Chromatographic detection method for compound folium cortex eucommiae preparation

Abstract

The invention relates to the technical field of chromatographic detection, in particular to a chromatographic detection method for a compound folium cortex eucommiae preparation. The method comprises the following steps: preparing a preparation sample according to the proportion of components of a prescription, and pretreating to obtain a to-be-detected sample solution; putting the sample solution into a chromatographic column and carrying out chromatographic separation to obtain a separated component; putting the components into a detector and carrying out chromatographic analysis to obtain a chromatogram; analyzing the chromatogram to obtain the proportion of a plurality of components in the sample, and correspondingly comparing the proportion with the proportion of a plurality of components in the comparison table to determine the proportion difference value of a single component; judging whether the chromatographic detection process meets the standard or not on the basis of a comparison result of the proportion difference values of the components and a preset value, generating a corresponding instruction when the chromatographic detection process does not meet the standard, and determining a corresponding processing mode on the basis of the instruction; the chromatographic detection process is optimized in a treatment mode to improve the detection precision of the chromatographic detection method on the pharmaceutical preparation, so that the influence of insufficient detection precision on the detection link of the pharmaceutical preparation is avoided.

Description

Technical Field

[0001] The invention relates to the technical field of chromatographic detection, and in particular to a chromatographic detection method for a compound eucommia leaf preparation. Background Art

[0002] With the rapid development of chromatographic detection technology, the role of chromatographic detection technology in multiple links such as drug research and development, production, and quality control is becoming more and more important. Chromatographic detection technology can be used to separate and identify various components in drugs, thereby ensuring the safety and effectiveness of drugs; for example, in the production application and quality control of drugs, chromatographic detection technology can be used to identify and analyze the components of drugs to ensure that the quality of the product meets the drug quality requirements.

[0003] When using chromatographic detection methods for analysis in the prior art, the drugs targeted are mostly composed of a single component. It is not in line with the actual situation to use a single component as a quality control indicator to judge the quality of multi-component drugs. For example, for a certain type of preparation mainly composed of Eucommia leaves and other components as auxiliary components, the drug components in the preparation are of various types and in different quantities. The existing chromatographic detection technology has the problem of being unable to optimize the chromatographic detection process based on the detected component ratio, thereby achieving self-adjustment to improve the detection accuracy of chromatographic detection of multi-component drugs. Summary of the invention

[0004] To this end, the present invention provides a chromatographic detection method for a compound eucommia leaf preparation, which is used to solve the problem that the chromatographic detection technology in the prior art cannot achieve self-regulation to improve the chromatographic detection accuracy when performing chromatographic detection on multi-component drugs.

[0005] To achieve the above object, the present invention provides a chromatographic detection method for a compound Eucommia ulmoides leaf preparation, comprising:

[0006] Preparing a preparation sample according to the proportion of each component in the prescription, and pre-treating the preparation sample to obtain a sample solution to be tested;

[0007] Placing the sample solution to be tested into a chromatographic column, and performing chromatographic separation on the sample solution to be tested to obtain separated components;

[0008] placing the separated components into a detector, and performing chromatographic analysis on the separated components to obtain a chromatogram;

[0009] Analyzing the chromatogram to obtain the ratios of several components in the preparation sample, and sequentially comparing the ratios of several components with the ratios of several components in the comparison table to determine the difference in the ratios of the components;

[0010] Determining whether the chromatographic detection process meets the standard based on the comparison results of the difference values ​​of the component ratios and the corresponding preset values, and generating corresponding instructions when it does not meet the standard;

[0011] The length of the chromatographic column, the illumination wavelength of the detector, or the transport speed of the sample solution entering the chromatographic column is determined based on the instruction.

[0012] Further, the process of determining whether the chromatographic detection process meets the standard based on the comparison results of the difference values ​​of the component ratios and the corresponding preset values ​​includes:

[0013] Calculate the average of the differences in the proportions of the components and record it as the average difference in proportions;

[0014] Based on the comparison result of the mean difference of the ratio with the preset mean difference of the ratio, or based on the number of components in the preparation sample, determining whether the chromatographic detection process meets the standard;

[0015] When it is determined that the chromatographic detection process does not meet the standard, the reason why the chromatographic detection process does not meet the standard is determined according to the difference between the proportional average difference and the preset proportional average difference.

