Method, device and equipment for controlling quality of oriental cherry
By combining thin-layer identification and high-performance liquid chromatography, the specific components and active ingredients in Guanshan cherry blossoms were qualitatively and quantitatively analyzed, which solved the gap in rapid and simple quality control in existing technologies and achieved comprehensive and accurate monitoring of the quality of Guanshan cherry blossoms.
Patent Information
- Application Number
- CN202511048040.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-29
- Publication Date
- 2025-09-16
AI Technical Summary
The existing technology lacks quality control methods for Guanshan cherry blossoms, especially a thin-layer identification method that is fast, simple, and does not require complex instruments. In addition, the traditional content determination method uses low-content isosakurabin and sakuratin as indicator components, making it difficult to effectively achieve quality monitoring.
The thin layer chromatography identification method was used to qualitatively analyze 1-O-caffeoyl-β-D-pyranoside in Guanshan cherry blossoms, and high performance liquid chromatography was used for quantitative analysis of isoquercetin. The component separation and detection were achieved through the principle of like dissolves like, the polarity difference of the developing solvent and the color reaction.
It achieves rapid and accurate quality control of Guanshan cherry blossoms, provides more comprehensive quality monitoring methods, solves the problem of low content of indicator components in traditional methods that are difficult to effectively monitor, and ensures the consistency of product quality and market competitiveness.
Smart Images
Figure CN120652038A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of quality control of traditional Chinese medicines, and in particular relates to a method, device and equipment for quality control of cherry blossoms in Guanshan. Background Art
[0002] Guanshan cherry blossoms, a species of flower in the genus Guanshan cherry (Prunus guanshanensis), belong to the Rosaceae subfamily. They are known for their beauty, anti-inflammatory, stress-relieving, and immune-boosting properties. They are used to slow skin aging, relieve inflammation, promote blood circulation, reduce anxiety, and boost the body's defenses against pathogens, demonstrating excellent results.
[0003] Currently, there are few quality control technologies for Guanshan cherry blossoms, and there is no thin-layer chromatography identification method that is rapid, simple, and does not require complex equipment. In addition, existing content determination methods use isoprunin and sakurantein as indicator components. Due to their low content and difficulty in detecting, the implementation of quality control for Guanshan cherry blossoms is somewhat limited. Summary of the Invention
[0004] The present application provides a method, device and equipment for quality control of Guanshan cherry blossoms to solve the problems that the quality control methods of Guanshan cherry blossoms in the existing technology are relatively lacking, especially the lack of thin-layer identification methods that are fast, simple and do not require complex instruments. At the same time, the traditional content determination method uses low-content isoprunin and sakuratin as indicator components, which makes it difficult to effectively achieve quality monitoring.
[0005] The first embodiment of the present application provides a quality control method for Guanshan cherry blossoms, comprising the following steps: performing qualitative analysis on a specific component in Guanshan cherry blossoms according to a thin layer identification method, wherein the specific component is 1-O-caffeoyl-β-D-pyranoglucoside; performing quantitative analysis on an active component in Guanshan cherry blossoms according to a content detection method, wherein the active component is isoquercetin; and combining the qualitative analysis and the quantitative analysis to obtain the quality characteristics of Guanshan cherry blossoms.
[0006] Preferably, the thin layer identification method includes: step 1: taking 0.1-5g of Guanshan cherry powder, adding 1-50mL of methanol, treating under ultrasonic conditions for 10-40 minutes, filtering and concentrating the filtrate to 0.5-2mL to obtain a test solution; step 2: preparing a reference solution containing 0.5mg / mL1-O-caffeoyl-β-D-pyranoglucoside; step 3: using thin layer chromatography, respectively taking 1-10μL of the test solution and the reference solution and spotting them on the same silica gel G thin layer plate, using a developing agent for development; taking out and drying, spraying 10% phosphomolybdic acid-ethanol solution, and heating at 120°C, and finally observing under 365nm ultraviolet light.
[0007] Preferably, the developing agent consists of dichloromethane, ether, methanol and formic acid, wherein the volume ratio of dichloromethane, ether, methanol and formic acid is (2-6):(1-5):(1-5):(0.01-0.10).
[0008] Preferably, the content detection method includes: Step 1: Accurately weigh 0.5-5.0 g of Sakura guanyam powder sieved through Pharmacopoeia No. 3 sieve, place in a conical flask, add 10-100 mL of 30-100% methanol aqueous solution, shake gently and soak for 10-50 minutes, then ultrasonically extract for 10-60 minutes, make up the weight and filter and collect the filtrate, pass through a 0.22 µm microporous membrane to obtain the test solution; Step 2: Prepare a reference solution containing an appropriate amount of isoquercetin so that its concentration reaches 0.1-2 mg of isoquercetin per ml; Step 3: Use octadecylsilane bonded silica gel as the filler and acetonitrile-0.01-1% formic acid water as the mobile phase. Use high performance liquid chromatography to draw 1-20µL of the reference solution and the test solution for analysis, and use the two-point method to calculate the content of isoquercetin.
