Method for rapidly detecting content of cane sugar in dried ginseng medicinal material
By establishing a correction model for the sucrose content and sugar content in dry ginseng samples, using sugar meter and high performance liquid chromatography, the problems of high price, long detection time and high technical requirements for detecting sucrose content in dry ginseng medicinal materials in the prior art are solved, and a fast, accurate and low-cost detection effect is achieved.
Patent Information
- Application Number
- CN202510060180.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-15
- Publication Date
- 2025-05-13
AI Technical Summary
In the prior art, the method for detecting the sucrose content in dried ginseng medicinal materials has problems such as high equipment price, long testing time and high technical requirements, which is difficult to meet the use of suppliers who do not have corresponding equipment or technical personnel.
The sample solution obtained after pre-treatment of the dry ginseng sample was measured and the sugar content and the sugar content were established through linear fitting. The sugar content and sugar content were used to achieve rapid and accurate detection using a sugar meter and high-performance liquid chromatography.
It realizes rapid and accurate detection of the sucrose content in dried ginseng medicinal materials, reduces the equipment price and testing time, and simplifies the operation process, making this method suitable for participating enterprises that do not meet laboratory conditions or do not have relevant technical personnel.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of traditional Chinese medicine component detection and relates to a rapid detection method for sucrose content in dry ginseng medicinal materials. Background Art
[0002] Ginseng (Panax ginseng CAMey) is mainly used as medicine in its dried root and is a precious Chinese herbal medicine. Ginseng is rich in sugar components, which are synthesized by photosynthesis and are closely related to growth metabolism. Sucrose is an important material component of ginseng medicinal materials, accounting for a relatively high proportion. The sucrose content is affected by many factors such as harvest time and processing. It has a great influence on the appearance of ginseng medicinal materials and the material composition of ginseng extracts. Therefore, it is very important to be able to quickly detect the sucrose content in ginseng medicinal materials.
[0003] At present, common methods for detecting sucrose include high-performance liquid chromatography and colorimetric methods. High-performance liquid chromatography can detect sucrose content more accurately, but the equipment is expensive and the detection time is long. The colorimetric method experiment is more complicated, and both have high technical requirements, which is not conducive to suppliers who do not have the corresponding equipment or technical personnel. Therefore, it is necessary to improve the existing detection methods. Summary of the invention
[0004] In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a method for quickly detecting the sucrose content in dry ginseng medicinal materials, which can quickly and accurately detect the sucrose content in ginseng.
[0005] To achieve the above-mentioned purpose and other related purposes, the present invention provides a method for rapid detection of sucrose content in dry ginseng medicinal materials, comprising: determining the sugar content and sucrose content of a sample solution obtained after pretreatment of the dry ginseng sample, respectively, performing linear fitting on the sugar content and the sucrose content, establishing a correction model for the sucrose content and sugar content in the dry ginseng sample, and determining the sucrose content in the dry ginseng sample by fitting the correction model with the measured sugar content; the fitting curve in the correction model for the sucrose content and sugar content in the dry ginseng sample is calculated according to formula (1), and the formula (1) is: sucrose = 5.258 × sugar content - 23.35.
[0006] Preferably, the dried ginseng sample is five-year-old ginseng. The dried ginseng is a ginseng medicinal material that is processed by washing and drying fresh ginseng. It is different from fresh ginseng, which is a ginseng medicinal material that is directly dug from the ginseng field and used directly after washing.
[0007] Preferably, the dry ginseng sample is in powder form.
[0008] Preferably, the pretreatment comprises: adding a dry ginseng sample to a solvent for extraction, and filtering to obtain a sample solution.
[0009] Preferably, the solvent is water.
[0010] More preferably, the water is water with a sacchariness value of 0. Using water with a sacchariness value of 0 for extraction can completely extract sucrose without causing a change in sucrose content.
[0011] Preferably, the ratio of the added mass g of the dry ginseng sample to the added volume mL of the solvent is 1:4-10, specifically 1:4-5, 1:5-10, preferably 1:5.
[0012] Preferably, the extraction is selected from one of cold soaking extraction or ultrasonic extraction, preferably cold soaking extraction.
[0013] More preferably, the cold infusion extraction comprises cold infusion followed by juicing.
[0014] More preferably, the cold soaking time is 2-30 min, specifically 2-5 min, 5-10 min, 10-30 min, preferably 10 min.