[0016] Further, the process of determining whether the chromatographic detection process meets the standard based on the number of components in the preparation sample includes:

[0017] Counting the amount of the components in the preparation sample;

[0018] Whether to increase the length of the chromatographic column is determined based on a comparison result of the component quantity with a preset component quantity.

[0019] Further, the process of determining whether to increase the length of the chromatographic column based on the comparison result of the number of components and the preset number of components includes:

[0020] Calculating the difference between the number of components and the preset number of components, and recording the difference as the difference in number of components;

[0021] Based on the comparison result of the component quantity difference and the preset component quantity difference, it is determined that the length of the chromatographic column is increased, and the increase in the length is proportional to the component quantity difference.

[0022] Further, the process of determining the reason why the chromatographic detection process does not meet the standard according to the difference between the ratio average difference and the preset ratio average difference includes:

[0023] Calculate the difference between the proportional mean difference and the preset proportional mean difference, and record it as the second-order proportional mean difference;

[0024] Determining the reason why the chromatographic detection process does not meet the standard based on the comparison result of the second-order ratio average difference and the preset second-order ratio average difference;

[0025] Determining corresponding treatment based on the cause includes: determining the irradiation wavelength of the detector, adjusting the delivery speed of the sample solution to be tested into the chromatographic column, or calculating the component variance based on the difference in several component proportions and re-determining the cause of non-compliance with the standard based on the component variance.

[0026] Further, the process of determining the illumination wavelength of the detector includes:

[0027] Based on the comparison result of the light reflectance average value and the preset light reflectance average value, it is determined that the irradiation wavelength is increased, and the increase amplitude of the irradiation wavelength is inversely proportional to the light reflectance average value;

[0028] When the detector illuminates the separated components, it obtains the light reflectance corresponding to each component, calculates the average value of several light reflectances, and records it as the light reflectance average value.

[0029] Further, when the illumination wavelength adjustment is completed, it is determined based on the comparison result of the component quantity ratio and the preset component quantity ratio that the light source intensity of the detector is increased, and the increase range of the light source intensity is inversely proportional to the component quantity ratio;

[0030] The ratio between the preset component quantity and the component quantity is calculated and recorded as the component quantity ratio.

[0031] Further, the process of calculating the component variance according to the difference in the component proportions and re-determining the reasons for non-compliance with the standard based on the component variance includes:

[0032] Based on the comparison result of the component variance and the preset component variance, the irradiation wavelength of the detector is determined, the conveying speed of the sample solution to be tested into the chromatographic column is adjusted, or the preparation sample is remade.

[0033] Further, the process of determining the transport speed of the sample solution to be tested into the chromatographic column includes:

[0034] Determining to reduce the conveying speed based on a comparison result of the component variance difference and a preset component variance difference, and the reduction range of the conveying speed is proportional to the component variance difference;

[0035] The difference between the component variance and the preset component variance is calculated and recorded as the component variance difference.

[0036] Furthermore, when the conveying speed is reduced, the replacement period of the filter device in the pretreatment is extended based on the comparison result of the speed reduction amount with the preset speed reduction amount, and the extension of the replacement period is proportional to the speed reduction amount.

[0037] Compared with the prior art, the chromatographic detection method for the compound eucommia leaf preparation of the present invention has the beneficial effect that the method prepares the preparation sample according to the proportion of each component of the prescription and performs pretreatment to obtain the sample solution to be tested; the sample solution to be tested is placed in a chromatographic column and chromatographically separated to obtain separated components; the separated components are placed in a detector and chromatographically analyzed to obtain a chromatogram; the chromatogram is analyzed to obtain the proportions of several components in the preparation sample, and the proportions of several components in the comparison table are compared accordingly to determine the difference in the proportion of a single component; based on the comparison result of the difference in the proportions of several components with the corresponding preset values, it is determined whether the chromatographic detection process meets the standard, and a corresponding instruction is generated when it does not meet the standard, and the length of the chromatographic column, the irradiation wavelength of the detector, or the conveying speed of the sample solution to be tested into the chromatographic column are determined based on the instruction; the chromatographic detection process is optimized by a corresponding processing method, and self-adjusted to improve the detection accuracy of the chromatographic detection method for drug preparations, thereby improving the detection accuracy of the component proportions of such drug preparations, thereby avoiding the impact of insufficient detection accuracy on the detection link of drug preparations.