[0009] Preferably, the high performance liquid chromatograph performs online degassing on the mobile phase before sample injection, and the gas content of the mobile phase after degassing is less than 0.1%.
[0010] Preferably, the detection wavelength of the high performance liquid chromatograph is 350-380 nm.
[0011] Preferably, the ultrasonic frequency range of the ultrasonic treatment is 20-60 kHz.
[0012] The second embodiment of the present application provides a Guanshan cherry quality control device, including: a sample processing module, used for the Guanshan cherry quality control method, weighing Guanshan cherry powder, adding a corresponding volume of methanol or methanol water solution, performing ultrasonic treatment, filtering, and concentration operations to prepare a test solution; a solution preparation module, used to accurately weigh 1-O-caffeoyl-β-D-pyranoside and isoquercetin, and adding methanol to prepare a reference solution; a detection and analysis module, including a thin layer chromatography device and a high performance liquid chromatograph; the thin layer chromatography device is used for thin layer identification The high performance liquid chromatograph is used for content detection method conditions, accurately injecting reference solution and test solution, collecting data and analyzing and calculating the isoquercetin content, and also has data processing and storage functions; the control and display module is used to control the operation of the entire device, set various parameters such as sample processing time, solution preparation concentration, detection instrument working parameters, etc., and display the device operation status, detection data and analysis results in real time.
[0013] Preferably, the control and display module also includes a human-computer interaction interface and an intelligent reminder module. When the sample processing time, solution preparation concentration or detection instrument working parameters exceed the preset range, it will promptly issue an audible and visual reminder, and use eye-catching signs on the interface to prompt the operator to make adjustments.
[0014] The third aspect of the present application provides an electronic device, including: a memory, a processor, and a computer program stored in the memory and executable on the processor. The processor executes the program to implement a Guanshan cherry blossom quality control method as described in the above embodiment.
[0015] Therefore, this application has the following beneficial effects: The present invention provides a quality control method for Prunus guanshanensis, which combines thin-layer chromatography (TLC) identification of the specific component 1-O-caffeoyl-β-D-pyranoglucoside with content detection of the active component isoquercetin. During the TLC identification, when preparing the sample solution, methanol, under the action of ultrasound, utilizes the principle of like dissolves like to destroy the cell structure of Prunus guanshanensis, prompting the dissolution of components such as 1-O-caffeoyl-β-D-pyranoglucoside in the methanol. During the TLC analysis stage, dichloromethane and ether in the developing solvent serve as low-polarity solvents, methanol provides a moderately polar environment, and a trace amount of formic acid is used to adjust the pH. The components are separated by the differences in adsorption-desorption capacity between the stationary phase (silica gel G) and the mobile phase (developing solvent). A 10% phosphomolybdic acid-ethanol solution is used as a color developer to undergo a redox color development reaction with 1-O-caffeoyl-β-D-pyranoglucoside, resulting in the appearance of specific color spots under 365nm ultraviolet light, thereby achieving qualitative detection of the component. During content testing, isoquercetin is fully dissolved and extracted in a methanol-water solution through immersion and ultrasound, utilizing intermolecular forces. During high-performance liquid chromatography analysis, octadecylsilane bonded silica gel is used as a filler. Based on the differences in hydrophobic and polar interactions between isoquercetin and the mobile phase (acetonitrile-formic acid water) and the stationary phase, quantitative determination of isoquercetin is achieved through the detection system of the high-performance liquid chromatography at a specific wavelength. This combination of qualitative and quantitative detection fills the gap in existing technologies for thin-layer identification methods that are fast, simple, and do not require complex instruments. It solves the problem that traditional content determination methods are difficult to effectively monitor due to the low content of indicator components, and provides a more comprehensive and accurate method for quality control of Guanshan cherry blossoms.
[0016] Additional aspects and advantages of the present application will be given in part in the description below, and in part will become apparent from the description below, or will be learned through practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The above and / or additional aspects and advantages of the present application will become apparent and easily understood from the following description of the embodiments in conjunction with the accompanying drawings, in which: Figure 1 This is a flow chart of the Guanshan cherry blossom quality control method provided according to an embodiment of the present application; Figure 2 This is a thin-layer chromatogram of 1-O-caffeoyl-β-D-glucopyranoside of Sakura guanshanensis provided in Example 1 of the present application, wherein 1-3 are test samples, 4 is a reference sample, and 5 is a negative control (blank solvent); Figure 3 This is a thin-layer chromatogram of 1-O-caffeoyl-β-D-glucopyranoside of Sakura guanshanensis provided in Example 2 of the present application, wherein 1-3 are test samples, 4 is a reference sample, and 5 is a negative control (blank solvent); Figure 4 This is a chromatogram of the reference substance of isoquercetin from Prunus guanshanensis provided in Example 3 of the present invention; Figure 5 This is a chromatogram of the sample of isoquercetin from Prunus guanshanensis provided in Example 3 of the present invention; Figure 6 This is a schematic diagram of the structure of the Guanshan cherry blossom quality control device provided according to an embodiment of the present application; Figure 7 A schematic diagram of the structure of an electronic device provided according to an embodiment of the present application. DETAILED DESCRIPTION
[0018] The following describes in detail embodiments of the present application. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present application, and should not be construed as limiting the present application.