[0015] Further preferably, the juicing is performed by squeezing out the ginseng juice using a garlic press, which is a conventional garlic press that can squeeze out ginseng juice.
[0016] More preferably, when the garlic press presses the ginseng juice, gauze is placed on the bottom.
[0017] Most preferably, the gauze is made of nylon.
[0018] Most preferably, the mesh size of the gauze is 90-110 meshes, preferably 100 meshes.
[0019] Most preferably, the gauze has 3-5 layers, preferably 4 layers.
[0020] More preferably, the ultrasonic extraction time is 55-65 min, specifically 55-60 min, 60-65 min, preferably 60 min.
[0021] Preferably, the filtration is membrane filtration.
[0022] More preferably, the filter membrane is a 0.45 μm filter membrane.
[0023] Preferably, the determination of the sugar content value comprises: measuring the sugar content of the sample solution using a saccharimeter to obtain the sugar content value of the sample solution.
[0024] Preferably, the measurement by the saccharimeter is a measurement process of a conventional saccharimeter.
[0025] More preferably, the saccharimeter needs to be calibrated before measurement. Specifically, click the power button of the saccharimeter to turn it on, drip clean water (to completely cover the bottom of the glass), press it shortly and then long press it until "calibrating" is displayed to enter the calibration state, and you can let go when the screen shows "calibrating". After the calibration is completed, the displayed sugar content value should be 0%.
[0026] More preferably, the amount of sample solution dripped into the saccharimeter during measurement is 2-3 drops.
[0027] Specifically, click the start button of the saccharimeter, drop the sample solution (completely cover the bottom of the glass), click to test, and record the sugar content. For the same sample, test twice and take the average value.
[0028] Preferably, the determination of sucrose content comprises the following steps:
[0029] 1) Add sucrose reference substance to solvent, dissolve it and make up to volume to obtain reference substance solution;
[0030] 2) Dilute the sample solution with water and filter it to obtain the test solution;
[0031] 3) using high performance liquid chromatography to measure the test solution of step 2) and the reference solution of step 1), respectively, and calculating the content of sucrose in the test solution by an external standard method.
[0032] Preferably, in step 1), the solvent is water.
[0033] More preferably, the water is water with a saccharimetric value of 0. Using water with a saccharimetric value of 0 for dissolution will not introduce changes in sucrose content.
[0034] Preferably, in step 1), the reference substance solution can be prepared directly as a reference substance solution, or can be prepared by first adding a solvent to prepare a reference substance stock solution and then adding a solvent to dilute it step by step.
[0035] Preferably, in step 1), the content of sucrose in the reference solution is in the range of 0.3-1.5 mg / mL.
[0036] Preferably, in step 2), the sample solution is diluted with water by 4-6 times, preferably 5 times.
[0037] More preferably, the water is water with a saccharimetric value of 0. Dilution with water with a saccharimetric value of 0 will not introduce changes in sucrose content.
[0038] Preferably, in step 2), the filtration is membrane filtration.
[0039] More preferably, the filter membrane is a 0.45 μm filter membrane.
[0040] Preferably, in step 3), the chromatographic column in the HPLC method is an ES chromatographic column. More preferably, the chromatographic column in the HPLC method is a Prevail Carbohydrate ES chromatographic column (4.6 mm×250 mm, 5 μm).
[0041] Preferably, in step 3), the detector in the high performance liquid chromatography is an evaporative light scattering detector (ELSD).
[0042] More preferably, the drift tube temperature of the evaporative light scattering detector (ELSD) is 40-50°C, such as 40-45°C, 45-50°C, preferably 45°C.
[0043] Preferably, in step 3), in the high performance liquid chromatography method, the column temperature is 25-35°C, such as 25-30°C, 30-35°C, preferably 30°C.
[0044] Preferably, in step 3), in the high performance liquid chromatography, the flow rate is 0.1-2 mL / min, such as 0.1-0.5 mL / min, 0.5-1 mL / min, 1-1.5 mL / min, 1-2 mL / min, preferably 1.0 mL / min.
[0045] Preferably, in step 3), in the high performance liquid chromatography, the mobile phase is acetonitrile-water, wherein phase A is acetonitrile and phase B is water.
[0046] Preferably, in step 3), the high performance liquid chromatography adopts isocratic elution and the analysis time is not less than 30 min, preferably 30 min.