[0038] Furthermore, the present invention further determines whether the chromatographic detection process meets the standards based on the comparison result of the ratio average difference and the preset ratio average difference. When it is determined based on the comparison result that the chromatographic detection process does not meet the standards, the difference between the ratio average difference and the preset ratio average difference can be calculated, and the reason for not meeting the standards can be determined based on the difference, and then the specific reason can be processed, thereby optimizing the chromatographic detection method and improving the chromatographic detection accuracy.

[0039] Furthermore, the present invention, based on the comparison result between the mean difference of the proportions and the preset mean difference of the proportions, further re-judges the chromatographic detection process according to the comparison result between the number of components in the preparation sample and the preset number of components, thereby improving the accuracy and reliability of the analysis of the chromatographic detection process.

[0040] Furthermore, when determining to increase the length of the chromatographic column based on the comparison result of the component quantity and the preset component quantity, the present invention can determine the increase in the length of the chromatographic column based on the comparison result of the component quantity difference and the preset component quantity difference. In this way, the separation time of the sample solution to be tested can be extended in a targeted manner, the degree of separation can be improved, and the influence of the component quantity on the chromatographic detection process can be reduced, thereby improving the accuracy of the chromatographic detection.

[0041] Furthermore, when the present invention determines that the reason why the chromatographic detection process does not meet the standards is that there is a problem when using the detector to perform chromatographic analysis on the separated components based on the comparison result of the second-order ratio mean difference and the preset second-order ratio mean difference, it is determined that the irradiation wavelength of the detector needs to be readjusted, and the increase in the irradiation wavelength can be determined based on the comparison result of the light reflectance average value and the preset light reflectance average value. In this way, the light reflectance can be improved, and then the detection sensitivity of the detector can be improved, thereby improving the accuracy of the chromatographic detection.

[0042] Furthermore, when analyzing the reasons why the chromatographic detection process does not meet the standards, in order to more accurately determine the reasons, the present invention further determines the reasons why the chromatographic detection process does not meet the standards based on the comparison results of the component variances and the preset component variances, and determines the corresponding processing methods, thereby improving the accuracy and reliability of the analysis of the reasons why the standards are not met.

[0043] Furthermore, the present invention also determines that the reason why the chromatographic detection process does not meet the standards is that there are problems in the pretreatment of the preparation samples, and that there are more impurities remaining in the sample solution to be tested due to insufficient filtration based on the comparison result of the second-order ratio mean difference with the preset second-order ratio mean difference. When this is determined, it is necessary to readjust the delivery speed of the sample solution to be tested entering the chromatographic column, and the reduction range of the delivery speed can be determined based on the comparison result of the component variance difference with the preset component variance difference. In this way, the filtration efficiency can be improved, thereby ensuring that the detection data in the subsequent chromatographic analysis is more accurate, thereby improving the accuracy of the chromatographic detection.

[0044] Furthermore, on the basis of determining to reduce the conveying speed, the present invention can also determine the extension time of the replacement cycle of the filter device based on the comparison result of the speed reduction amount and the preset speed reduction amount. In this way, the use cost of the equipment required for chromatographic detection can be saved by extending the replacement cycle of the filter device. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 It is a module schematic diagram of a chromatographic detection method for a compound Eucommia ulmoides leaf preparation in the present invention;

[0046] Figure 2 It is a schematic flow diagram of a chromatographic detection method for a composite Eucommia leaf preparation in the present invention;

[0047] Figure 3 It is a logic flow chart for determining whether the chromatographic detection process meets the standard based on the proportional average difference in the present invention;

[0048] Figure 4 A logic flow chart of determining the reason why the chromatographic detection process does not meet the standard and the corresponding processing method based on the second-order ratio average difference in the present invention;

[0049] Figure 5 The present invention is a logic flow chart for re-determining the reasons why the chromatographic detection process does not meet the standards based on component variance and the corresponding processing methods. DETAILED DESCRIPTION