[0019] The following describes a method, device and equipment for quality control of cherry blossoms in Guanshan County according to an embodiment of the present application with reference to the accompanying drawings. In response to the problem of the lack of quality control technology for cherry blossoms in Guanshan County mentioned in the above background technology, the present application provides a method for quality control of cherry blossoms in Guanshan County, in which the thin layer identification of the specific component 1-O-caffeoyl-β-D-pyranoglucoside is combined with the content detection of the effective component isoquercetin. In the thin layer identification, when the test solution is prepared, methanol, under the action of ultrasound, utilizes the principle of like dissolves like to destroy the cell structure of cherry blossoms in Guanshan County, and promotes the dissolution of components such as 1-O-caffeoyl-β-D-pyranoglucoside in methanol. In the thin layer chromatography analysis stage, dichloromethane and ether in the developing agent are used as low-polarity solvents, methanol provides a medium-polarity environment, and a trace amount of formic acid is used to adjust the pH. The separation of each component is achieved through the difference in adsorption-desorption capacity between the stationary phase (silica gel G) and the mobile phase (developing agent). A 10% phosphomolybdic acid-ethanol solution, used as a colorimetric developer, undergoes a redox colorimetric reaction with 1-O-caffeoyl-β-D-glucopyranoside, resulting in the formation of a specific color spot under 365nm ultraviolet light, enabling qualitative detection of the ingredient. For content determination, isoquercetin is thoroughly dissolved and extracted in a methanol-water solution through immersion and sonication, utilizing intermolecular forces. High-performance liquid chromatography (HPLC) analysis, using octadecylsilane bonded silica as a filler, enables quantitative determination of isoquercetin at a specific wavelength using the HPLC detection system, leveraging the hydrophobic and polar interactions between isoquercetin and the mobile phase (acetonitrile-formic acid water) and stationary phase. This combined qualitative and quantitative approach fills a gap in existing thin-layer identification techniques that are rapid, simple, and instrument-free. It addresses the challenges of traditional content determination methods, which often hinder effective monitoring of target components due to their low concentrations, and provides a more comprehensive and accurate method for quality control of Guanshan cherry blossoms.
[0020] Specifically, Figure 1 This is a flow chart of the Guanshan cherry blossom quality control method provided in an embodiment of the present application.
[0021] like Figure 1 As shown, the Guanshan cherry blossom quality control method includes the following steps: In step S101, a qualitative analysis of specific components in the Guanshan cherry blossoms is performed according to the thin layer chromatography identification method.
[0022] Among them, the specific component is 1-O-caffeoyl-β-D-glucopyranoside.
[0023] It can be understood that the embodiments of the present application can accurately separate the specific component from the complex component system of the Guanshan cherry blossoms based on the differences in the distribution coefficients of different components between the stationary phase and the mobile phase, and present characteristic spots on the thin layer plate, visually confirming its existence, and laying a solid foundation for subsequent quality evaluation; in terms of purity judgment, by observing whether the spot shape is regular, whether the size is uniform, whether the color depth is consistent, and other characteristics, the purity of 1-O-caffeoyl-β-D-pyranoglucoside can be preliminarily determined; in terms of process optimization, given that different process conditions in the Guanshan cherry blossom processing process have an impact on the content and purity of this component, the thin layer identification results can be fed back to the production link to help adjust process parameters such as extraction temperature, time, and solvent type to improve the extraction efficiency and purity of this component.
[0024] In the embodiment of the present application, the thin layer identification method includes: step 1: take 0.1-5g of Guanshan cherry powder, add 1-50mL of methanol, treat under ultrasonic conditions for 10-40 minutes, filter and concentrate the filtrate to 0.5-2mL to obtain a test solution; step 2: prepare a reference solution containing 0.5mg / mL1-O-caffeoyl-β-D-pyranoglucoside; step 3: using thin layer chromatography, respectively absorb 1-10μL of the test solution and the reference solution and spot them on the same silica gel G thin layer plate, use a developing agent for development; take out and dry, spray with 10% phosphomolybdic acid-ethanol solution, heat at 120°C, and finally observe under 365nm ultraviolet light.
[0025] The developing agent is composed of dichloromethane, ether, methanol and formic acid, wherein the volume ratio of dichloromethane, ether, methanol and formic acid is (2-6):(1-5):(1-5):(0.01-0.10).
[0026] It can be understood that the embodiments of the present application sequentially prepare a test solution by ultrasonic extraction and concentration of the Guanshan cherry powder with methanol, prepare a reference solution containing a specific concentration of 1-O-caffeoyl-β-D-pyranoglucoside, and then use dichloromethane, ether, methanol and formic acid in a specific volume ratio as developing agents. The test sample and reference solution are spotted and developed by thin layer chromatography, and the color is developed and then observed under 365nm ultraviolet light. This method can accurately separate and qualitatively identify the specific component, has high accuracy and good repeatability, and can effectively ensure the quality of Guanshan cherry related products.