[0047] More preferably, the specific procedure of the isocratic elution is: the analysis time is greater than 0 and not less than 30 min, preferably 0-30 min; the volume ratio of phase A:phase B is 70-80:20-30-70-80:20-30, preferably 75:25-75:25.
[0048] Preferably, in step 3), the external standard method refers to: respectively taking a series of different volumes of the reference solution of step 1), respectively preparing a series of solutions of different concentrations, and using a high performance liquid chromatograph for sample analysis to obtain a linear relationship between the concentration and peak area of sucrose in the reference solution, and using the chromatographic peak area of sucrose to correspond to its corresponding concentration, drawing a corresponding standard working curve, and calculating the regression equation of the standard working curve. Then, the test solution of step 2) is detected by a high performance liquid chromatograph, and the obtained chromatographic peak area of sucrose in the test solution is respectively substituted into the regression equation of the standard working curve to calculate the content of sucrose.
[0049] More preferably, in the standard working curve, the peak area of sucrose is used as the ordinate, and the concentration of sucrose in the reference solution is used as the abscissa.
[0050] Preferably, the linear fitting of the Brix value and the sucrose content is processed using Minitab software.
[0051] The water used in the present invention is all purified water.
[0052] As described above, the present invention provides a method for rapid detection of sucrose content in dry ginseng medicinal materials, which has the following beneficial effects:
[0053] (1) Since the saccharimeter uses the principle of refractive index for analysis, the lower the sugar concentration in the solution, the smaller the corresponding refractive index and the lower the saccharimetric value. The saccharimetric value of the ginseng medicinal material extract was detected by a saccharimeter, and the sucrose content therein was detected by high performance liquid chromatography. A calibration model of sucrose content and saccharimetric value in ginseng medicinal materials was established by linear fitting. The model is accurate and reliable and can realize rapid detection of sucrose content in ginseng medicinal materials.
[0054] (2) The present invention provides a method for rapid detection of sucrose content in dry ginseng medicinal materials, which uses a saccharimeter as a technical support and a liquid phase method as a reference basis, and can accurately and rapidly obtain the sucrose content.
[0055] (3) The present invention provides a rapid detection method for the sucrose content in dry ginseng medicinal materials. The sample pretreatment is simple, the detection time can be completed within half an hour, the required equipment is relatively low in price, and it is relatively easy to train the detection personnel. Therefore, ginseng processing enterprises that do not have laboratory conditions or relevant technical personnel can realize the rapid detection of ginseng sucrose. BRIEF DESCRIPTION OF THE DRAWINGS
[0056] Figure 1 The chromatogram shown is a chromatogram of the present invention for detecting the sucrose content in dry ginseng medicinal materials after cold soaking extraction, wherein 1 is sucrose.
[0057] Figure 2 The chromatogram shown is a chromatogram of the present invention for detecting the sucrose content in dry ginseng medicinal materials after ultrasonic extraction, wherein 1 is sucrose and 2 is maltose.
[0058] Figure 3 Shown is a fitting curve diagram of sucrose and sugar content in the present invention.
[0059] Figure 4 It is shown as the residual normal probability plot in the present invention.
[0060] Figure 5 Shown is the observed value sequence diagram of the residual in the present invention. DETAILED DESCRIPTION
[0061] The present invention is further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not used to limit the scope of protection of the present invention.
[0062] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.
[0063] The reagents and instruments used in the following examples are as follows:
[0064] 1. Reagents
[0065] Reference substance: sucrose (China Food and Drug Inspection Institute, batch number: 111507-202406, purity ≥99.80%).
[0066] Samples: All ginseng medicinal materials are five-year-old ginseng, and the specific 50 batches are shown in Table 1 below.
[0067] Table 1
[0068]
[0069] Reagents: ethanol (analytical grade AR, Sinopharm Chemical Reagent Co., Ltd.), acetonitrile (chromatographic grade, Thermo Fisher Scientific), and ultrapure water were prepared by Milli-Q Advantage A10 ultrapure water system (Merck Millipore, Germany).
[0070] 2. Instruments
[0071] Agilent 1260 high performance liquid chromatograph (Agilent, USA), G4260B evaporative light scattering detector (Agilent, USA), XS205 analytical electronic balance (Mettler Toledo, Switzerland), HH-4 digital constant temperature water bath (Changzhou Guohua Electric Co., Ltd.), Diye professional saccharimeter (accuracy 0.1%, Shenzhen Liushu Technology Co., Ltd.), rechargeable juicer (300 mL, WMF, Germany).