[0050] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0051] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0052] It should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the term "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0053] See also Figure 1As shown, it is a module schematic diagram of a system for a chromatographic detection method for compound Eucommia leaf preparation in the present embodiment. The system includes a sample preparation module, a sample pretreatment module, a chromatographic separation module, a chromatogram making module, a statistical module, an analysis module, and an adjustment module. Specifically, in the present embodiment, the preparation sample is made by the sample preparation module, and in the process of making the preparation sample, the component ratio of the preparation sample is strictly proportioned according to the prescription, and the preparation sample is solid. The sample pretreatment module connected to the sample preparation module is pretreated for the preparation sample to obtain a sample solution to be tested, and the pretreatment process includes grinding, sieving, extraction, and filtering, wherein the extraction method includes ultrasonic extraction and reflux extraction, and an appropriate amount of solvent (such as acetonitrile, methanol, etc.) is added during the extraction process, and filtering is to remove insoluble impurities to obtain a sample solution to be tested that can be detected and analyzed. The chromatographic separation module is connected to the sample pretreatment module, and the chromatographic separation module includes a chromatographic column and a mobile phase, and then the sample solution to be tested is injected into the chromatographic column, and gradient elution is performed by the chromatographic column and the mobile phase to obtain a separation component that can be analyzed by chromatography. The chromatogram making module is connected to the chromatographic separation module, and the chromatogram making module includes a detector, and the separated components flow into the detector. The detector includes a light source and a grating. The light emitted by the light source is dispersed into light of different wavelengths through the grating, and then irradiated on the separated components. After the compound molecules in the separated components absorb light of a specific wavelength, light scattering will occur. The detector captures these scattered lights and converts them into electrical signals, and obtains chromatographic peaks after processing. A chromatogram is drawn based on the chromatographic peaks. The detector in this embodiment uses a variable wavelength detector. The statistical module is connected to the chromatogram making module, and the statistical module includes a component calculation unit and a control unit. The component calculation unit can analyze the retention time and peak area of ​​each chromatographic peak according to the obtained chromatogram, and then can quantitatively calculate the ratio values ​​of several components in the preparation sample in the sample, and then compare the several component ratios with the several component ratios in the control table unit one by one, so as to determine the absolute value of the difference between the single component ratio and the corresponding component ratio, and record the absolute value of the difference as the component ratio difference. The several component ratios in the control unit here can be used as a comparison benchmark. The analysis module is connected to the statistical module. The analysis module obtains a number of component ratio differences and compares the number of component ratio differences with preset values. It can determine whether the current chromatographic detection process meets the preset standards based on the comparison results. If it is determined that the current chromatographic detection process does not meet the standards, the reasons for not meeting the standards can be determined, and then corresponding correction instructions can be generated based on the reasons.The regulating module is respectively connected with the analyzing module, the sample preparing module, the sample pre-processing module, the chromatographic separation module and the chromatogram making module, and determines the length of the chromatographic column, the irradiation wavelength of the detector, or the conveying speed of the sample solution to be tested into the chromatographic column based on the instructions, and optimizes the chromatographic detection process of this time by analyzing and comparing the results, thereby improving the detection accuracy of the component ratio of this type of drug preparation, thereby avoiding the impact of insufficient detection accuracy on the detection link of the drug preparation, and ensuring the quality and safety of the drug preparation.

[0054] In the present embodiment, a prescription of a compound Eucommia leaf preparation is provided. The prescription is based on the theory of "liver, spleen and kidney co-regulation", with Eucommia leaf as the main medicine, with tonifying kidney and strengthening bones, invigorating qi and strengthening spleen as the treatment goals, and the proportion of the medicinal components is 15g of Eucommia leaf, 15g of Ganoderma lucidum, 15g of Pueraria root, 6g of fried Gardenia jasminoides, and 6g of steamed tangerine peel; Usage: 1 dose per day, decocted in water, warm in the morning and evening. The preparation made by the chromatographic detection method in the present embodiment is subjected to chromatographic detection to accurately determine the proportion of each component in the preparation, thereby providing a reliable detection means for the production process of the preparation, so as to better ensure the quality of the preparation. The chromatographic detection method in the present embodiment can be applied to, including but not limited to, compound Eucommia leaf preparations.