[0027] In step S102, the effective components in the Guanshan cherry blossoms are quantitatively analyzed according to the content detection method.
[0028] Among them, the active ingredient is isoquercetin.
[0029] It can be understood that the embodiment of the present application uses a content detection method to carry out quantitative analysis on the active ingredient isoquercetin in Guanshan cherry, which can accurately determine the content of isoquercetin. By relying on specific analytical techniques such as high-performance liquid chromatography, the specific content value is separated and detected from the sample based on its physical and chemical properties and chromatographic behavior, providing scientific and objective quantitative indicators for the quality evaluation of Guanshan cherry; regular testing is carried out on samples from different batches, growth stages or storage conditions, and the fluctuation of isoquercetin content is grasped in real time, and unstable factors such as planting environment and processing technology are discovered in time, so as to make adjustments and improvements to ensure product quality consistency; through content detection, the relationship between isoquercetin content and production process is clarified, and the optimal extraction conditions and the influence of different processing methods on its content are determined, providing a basis for selecting a suitable process and improving product quality and economic benefits.
[0030] In the embodiment of the present application, the content detection method includes: step 1: accurately weigh 0.5-5.0g of Guanshan cherry powder screened by Pharmacopoeia No. 3 sieve, place it in a conical flask, add 10-100mL of 30-100% methanol aqueous solution, shake gently and soak for 10-50 minutes, then ultrasonically extract for 10-60 minutes, filter and collect the filtrate after making up the weight, and pass it through a 0.22µm microporous filter membrane to obtain a test solution; step 2: prepare a reference solution containing an appropriate amount of isoquercetin so that its concentration reaches 0.1-2mg of isoquercetin per milliliter; step 3: select octadecylsilane bonded silica gel as the filler, acetonitrile-0.01-1% formic acid water as the mobile phase, and use a high performance liquid chromatograph to draw 1-20µL of the reference solution and the test solution for analysis, and calculate the content of isoquercetin by the two-point method.
[0031] The detection wavelength of the high performance liquid chromatography is 350-380 nm, and the ultrasonic frequency range of the ultrasonic treatment is 20-60 kHz.
[0032] It can be understood that the embodiments of the present application are to precisely weigh the Kwanshan cherry powder, combine immersion with an appropriate concentration of methanol-water solution and ultrasonic extraction, and obtain a pure test solution through filtration and microporous filter membrane treatment; prepare a reference solution containing a known concentration of isoquercetin as a reference; use octadecylsilane bonded silica gel as a filler and acetonitrile-specific concentration of formic acid water as the mobile phase, and utilize high performance liquid chromatography to achieve efficient separation of isoquercetin from other components, and accurately calculate its content by the two-point method. This method provides a scientific and accurate means for the quality control of Kwanshan cherry, and can monitor the stability of the isoquercetin content.
[0033] It should be noted that the high performance liquid chromatograph will perform online degassing on the mobile phase before injection, and the gas content of the mobile phase after degassing is less than 0.1%.
[0034] In step S103, the qualitative analysis and the quantitative analysis are combined to obtain the quality characteristics of the Guanshan cherry blossoms.
[0035] Among them, quality characteristics refer to the comprehensive features of chemical composition, sensory properties, biological activity, etc., which reflect the quality and potential value of Guanshan cherry blossoms.
[0036] It is understandable that the embodiments of the present application combine qualitative analysis with quantitative analysis to evaluate the quality characteristics of Guanshan cherry blossoms. Qualitative analysis can accurately identify the types, characteristics, and interrelationships of the active ingredients in Guanshan cherry blossoms, providing a basic framework for understanding their quality essence; quantitative analysis can accurately determine the specific content of each ingredient, providing specific quantitative indicators for quality assessment. The two complement each other, achieving a comprehensive and multi-level analysis of the quality of Guanshan cherry blossoms, not only covering the composition of the ingredients, but also clarifying the content levels of the ingredients, and can accurately identify the quality differences between Guanshan cherry blossoms from different sources, batches, or growth environments, providing a scientific and reliable basis for quality differentiation. During the production, processing, and storage process, the combination of the two analytical methods can monitor quality changes in real time, promptly discover and resolve problems that affect quality consistency, and ensure stable product quality. At the same time, in terms of product research and development, in-depth quality characteristic analysis provides an important reference for product formula design, efficacy evaluation, etc., improves the scientific nature and success rate of product research and development, effectively avoids the limitations of a single analytical method, makes quality evaluation more comprehensive, objective, and accurate, improves the product's reputation and market recognition, and enhances market competitiveness.