[0072] Example 1
[0073] 1. Sample pretreatment
[0074] Preparation of sample solution: Take 1 g of powder of dry ginseng sample from batch 20221103, accurately weigh it, add 5 mL of water, soak it in cold water for 10 min, use a garlic press (with four layers of 100-mesh nylon gauze on the bottom) to squeeze out the ginseng juice, filter it with a 0.45 μm microporous filter membrane, and use it as sample solution 1# for later use.
[0075] 2. Determine the sugar content
[0076] The sugar content of sample solution 1# is measured using a sugar meter to obtain the sugar content value of sample solution 1#.
[0077] Specifically, click the power button of the saccharimeter to turn it on, drop clean water in (it must completely cover the bottom of the glass), press it short and long until it displays "Calibrating" to enter the calibration state, and you can let go when the screen displays "Calibrating". After the calibration is completed, the displayed sugar content value should be 0%.
[0078] Then click the start button of the saccharimeter, drip sample solution 1#2 drops (need to completely cover the bottom of the glass), click to test, and record the sugar content. For the same sample, test twice and take the average value.
[0079] 3. Preparation of reference solution
[0080] Accurately weigh the sucrose reference substance, add water to make a reference substance solution containing 1.5 mg and 0.3 mg of each per 1 mL, shake well, and the solution is ready.
[0081] 4. Preparation of test solution
[0082] Dilute sample solution 1# by 5 times with ultrapure water, and filter through a 0.45 μm microporous filter membrane to obtain test solution 1#.
[0083] 5. Determination of sucrose content
[0084] The test solution and reference solution were determined by high performance liquid chromatography, and the sucrose content in the test solution was calculated by the external standard method.
[0085] The chromatographic conditions of the high performance liquid chromatography method are as follows: the chromatographic column is a Prevail Carbohydrate ES chromatographic column (4.6mm×250mm, 5μm); the detector is an evaporative light scattering detector (ELSD), and the drift tube temperature is 45°C; the column temperature is 30°C; the flow rate is 1.0mL / min; the mobile phase is acetonitrile-water, wherein phase A is acetonitrile and phase B is water; isocratic elution is used, and the analysis time is 30min.
[0086] The specific procedure of isocratic elution is: 0-30min, the volume ratio of phase A:phase B is 75:25-75:25.
[0087] 6. Establish a calibration model
[0088] The sugar content and sucrose content were linearly fitted to establish a calibration model for the sucrose content and sugar content in ginseng medicinal materials. The fitting curve in the calibration model was calculated according to formula (1), wherein the formula (1) is: sucrose = 5.258 × sugar content - 23.35. The sucrose content in the dry ginseng sample was determined by fitting the calibration model with the measured sugar content.
[0089] Example 2
[0090] 1. Sample pretreatment
[0091] Preparation of sample solution: Take 1 g of powder of dry ginseng sample from batch 220701R1, accurately weigh it, add 4 mL of water, soak it in cold water for 30 min, press out the ginseng juice with a garlic press (with 5 layers of 90-mesh nylon gauze on the bottom), filter it with a 0.45 μm microporous filter membrane, and use it as sample solution 2# for later use.
[0092] 2. Determine the sugar content
[0093] The sugar content of sample solution 2# is measured using a saccharimeter to obtain the sugar content value of sample solution 2#.
[0094] Specifically, click the power button of the saccharimeter to turn it on, drop clean water in (it must completely cover the bottom of the glass), press it short and long until it displays "Calibrating" to enter the calibration state, and you can let go when the screen displays "Calibrating". After the calibration is completed, the displayed sugar content value should be 0%.
[0095] Then click the start button of the saccharimeter, drip 2#3 drops of sample solution (need to completely cover the bottom of the glass), click to test, and record the sugar content. For the same sample, test twice and take the average value.
[0096] 3. Preparation of reference solution
[0097] Accurately weigh the sucrose reference substance, add water to make a reference substance solution containing 1.5 mg and 0.3 mg of each per 1 mL, shake well, and the solution is ready.
[0098] 4. Preparation of test solution
[0099] Dilute sample solution 2# by 6 times with ultrapure water, and filter through a 0.45 μm microporous filter membrane to obtain test solution 2#.
[0100] 5. Determination of sucrose content
[0101] The test solution and reference solution were determined by high performance liquid chromatography, and the sucrose content in the test solution was calculated by the external standard method.