[0055] See also Figure 2 As shown, it is a schematic flow diagram of a chromatographic detection method for a compound Eucommia leaf preparation in this embodiment. The process includes the following steps:

[0056] S1: Prepare a preparation sample according to the proportion of each component in the prescription, and pretreat the preparation sample to obtain a sample solution to be tested.

[0057] S2: placing the sample solution to be tested into a chromatographic column, and performing chromatographic separation on the sample solution to be tested to obtain separated components.

[0058] S3: placing the separated components into a detector, and performing chromatographic analysis on the separated components to obtain a chromatogram.

[0059] S4: Analyze the chromatogram to obtain the ratios of several components in the preparation sample, and compare the ratios of several components with the ratios of several components in the comparison table in turn to determine the difference in the ratios of the components.

[0060] S5: Determine whether the chromatographic detection process meets the standard based on the comparison results of the difference values ​​of the component proportions and the corresponding preset values, and generate corresponding instructions when it does not meet the standard.

[0061] S6: Determine the length of the chromatographic column, the illumination wavelength of the detector, or the transport speed of the sample solution entering the chromatographic column based on the instruction.

[0062] See also Figure 3 As shown, it is a logic flow chart for determining whether the chromatographic detection process meets the standard based on the average difference of the proportions in this embodiment. The process of determining whether the chromatographic detection process meets the standard based on the comparison results of the difference of the component proportions and the corresponding preset values ​​includes:

[0063] Calculate the average value of several component ratio differences and record it as the ratio average difference; determine whether the chromatographic detection process meets the standards based on the comparison result of the ratio average difference and the preset ratio average difference, or, based on the number of components in the preparation sample; when it is determined that the chromatographic detection process does not meet the standards, determine the reason why the chromatographic detection process does not meet the standards based on the difference between the ratio average difference and the preset ratio average difference.

[0064] Specifically, in this embodiment, the preset ratio average difference H0 can be divided into a first preset ratio average difference H1 and a second preset ratio average difference H2, and the preset ratio average difference standard H3=3%, H1=0.85×H3, H2=1.35×H3 is set. It should be noted that H1, H2 and H3 can be set as needed; the comparison process based on the ratio average difference H with H1 and H2 is as follows:

[0065] If the average ratio difference H is less than or equal to the first preset average ratio difference H1, it means that the average ratio difference H under the current chromatographic detection is relatively small, that is, the ratio of each component in the preparation sample is not much different from the ratio of each component in the control. Therefore, it can be determined that the chromatographic detection process meets the preset standards.

[0066] If the average ratio difference H is greater than the first preset average ratio difference H1 and less than or equal to the second preset average ratio difference H2, it is impossible to accurately determine whether the chromatographic detection process meets the preset standard based on the average ratio difference H. It is necessary to compare the component quantity B in the preparation sample with the preset component quantity B0, and then re-judge the chromatographic detection process based on the comparison results.

[0067] If the average ratio difference H is greater than the second preset average ratio difference H2, it means that the average ratio difference H under the current chromatographic detection is relatively large, that is, the difference between the proportions of each component in the preparation sample and the proportions of each component in the control is large, exceeding the preset standard too much, so it can be determined that the chromatographic detection process does not meet the preset standard; at this time, the reason for non-compliance with the standard can be determined based on the difference between H and H0, more specifically, the difference between H and H2 is calculated.

[0068] Further, the process of determining whether the chromatographic detection process meets the standard based on the number of components in the preparation sample includes:

[0069] Counting the number of the components in the preparation sample; and determining whether to increase the length of the chromatographic column based on a comparison result of the number of the components with a preset number of components.

[0070] Specifically, in this embodiment, the preset number of components B0 is set to 9; the comparison process based on the number of components B and B0 is as follows:

[0071] If the number of components B is less than or equal to the preset number of components B0, it means that the number of components in the current preparation sample is relatively small, and the number of components in the preparation sample will not have a major impact on the chromatographic detection process. On this basis, if the proportion average difference H is still greater than the first preset proportion average difference H1 and less than or equal to the second preset proportion average difference H2, it can be determined that the chromatographic detection process does not meet the preset standards, and the reason why the chromatographic detection process does not meet the standards needs to be determined based on the difference between H and H0.