[0037] According to the quality control method of Guanshan cherry proposed in the embodiment of the present application, the thin layer identification of the specific component 1-O-caffeoyl-β-D-pyranoglucoside is combined with the content detection of the effective component isoquercetin. In the thin layer identification, when the test solution is prepared, methanol is subjected to ultrasound and uses the principle of like dissolves like to destroy the cell structure of Guanshan cherry, prompting the dissolution of components such as 1-O-caffeoyl-β-D-pyranoglucoside in methanol. In the thin layer chromatography analysis stage, dichloromethane and ether in the developing agent are used as low-polarity solvents, methanol provides a medium-polarity environment, and a trace amount of formic acid is used to adjust the pH. The separation of each component is achieved through the difference in adsorption-desorption capacity between the stationary phase (silica gel G) and the mobile phase (developing agent). 10% phosphomolybdic acid-ethanol solution is used as a color developer to undergo a redox color reaction with 1-O-caffeoyl-β-D-pyranoglucoside, presenting specific color spots under 365nm ultraviolet light, thereby achieving qualitative detection of the component. During content testing, isoquercetin is fully dissolved and extracted in a methanol-water solution through immersion and ultrasound, utilizing intermolecular forces. During high-performance liquid chromatography analysis, octadecylsilane bonded silica gel is used as a filler. Based on the differences in hydrophobic and polar interactions between isoquercetin and the mobile phase (acetonitrile-formic acid water) and the stationary phase, quantitative determination of isoquercetin is achieved through the detection system of the high-performance liquid chromatography at a specific wavelength. This combination of qualitative and quantitative detection fills the gap in existing technologies for thin-layer identification methods that are fast, simple, and do not require complex instruments. It solves the problem that traditional content determination methods are difficult to effectively monitor due to the low content of indicator components, and provides a more comprehensive and accurate method for quality control of Guanshan cherry blossoms.
[0038] The following is an example of a method for quality control of Guanshan cherry blossoms. Using the abundant components 1-O-caffeoyl-β-D-glucopyranoside and isoquercetin as indicators, a thin layer qualitative identification and content detection method for Guanshan cherry blossoms were established. Among them, the quality inspection methods include the following thin layer identification and content detection methods: A. Thin-layer Chromatographic Identification of 1-O-caffeoyl-β-D-glucopyranoside Take 0.1-5 g of Sakura guanyin powder, add 1-50 mL of methanol, ultrasonically treat for 10-40 min, filter, and concentrate the filtrate to 0.5-2 mL as the test solution.
[0039] Separately, take 1-O-caffeoyl-β-D-glucopyranoside and add methanol to prepare a reference solution containing 0.5 mg per 1 mL.
[0040] According to the thin layer chromatography test, 1-10 μL of the test sample and reference sample solutions were respectively taken and spotted on the same silica gel G thin layer plate, and dichloromethane-ether-methanol-formic acid with a volume ratio of 2-6:1-5:1-5:0.01-0.10 was used as the developing solvent. The plate was developed, taken out, dried, sprayed with 10% phosphomolybdic acid-ethanol solution, heated at 120°C, and examined under 365nm ultraviolet light.
[0041] B. Isoquercetin Content Detection Method Accurately weigh 0.5-5.0 g of Sakura guanyam powder that has passed through No. 3 pharmacopoeia sieve, place it in a conical flask, add 10-100 mL of 30-100% methanol aqueous solution, weigh, shake gently, soak for 10-50 minutes, then ultrasonically extract for 10-60 minutes, make up the weight, filter, take the filtrate, and pass it through a 0.22 µm microporous filter membrane to obtain the test solution.
[0042] Take an appropriate amount of isoquercetin, accurately weigh it, and add methanol to prepare a reference solution containing 0.1-2 mg of isoquercetin per 1 ml.
[0043] Octadecylsilane bonded silica gel was used as the filler and acetonitrile-0.01-1% formic acid water was used as the mobile phase.
[0044] Accurately pipette 1-20 μl of the reference solution and 1-20 μl of the test solution, inject them into the high performance liquid chromatograph, and calculate the content using the two-point method.
[0045] Among them, the quality inspection methods include one or more of the following thin layer identification methods and content determination methods: A. Thin-layer Chromatographic Identification of 1-O-caffeoyl-β-D-glucopyranoside Take 1 g of Sakura guanyin powder, add 10 mL of methanol, ultrasonically treat for 30 min, filter, and concentrate the filtrate to 1 mL as the test solution.
[0046] Separately, take 1-O-caffeoyl-β-D-glucopyranoside and add methanol to prepare a reference solution containing 0.5 mg per 1 mL.
[0047] According to the thin layer chromatography test, 2 μL of the test sample and reference sample solutions were respectively taken and spotted on the same silica gel G thin layer plate, and dichloromethane-ether-methanol-formic acid with a volume ratio of 3:1:1:0.10 was used as the developing solvent. The plate was developed, taken out, dried, sprayed with 10% phosphomolybdic acid-ethanol solution, heated at 120°C, and examined under 365nm ultraviolet light.