[0102] The chromatographic conditions of the high performance liquid chromatography method are as follows: the chromatographic column is a Prevail Carbohydrate ES chromatographic column (4.6mm×250mm, 5μm); the detector is an evaporative light scattering detector (ELSD), and the drift tube temperature is 48°C; the column temperature is 32°C; the flow rate is 0.8mL / min; the mobile phase is acetonitrile-water, wherein phase A is acetonitrile and phase B is water; isocratic elution is used, and the analysis time is 30min.
[0103] The specific procedure of isocratic elution is: 0-30min, the volume ratio of phase A:phase B is 76:24-76:24.
[0104] 6. Establish a calibration model
[0105] The sugar content and sucrose content were linearly fitted to establish a calibration model for the sucrose content and sugar content in ginseng medicinal materials. The fitting curve in the calibration model was calculated according to formula (1), wherein the formula (1) is: sucrose = 5.258 × sugar content - 23.35. The sucrose content in the dry ginseng sample was determined by fitting the calibration model with the measured sugar content.
[0106] Example 3
[0107] 1. Sample pretreatment
[0108] Preparation of sample solution: Take the powder of dry ginseng sample from batch 230102, accurately weigh 1 g, add 10 mL of water, perform ultrasonic extraction for 60 min, filter with a 0.45 μm microporous filter membrane, and use this as sample solution #3 for later use.
[0109] 2. Determine the sugar content
[0110] The sugar content of sample solution 3# is measured using a saccharimeter to obtain the sugar content value of sample solution 3#.
[0111] Specifically, click the power button of the saccharimeter to turn it on, drop clean water in (it must completely cover the bottom of the glass), press it short and long until it displays "Calibrating" to enter the calibration state, and you can let go when the screen displays "Calibrating". After the calibration is completed, the displayed sugar content value should be 0%.
[0112] Then click the start button of the saccharimeter, add 2 drops of sample solution 3# (need to completely cover the bottom of the glass), click to test, and record the sugar content. For the same sample, test twice and take the average value.
[0113] 3. Preparation of reference solution
[0114] Accurately weigh the sucrose reference substance, add water to make a reference substance solution containing 1.5 mg and 0.3 mg of each per 1 mL, shake well, and the solution is ready.
[0115] 4. Preparation of test solution
[0116] Dilute sample solution 3# by 4 times with ultrapure water, and filter through a 0.45 μm microporous filter membrane to obtain test solution 3#.
[0117] 5. Determination of sucrose content
[0118] The test solution and reference solution were determined by high performance liquid chromatography, and the sucrose content in the test solution was calculated by the external standard method.
[0119] The chromatographic conditions of the high performance liquid chromatography method are as follows: the chromatographic column is a Prevail Carbohydrate ES chromatographic column (4.6mm×250mm, 5μm); the detector is an evaporative light scattering detector (ELSD), and the drift tube temperature is 48°C; the column temperature is 28°C; the flow rate is 1.2mL / min; the mobile phase is acetonitrile-water, wherein phase A is acetonitrile and phase B is water; isocratic elution is used, and the analysis time is 30min.
[0120] The specific procedure of isocratic elution is: 0-30min, volume ratio of phase A:phase B is 73:27-73:27.
[0121] 6. Establish a calibration model
[0122] The sugar content and sucrose content were linearly fitted to establish a calibration model for the sucrose content and sugar content in ginseng medicinal materials. The fitting curve in the calibration model was calculated according to formula (1), wherein the formula (1) is: sucrose = 5.258 × sugar content - 23.35. The sucrose content in the dry ginseng sample was determined by fitting the calibration model with the measured sugar content.
[0123] Example 4
[0124] The 50 batches of dried ginseng samples shown in Table 1 were measured for sugar content according to Example 1, and the obtained sugar content ranged from 6.315% to 8.510%. The sucrose content was measured according to Example 1, and the obtained sucrose content ranged from 10.41% to 21.87%. The specific results are shown in Table 2. The correlation (Pearson correlation) analysis in Minitab (version: 10.0.17763) software was used, and the correlation coefficient between sugar content and sucrose was 0.922.
[0125] Table 2
[0126]
[0127] Then, the sucrose content was used as the horizontal axis and the sugar content was used as the vertical axis to fit the line graph, and a linear regression analysis was performed. The fitting curve was: sucrose = 5.258 × sugar content - 23.35. Figure 3-5 .