[0072] If the number of components B is greater than the preset number of components B0, it means that the number of components in the current preparation sample is quite large. The more components in the preparation sample, the worse the quality of the separated components obtained when the sample solution is chromatographically separated. At this time, the length of the chromatographic column can be increased, mainly by replacing it with a new chromatographic column that is longer than the current chromatographic column. This can extend the separation time of the sample solution to be tested, thereby increasing the degree of separation and reducing the impact of the number of components on the chromatographic detection process.

[0073] Further, the process of determining whether to increase the length of the chromatographic column based on the comparison result of the number of components and the preset number of components includes:

[0074] The difference between the number of components and the preset number of components is calculated, and the difference is recorded as the difference in the number of components; based on the comparison result of the difference in the number of components and the preset difference in the number of components, it is determined to increase the length of the chromatographic column, and the increase in the length is proportional to the difference in the number of components.

[0075] Specifically, in this embodiment, when it is determined that the number of components B is greater than the preset number of components B0, the length of the chromatographic column needs to be increased, and the preset component number difference Y0 can be divided into a first preset component number difference Y1 and a second preset component number difference Y2, and the preset component number difference Y3 is set to be 3, Y1=Y3-1, and Y2=Y3+2. It should be noted that Y1, Y2, and Y3 can all change with the change of the number of preparation components; the comparison process based on the component number difference Y and Y1 and Y2 is as follows:

[0076] If the component quantity difference Y is less than or equal to the first preset component quantity difference Y1, it is determined that 2 centimeters need to be added to the original chromatographic column length; if the component quantity difference Y is greater than the first preset component quantity difference Y1 and less than or equal to the second preset component quantity difference Y2, it is determined that 4 centimeters need to be added to the original chromatographic column length; if the component quantity difference Y is greater than the second preset component quantity difference Y2, it is determined that more than 6 centimeters need to be added to the original chromatographic column length. The increase in the length of the chromatographic column is aimed at ensuring that the inaccurate detection caused by the excessive number of components can be reduced. Therefore, the increase in the value can also be corrected to other values ​​without specific limitation. After determining the increase in the value, the corresponding chromatographic column is replaced.

[0077] See also Figure 4 As shown, it is a logic flow chart of determining the reason why the chromatographic detection process does not meet the standard based on the second-order proportional average difference and the corresponding processing method in this embodiment. The process of determining the reason why the chromatographic detection process does not meet the standard based on the difference between the proportional average difference and the preset proportional average difference includes:

[0078] The difference between the mean difference in proportions and the preset mean difference in proportions is calculated and recorded as the second-order mean difference in proportions; the reason why the chromatographic detection process does not meet the standard is determined based on the comparison result of the second-order mean difference in proportions and the preset second-order mean difference in proportions; the corresponding treatment is determined based on the reason, including: determining the irradiation wavelength of the detector, the transport speed of the sample solution to be tested into the chromatographic column, or, calculating the component variance according to several of the component proportion differences and re-determining the reason why it does not meet the standard based on the component variance.

[0079] Specifically, in this embodiment, the preset second-order proportional average difference W0 can be divided into a first preset second-order proportional average difference W1 and a second preset second-order proportional average difference W2, and the preset second-order proportional average difference W3=1.15%, W1=1.2×W3, W2=1.6×W3. It should be noted that W3 can change with the change of H and H2, and the values ​​of W1 and W2 can also be reset; the comparison process based on the second-order proportional average difference W with W1 and W2 is as follows:

[0080] If the second-order proportional average difference W is less than or equal to the first preset second-order proportional average difference W1, it means that the difference between the proportional average difference H and the preset proportional average difference H0 is relatively small. It can be determined that the reason why the chromatographic detection process does not meet the standards is that there is a problem when using the detector to perform chromatographic analysis on the separated components, and it is determined that the irradiation wavelength of the detector needs to be readjusted.

[0081] If the second-order proportion mean difference W is greater than the first preset second-order proportion mean difference W1 and is less than or equal to the second preset second-order proportion mean difference W2, it is impossible to accurately determine the reason for non-compliance with the standard, and it is necessary to calculate the component variance E based on several component proportion differences and re-determine based on the component variance E.