[0048] B. Isoquercetin Content Detection Method Accurately weigh 1 g of Sakura guanshanensis powder that has passed through No. 3 pharmacopoeia sieve, place it in a conical flask, add 10 mL of 60% methanol aqueous solution, weigh, shake gently, soak for 30 minutes, then ultrasonically extract for 15 minutes, make up the weight, filter, take the filtrate, and pass it through a 0.22 µm microporous filter membrane to obtain the test solution.
[0049] Take an appropriate amount of isoquercetin, weigh it accurately, and add methanol to prepare a reference solution containing 0.5 mg of isoquercetin per 1 ml.
[0050] Octadecylsilane bonded silica gel was used as the filler and acetonitrile-0.01-1% formic acid water was used as the mobile phase.
[0051] Accurately pipette 10 μl of the reference solution and 10 μl of the test solution respectively, inject them into the high performance liquid chromatograph, and calculate the content using the two-point method.
[0052] The present invention will be further described below through typical examples.
[0053] Example 1 like Figure 2 As shown, thin layer chromatography identification of 1-O-caffeoyl-β-D-pyranoside Take 2 g of Sakura guanyin powder, add 15 mL of methanol, ultrasonically treat for 20 min, filter, and concentrate the filtrate to 1.5 mL as the test solution.
[0054] Separately, take 1-O-caffeoyl-β-D-glucopyranoside and add methanol to prepare a reference solution containing 0.5 mg per 1 mL.
[0055] According to the thin layer chromatography test, 1.5 μL of the test sample and reference sample solutions were respectively taken and spotted on the same silica gel G thin layer plate, and dichloromethane-ether-methanol-formic acid with a volume ratio of 3.5:1.5:1.5:0.10 was used as the developing solvent. The plate was developed, taken out, dried, sprayed with 10% phosphomolybdic acid-ethanol solution, heated at 120°C, and examined under 365 nm ultraviolet light.
[0056] Example 2 like Figure 3 As shown, thin layer chromatography identification of 1-O-caffeoyl-β-D-pyranoside Take 1.5 g of Sakura guanyin powder, add 20 mL of methanol, ultrasonically treat for 15 min, filter, and concentrate the filtrate to 1.0 mL as the test solution.
[0057] Separately, take 1-O-caffeoyl-β-D-glucopyranoside and add methanol to prepare a reference solution containing 0.5 mg per 1 mL.
[0058] According to the thin layer chromatography test, 1 μL of the test sample and reference sample solutions were respectively taken and spotted on the same silica gel G thin layer plate, and developed with dichloromethane-ethyl ether-methanol-formic acid in a volume ratio of 2:1:1:0.01. The plate was taken out, dried, sprayed with 10% phosphomolybdic acid-ethanol solution, heated at 120°C, and examined under 365nm ultraviolet light.
[0059] Example 3 Isoquercetin content detection method Accurately weigh 5 g of Sakura guanshanensis powder that has passed through No. 3 pharmacopoeia sieve, place it in a conical flask, add 40 mL of 50% methanol aqueous solution, weigh, shake gently, soak for 20 minutes, then ultrasonically extract for 20 minutes, make up the weight, filter, take the filtrate, and pass it through a 0.22 µm microporous filter membrane to obtain the test solution.
[0060] Take an appropriate amount of isoquercetin, weigh it accurately, and add methanol to prepare a reference solution containing 0.5 mg of isoquercetin per 1 ml.
[0061] Octadecylsilane bonded silica gel was used as the filler, and acetonitrile-0.1% formic acid water was used as the mobile phase.
[0062] like Figure 4 and Figure 5 As shown, 20 μl of the reference solution and 20 μl of the test solution were accurately aspirated and injected into the high performance liquid chromatograph, and the content was calculated using the two-point method.
[0063] In summary, the present invention uses thin-layer chromatography and high-performance liquid chromatography (HPLC) methods to qualitatively identify and quantitatively detect 1-O-caffeoyl-β-D-glucopyranoside and isoquercetin in Guanshan cherry blossoms, achieving effective quality control of this raw material. Experiments have demonstrated that this method is accurate, highly sensitive, and easily detectable, making it suitable for routine quality testing of Guanshan cherry blossoms.
[0064] Next, the Guanshan cherry blossom quality control device proposed according to the embodiment of the present application will be described with reference to the accompanying drawings.
[0065] Figure 6 It is a block diagram of the Guanshan cherry blossom quality control device according to an embodiment of the present application.
[0066] like Figure 6 As shown, the Guanshan cherry blossom quality control device 10 includes: a sample processing module 100, a solution preparation module 200, a detection and analysis module 300 and a control and display module 400.
[0067] Among them, the sample processing module 100 is used to weigh the Guanshan cherry powder, add the corresponding volume of methanol or methanol water solution, perform ultrasonic treatment, filtration, and concentration operations to prepare the test solution; the solution preparation module 200 is used to accurately weigh 1-O-caffeoyl-β-D-pyranoside and isoquercetin, and add methanol to prepare reference solutions respectively; the detection and analysis module 300 includes a thin layer chromatography device and a high performance liquid chromatograph; the thin layer chromatography device is used for thin layer identification method conditions, and performs spotting, development, color development and other operations on the test solution and the reference solution, and observes and records under 365nm ultraviolet light; the high performance liquid chromatograph is used for content detection method conditions, accurately injects the reference solution and the test solution, collects data and analyzes and calculates the isoquercetin content, and also has data processing and storage functions; the control and display module 400 is used to control the operation of the entire device, set various parameters such as sample processing time, solution preparation concentration, detection instrument working parameters, and display the device operation status, detection data and analysis results in real time.
