardenia and its processed products according to claim 1, wherein, In step four, the silica gel thin layer plate is silica gel GF254 thin layer plate, and the ultraviolet light wavelength of the ultraviolet lamp is one of 365nm, 302nm and 254nm.

5. The method for identifying Gardenia and its processed products according to claim 1, wherein, The gardenia processed product includes fried gardenia and charred gardenia.

6. The method for identifying Gardenia and its processed products according to claim 5, wherein, The preparation method of each sample powder is: Each sample is placed in a pre-prepared mixed solution prepared from bitter gourd juice, ginger juice and lemon juice, soaked at 50~70℃ for 3~5h, taken out, dried, and ground into powder to obtain each sample powder.

7. The method for identifying Gardenia and its processed products according to claim 6, wherein, In the pre-prepared mixed solution, the volume ratio of bitter gourd juice, ginger juice and lemon juice is 6:5: (30~35).

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