[0082] If the second-order proportion average difference W is greater than the second preset second-order proportion average difference W2, it means that the difference between the proportion average difference H and the preset proportion average difference H0 is relatively large. It can be determined that the reason why the chromatographic detection process does not meet the standards is that there are problems in the pretreatment of the preparation samples, specifically, there are problems with the filtration operation in the pretreatment. Insufficient filtration leads to a large number of residual impurities in the sample solution to be tested, thereby affecting the detection process. It is determined that the delivery speed of the sample solution to be tested entering the chromatographic column needs to be readjusted.

[0083] Further, the process of determining the illumination wavelength of the detector includes:

[0084] Based on the comparison result of the average light reflectance value with the preset average light reflectance value, it is determined to increase the irradiation wavelength and the increase amplitude of the irradiation wavelength is inversely proportional to the average light reflectance value; wherein, when the detector illuminates the separated components, the light reflectance corresponding to each component is obtained, and the average value of several light reflectances is calculated and recorded as the average light reflectance value.

[0085] Specifically, in this embodiment, the light reflectance of each component is used to compare and represent the depth of the color of each component. The smaller the light reflectance, the lighter the color of the corresponding component. The light reflectance can be increased by increasing the irradiation wavelength, thereby improving the detection sensitivity of the detector. The preset light reflectance average value P0 can be divided into a first preset light reflectance average value P1 and a second preset light reflectance average value P2. The preset light reflectance average value P3=30%, P1=0.55×P3, P2=1.85×P3 is set. It should be noted that P3 can be reset as needed, and the coefficients in P1 and P2 can also be set as needed. The comparison process based on the light reflectance average value P with P1 and P2 is as follows:

[0086] If the average light reflectivity value P is less than or equal to the first preset average light reflectivity value P1, the first irradiation wavelength adjustment coefficient is used to increase the irradiation wavelength by 150 nanometers on the original basis; if the average light reflectivity value P is greater than the first preset average light reflectivity value P1 and less than or equal to the second preset average light reflectivity value P2, the second irradiation wavelength adjustment coefficient is used to increase the irradiation wavelength by 80 nanometers on the original basis; if the average light reflectivity value P is greater than the second preset average light reflectivity value P2, the third irradiation wavelength adjustment coefficient is used to increase the irradiation wavelength by 50 nanometers on the original basis. The increase value of the irradiation wavelength can be appropriately adjusted to improve the detection sensitivity of the detector.

[0087] Furthermore, when the irradiation wavelength adjustment is completed, the light source intensity of the detector is increased based on the comparison result of the component quantity ratio and the preset component quantity ratio, and the increase in the light source intensity is inversely proportional to the component quantity ratio; wherein the ratio between the preset component quantity and the component quantity is calculated and recorded as the component quantity ratio.

[0088] Specifically, in this embodiment, after the irradiation wavelength adjustment of the detector is completed, the signal interference between the components needs to be considered. The more components in the preparation, the greater the impact on the detection sensitivity of the detector. At this time, the interference between the signals can be reduced by increasing the intensity of the light source; the preset component quantity ratio F0 can be divided into a first preset component quantity ratio F1 and a second preset component quantity ratio F2. At this time, the preset component quantity B0 is less than the component quantity B, and the preset component quantity ratio standard F3=70%, F1=1.5×F3, F2=2.3×F3 is set. It should be noted that the value of F3 can be set as needed, and the coefficients of F1 and F2 can also be adjusted; the comparison process based on the component quantity ratio F with F1 and F2 is as follows:

[0089] If the component quantity ratio F is less than or equal to the first preset component quantity ratio F1, the light source intensity is increased to 3.35 times of the initial value by using the first light source intensity adjustment coefficient; if the component quantity ratio F is greater than the first preset component quantity ratio F1 and less than or equal to the second preset component quantity ratio F2, the light source intensity is increased to 2.65 times of the initial value by using the second light source intensity adjustment coefficient; if the component quantity ratio F is greater than the second preset component quantity ratio F2, the light source intensity is increased to 1.85 times of the initial value by using the third light source intensity adjustment coefficient. The increase ratio of the light source intensity can be adjusted accordingly to reduce signal interference and enhance the detection sensitivity of the detector.