[0068] In an embodiment of the present application, the control and display module 400 also includes a human-computer interaction interface and an intelligent reminder module. When the sample processing time, solution preparation concentration or detection instrument working parameters exceed the preset range, an audible and visual reminder is issued in time, and a conspicuous mark is used on the interface to prompt the operator to make adjustments.
[0069] It should be noted that the above explanation of the embodiment of the Guanshan cherry blossom quality control method is also applicable to the Guanshan cherry blossom quality control device of this embodiment, and will not be repeated here.
[0070] According to the Guanshan cherry blossom quality control device proposed in the embodiment of the present application, thin-layer identification of the specific component 1-O-caffeoyl-β-D-pyranoglucoside is combined with the content detection of the active ingredient isoquercetin. During the thin-layer identification, when preparing the sample solution, methanol, under the action of ultrasound, uses the principle of like dissolves like to destroy the Guanshan cherry blossom cell structure, prompting the dissolution of components such as 1-O-caffeoyl-β-D-pyranoglucoside in methanol. During the thin-layer chromatography analysis stage, dichloromethane and ether in the developing solvent serve as low-polarity solvents, methanol provides a medium-polarity environment, and a trace amount of formic acid adjusts the pH. The separation of the components is achieved by the difference in adsorption-desorption capacity between the stationary phase (silica gel G) and the mobile phase (developing solvent). 10% phosphomolybdic acid-ethanol solution is used as a color developer to undergo a redox color reaction with 1-O-caffeoyl-β-D-pyranoglucoside, presenting specific color spots under 365nm ultraviolet light, thereby achieving qualitative detection of the component. During content testing, isoquercetin is fully dissolved and extracted in a methanol-water solution through immersion and ultrasound, utilizing intermolecular forces. During high-performance liquid chromatography analysis, octadecylsilane bonded silica gel is used as a filler. Based on the differences in hydrophobic and polar interactions between isoquercetin and the mobile phase (acetonitrile-formic acid water) and the stationary phase, quantitative determination of isoquercetin is achieved through the detection system of the high-performance liquid chromatography at a specific wavelength. This combination of qualitative and quantitative detection fills the gap in existing technologies for thin-layer identification methods that are fast, simple, and do not require complex instruments. It solves the problem that traditional content determination methods are difficult to effectively monitor due to the low content of indicator components, and provides a more comprehensive and accurate method for quality control of Guanshan cherry blossoms.
[0071] Figure 7 This is a schematic diagram of the structure of an electronic device provided in an embodiment of the present application. The electronic device may include: Memory 701 , processor 702 , and computer programs stored in the memory 701 and executable on the processor 702 .
[0072] When the processor 702 executes the program, the Guanshan cherry blossom quality control method provided in the above embodiment is implemented.
[0073] Furthermore, the electronic device further includes: The communication interface 703 is used for communication between the memory 701 and the processor 702 .
[0074] The memory 701 is used to store computer programs that can be run on the processor 702 .
[0075] The memory 701 may include a high-speed RAM (Random Access Memory) memory, and may also include a non-volatile memory, such as at least one disk memory.
[0076] If the memory 701, processor 702, and communication interface 703 are implemented independently, the communication interface 703, memory 701, and processor 702 can be connected to each other via a bus and communicate with each other. The bus can be an ISA (Industry Standard Architecture) bus, a PCI (Peripheral Component Interconnect) bus, or an EISA (Extended Industry Standard Architecture) bus. Buses can be divided into address buses, data buses, control buses, etc. For ease of representation, Figure 7 Only one thick line is used in the diagram, but this does not mean that there is only one bus or one type of bus.
[0077] Optionally, in a specific implementation, if the memory 701, the processor 702 and the communication interface 703 are integrated on a chip, the memory 701, the processor 702 and the communication interface 703 can communicate with each other through an internal interface.
[0078] The processor 702 may be a CPU (Central Processing Unit), or an ASIC (Application Specific Integrated Circuit), or one or more integrated circuits configured to implement the embodiments of the present application.
[0079] In the description of this specification, reference to the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification, as well as features of different embodiments or examples, unless they are mutually inconsistent.
[0080] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features being referred to. Thus, a feature specified as "first" or "second" may explicitly or implicitly include at least one such feature. Throughout the description of this application, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.
[0081] Any process or method description in a flowchart or otherwise described herein may be understood to represent a module, segment or portion of code comprising one or more executable instructions for implementing the steps of a custom logical function or process, and the scope of the preferred embodiments of the present application includes alternative implementations in which functions may be performed out of the order shown or discussed, including performing functions in a substantially simultaneous manner or in the reverse order depending on the functions involved, which should be understood by those skilled in the art to which the embodiments of the present application belong.