[0128] Depend on Figure 3 It can be seen that in the fitting relationship, the P value is 0.000, indicating that the association between sucrose and sugar content is statistically significant. The R-Sq of 85.0% indicates that the sucrose content can explain approximately 85% of the variation in sugar content. The S value represents the standard deviation of the distance between the data value and the fitted value, measured in the unit of the response variable. S can be used to evaluate the degree to which the model describes the response value. The lower the S value, the more difficult it is for the model to describe the response. The S value of this model is 1.2117, so the model fit is good.
[0129] At the same time, from Figure 4 The residual normal probability plot shows that the residual probability plot is roughly a straight line, and the residual values are all less than 2.80. Figure 5 The observed value sequence diagram shows that the residuals in the diagram are randomly distributed around the center line. In summary, the model has good linearity and the prediction results are reliable.
[0130] Example 5
[0131] Take 1g of ginseng powder (batch number: 230901), weigh it accurately, add 3, 4, 5, and 10 times of ultrapure water respectively, mix well, ultrasonicate for 60 minutes, filter, pass through a 0.45μm microporous filter membrane, and measure the sugar content and sucrose content of the obtained sample solution according to the conditions of Example 1. From the results, when the extraction times are 4, 5, and 10 times, the sucrose content in the sample can be extracted relatively well. However, when the extraction times is 5, the sucrose can be effectively extracted completely, and the sugar content value can be within the appropriate detection range without being too high or too low. Therefore, the extraction times is determined to be 5 times. See Table 3 for details.
[0132] Table 3
[0133]
[0134] Example 6
[0135] Take 1g of ginseng powder (batch number: R20231002), weigh accurately, add 5mL of ultrapure water, mix well, extract by ultrasonic and cold soaking respectively, filter, pass through 0.45μm microporous filter membrane, and measure the sugar content and sucrose content of the obtained sample solution according to the conditions of Example 1. The results are shown in Table 4. From Table 4, it can be seen that both extraction methods can completely extract sucrose, and the deviation of sucrose content between the two extraction methods is 0.24%. However, the sugar content value of ultrasonic extraction is higher than that of cold soaking extraction. According to liquid chromatography, the sugar content of the sample solution is 0.24%. Figure 1 , 2 It shows that ultrasonic extraction increases the maltose component compared to cold soaking. The increase of maltose increases the sugar content value. Therefore, cold soaking is chosen to reduce the interference of sucrose detection.
[0136] Table 4
[0137]
[0138] Example 7
[0139] Take 1g of ginseng powder (batch number: 230901), accurately weigh, add 5mL of water, cold soak for 2min, 5min, 10min, and 30min, filter, pass through a 0.45μm microporous filter membrane, and measure the sugar content and sucrose content of the obtained sample solution according to the conditions of Example 1. The results show that the RSD% of sugar content is 0.98 and the RSD% of sucrose content is 2.45 in the four extraction times. The specific results are shown in Table 5. It can be seen that there is no significant difference in the detection of ginseng powder sugar content by cold soaking for 2min-30min. However, the extraction time is set to 10 minutes, which is more moderate, so the extraction time is set to 10 minutes.
[0140] Table 5
[0141]
[0142] Comparative test example 1
[0143] The same dry ginseng sample was taken and the sucrose content in the dry ginseng sample was determined by two methods respectively.
[0144] First, the sucrose content in the dry ginseng sample was determined by high performance liquid chromatography, and the corresponding detection conditions were the same as step 5 in Example 1. The determination results are shown in Table 6 below.
[0145] Secondly, the sugar content of the dry ginseng sample was determined by using a saccharimeter, and then the sucrose content in the dry ginseng sample was determined by fitting the determined calibration model. The determination results are shown in Table 6 below.
[0146] Table 6
[0147] Determination of sucrose content by HPLC Calibration model for determination of sucrose content Pre-processing steps Complicated Simple Reference solution need unnecessary Testing Instruments High performance liquid chromatography Brix Meter Instrument Price expensive Cheap Operator Requires specially trained professionals to operate Simple training of personnel can be operated 1 sample measurement time 5h 30min
[0148] As can be seen from Table 6, the present invention determines the content of sucrose in the dry ginseng sample by establishing a calibration model for fitting, which can quickly and accurately detect the sucrose content in the dry ginseng with low cost and good accuracy.
[0149] In summary, the present invention provides a rapid detection method for sucrose content in dry ginseng medicinal materials, which can establish a calibration model of sucrose content and sugar content in ginseng medicinal materials through linear fitting. The model is accurate and reliable, and can accurately and quickly obtain the sucrose content. Therefore, the present invention overcomes various shortcomings in the prior art and has high industrial utilization value.
[0150] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.
Claims
1. A rapid detection method for sucrose content in dry ginseng medicinal materials, comprising: The sugar content and sucrose content of the sample solution obtained after pretreatment of the dry ginseng sample are respectively measured, and then the sugar content and the sucrose content are linearly fitted to establish a correction model of the sucrose content and sugar content in the dry ginseng sample, and the sucrose content in the dry ginseng sample is determined by fitting the correction model with the measured sugar content; the fitting curve in the correction model of the sucrose content and sugar content in the dry ginseng sample is calculated according to formula (1), and the formula (1) is: sucrose = 5.258 × sugar content - 23.
35.
2. The method for rapid detection of sucrose content in dry ginseng medicinal materials according to claim 1, characterized in that: Includes any one or more of the following conditions: A1) the dry ginseng sample is in powder form; A2) The pretreatment comprises: adding a solvent to the dry ginseng sample for extraction, and filtering to obtain a sample solution.
3. The method for rapid detection of sucrose content in dry ginseng medicinal materials according to claim 2, characterized in that: A2) includes any one or more of the following conditions: A21) the solvent is water; A22) the ratio of the added mass of the dry ginseng sample to the added volume of the solvent is 1:4-10, g / mL; A23) the extraction is selected from one of cold soaking extraction and ultrasonic extraction; A24) The filtration is membrane filtration.
4. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 3, characterized in that: Also includes any one or more of the following conditions: A231) In A23), the cold soaking extraction comprises squeezing the juice after cold soaking; A241) In A24), the filter membrane is a 0.45 μm filter membrane.
5. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 4, characterized in that: A231) also includes any one or more of the following conditions: A2311) The cold soaking time is 2-30min; A2312) The juicing process uses a garlic press to squeeze out the ginseng juice.
6. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 1, characterized in that: The determination of the sugar content includes: measuring the sugar content of the sample solution with a sugar meter to obtain the sugar content of the sample solution.
7. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 1, characterized in that: The determination of the sucrose content comprises the following steps: 1) Add sucrose reference substance to solvent, dissolve it and make up to volume to obtain reference substance solution; 2) Dilute the sample solution with water and filter it to obtain the test solution; 3) using high performance liquid chromatography to measure the test solution of step 2) and the reference solution of step 1), respectively, and calculating the content of sucrose in the test solution by an external standard method.
8. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 7, characterized in that: In step 1) or 2), any one or more of the following conditions are included: B1) In step 1), the solvent is water; B2) In step 1), the content of sucrose in the reference solution is in the range of 0.3-1.5 mg / mL; B3) In step 2), the sample solution is diluted with water by 4-6 times; B4) In step 2), the filtration is membrane filtration; preferably, the membrane is a 0.45 μm membrane.
9. The method for rapid detection of sucrose content in dry ginseng medicinal material according to claim 7, characterized in that: In step 3), any one or more of the following conditions are included: C1) The chromatographic column in the high performance liquid chromatography is an ES chromatographic column; C2) The detector in the high performance liquid chromatography is an evaporative light scattering detector; C3) In the high performance liquid chromatography, the column temperature is 25-35°C; C4) In the high performance liquid chromatography, the flow rate is 0.1-2 mL / min; C5) In the high performance liquid chromatography, the mobile phase is acetonitrile-water, wherein phase A is acetonitrile and phase B is water; C6) In the high performance liquid chromatography, isocratic elution is adopted and the analysis time is not less than 30 minutes.
10. A rapid detection method for sucrose content in dry ginseng medicinal material according to claim 9, characterized in that: Also includes any one or more of the following conditions: C11) In item C1), the chromatographic column used in the HPLC method is a Prevail Carbohydrate ES chromatographic column, 4.6 mm×250 mm, 5 μm; C21) In item C2), the drift tube temperature of the evaporative light scattering detector is 40-50°C; C61) In item C6), the analysis time is 30 min; C62) In item C6), the specific procedure of the isocratic elution is: the analysis time is greater than 0 and not less than 30 min; the volume ratio of phase A:phase B is 70-80:20-30-70-80:20-30.