[0082] Although the embodiments of the present application have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be understood as limitations on the present application. Ordinary technicians in this field can change, modify, replace and modify the above embodiments within the scope of the present application.
Claims
1. A method for controlling the quality of Guanshan cherry blossoms, characterized in that: The following steps are involved: The specific component in the Guanshan cherry blossoms was qualitatively analyzed according to the thin layer identification method, wherein the specific component was 1-O-caffeoyl-β-D-pyranoside; The active ingredient in the Guanshan cherry blossoms was quantitatively analyzed according to the content detection method, wherein the active ingredient was isoquercetin; The qualitative analysis and the quantitative analysis are combined to obtain the quality characteristics of the Guanshan cherry blossoms.
2. A Guanshan cherry blossom quality control method according to claim 1, characterized in that: The thin layer identification method comprises: Step 1: Take 0.1-5g of Sakura guanshanensis powder, add 1-50mL of methanol, treat under ultrasonic conditions for 10-40 minutes, filter and concentrate the filtrate to 0.5-2mL to obtain the test solution; Step 2: Prepare a reference solution containing 0.5 mg / mL 1-O-caffeoyl-β-D-pyranoside; Step 3: Use thin layer chromatography to aspirate 1-10 μL of the test solution and reference solution onto the same silica gel G thin layer plate, and develop it with a developing agent; take it out and dry it, spray it with 10% phosphomolybdic acid-ethanol solution, heat it at 120°C, and finally observe it under 365nm ultraviolet light.
3. A Guanshan cherry blossom quality control method according to claim 2, characterized in that: The developing agent consists of dichloromethane, ether, methanol and formic acid, wherein the volume ratio of the dichloromethane, ether, methanol and formic acid is (2-6):(1-5):(1-5):(0.01-0.10).
4. The method for controlling the quality of Guanshan cherry blossoms according to claim 1, wherein: The content detection method includes: Step 1: Accurately weigh 0.5-5.0 g of Sakura guanyam powder sieved through Pharmacopoeia No. 3 sieve, place in a conical flask, add 10-100 mL of 30-100% methanol aqueous solution, shake gently and soak for 10-50 minutes, then ultrasonically extract for 10-60 minutes, make up the weight and filter and collect the filtrate, pass through a 0.22 µm microporous membrane to obtain the test solution; Step 2: Prepare a reference solution containing an appropriate amount of isoquercetin so that its concentration reaches 0.1-2 mg of isoquercetin per ml; Step 3: Use octadecylsilane bonded silica gel as the filler and acetonitrile-0.01-1% formic acid water as the mobile phase. Use high performance liquid chromatography to draw 1-20µL of the reference solution and the test solution for analysis, and use the two-point method to calculate the content of isoquercetin.
5. A Guanshan cherry blossom quality control method according to claim 3 or 4, characterized in that: The high performance liquid chromatograph performs online degassing on the mobile phase before sample injection, and the gas content of the mobile phase after degassing is less than 0.1%.
6. The method for controlling the quality of Guanshan cherry blossoms according to claim 5, characterized in that: The detection wavelength of the high performance liquid chromatograph is 350-380 nm.
7. A Guanshan cherry blossom quality control method according to claim 2 or 4, characterized in that: The ultrasonic frequency range of the ultrasonic treatment is 20-60 kHz.
8. A quality control device for Guanshan cherry blossoms, characterized in that: include: A sample processing module, for weighing the Guanshan cherry powder according to any one of claims 1 to 7, adding a corresponding volume of methanol or methanol-water solution, performing ultrasonic treatment, filtering, and concentration operations to prepare a test solution; The solution preparation module is used to accurately weigh 1-O-caffeoyl-β-D-glucopyranoside and isoquercetin, and add methanol to prepare reference solutions; The detection and analysis module includes a thin-layer chromatography device and a high-performance liquid chromatography instrument; the thin-layer chromatography device is used for thin-layer identification method conditions, and performs operations such as spotting, developing, and coloring the test solution and the reference solution, and observes and records under 365nm ultraviolet light; the high-performance liquid chromatography is used for content detection method conditions, accurately injecting the reference solution and the test solution, collecting data and analyzing and calculating the isoquercetin content, and also has data processing and storage functions; The control and display module is used to control the operation of the entire device, set various parameters such as sample processing time, solution preparation concentration, detection instrument working parameters, etc., and display the device operation status, detection data and analysis results in real time.
9. The Guanshan cherry blossom quality control device according to claim 7, characterized in that: The control and display module also includes a human-computer interaction interface and an intelligent reminder module. When the sample processing time, solution preparation concentration or detection instrument working parameters exceed the preset range, it will promptly issue an audible and visual reminder, and use eye-catching signs on the interface to prompt the operator to make adjustments.
10. An electronic device, characterized in that: include: A memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the program to implement a method for controlling the quality of cherry blossoms in Guanshan as described in any one of claims 1 to 7.