[0090] See also Figure 5As shown, it is a logic flow chart of re-determining the reason why the chromatographic detection process does not meet the standard based on the component variance and the corresponding processing method in this embodiment. The process of calculating the component variance according to the difference of several component proportions and re-determining the reason why it does not meet the standard based on the component variance includes:

[0091] Based on the comparison result of the component variance and the preset component variance, the irradiation wavelength of the detector is determined, the conveying speed of the sample solution to be tested into the chromatographic column is adjusted, or the preparation sample is remade.

[0092] Specifically, in this embodiment, the difference values ​​of each component proportion are counted, and the component variance is obtained by calculation according to the difference values ​​of several component proportions. The preset component variance E0 can be divided into a first preset component variance E1 and a second preset component variance E2. The preset component variance standard E3=0.45, E1=0.95×E3, and E2=1.45×E3 are set. It should be noted that E1, E2, and E3 can all be set to other values. The comparison process based on the component variance E with E1 and E2 is as follows:

[0093] If the component variance E is less than or equal to the first preset component variance E1, it means that the current E is relatively small, indicating that the numerical values ​​of the differences in the proportions of the components are relatively close and the difference is not large. Therefore, it can be determined that the reason why the chromatographic detection process does not meet the standards is that the detection sensitivity of the detector is insufficient, and it is necessary to reduce the proportion average difference H by increasing the irradiation wavelength of the detector.

[0094] If the component variance E is greater than the first preset component variance E1 and less than or equal to the second preset component variance E2, it can be determined that the reason why the chromatographic detection process does not meet the standards is that there is a problem with the filtration operation in the pretreatment, resulting in a large amount of impurities remaining in the sample solution to be tested. It is necessary to reduce the transport speed of the sample solution to be tested entering the chromatographic column to improve the filtration efficiency of the solution.

[0095] If the component variance E is greater than the second preset component variance E2, it means that the current E is relatively large, indicating that the numerical values ​​of the differences in the proportions of each component are relatively dispersed and vary greatly. Therefore, it can be determined that the reason why the chromatographic detection process does not meet the standards is that there is a problem with the preparation sample, resulting in the detected proportions of each component being inconsistent with the proportions of each component in the control unit, and the preparation sample needs to be re-prepared.

[0096] Further, the process of adjusting the delivery speed of the sample solution to be tested into the chromatographic column includes:

[0097] Based on the comparison result of the component variance difference and the preset component variance difference, it is determined to reduce the conveying speed, and the reduction amplitude of the conveying speed is proportional to the component variance difference; wherein, the difference between the component variance and the preset component variance is calculated and recorded as the component variance difference.

[0098] Specifically, in this embodiment, the component variance difference M is obtained by calculating the component variance E and the first preset component variance E1, M=E-E1, the preset component variance difference M0 can be divided into the first preset component variance difference M1 and the second preset component variance difference M2, and the preset component variance difference standard M3=0.1, M1=0.85×M3, M2=1.25×M3 is set. It should be noted that the assignment of M3 is related to E, E1, E2 and E3, and the value of M shall not exceed the difference between E2 and E; the comparison process based on the component variance difference M with M1 and M2 is as follows:

[0099] If the component variance difference M is less than or equal to the first preset component variance difference M1, the conveying speed is reduced to 0.9 times of the initial value by using the first speed adjustment coefficient; if the component variance difference M is greater than the first preset component variance difference M1 and less than or equal to the second preset component variance difference M2, the conveying speed is reduced to 0.7 times of the initial value by using the second speed adjustment coefficient; if the component variance difference M is greater than the second preset component variance difference M2, the conveying speed is reduced to 0.5 times of the initial value by using the third speed adjustment coefficient. The reduction ratio of the conveying speed can also be set to other values, and the filtration efficiency can be improved by reducing the conveying speed, so as to ensure that the data obtained during the subsequent chromatographic analysis is more accurate; in this embodiment, the sample solution to be tested is automatically injected into the chromatographic column using a mechanical device, and the conveying speed is set in advance when the mechanical device is used, so the speed of injecting the sample solution to be tested into the chromatographic column can be adjusted by modifying the speed adjustment coefficient.

[0100] Furthermore, when the conveying speed is reduced, the replacement period of the filter device in the pretreatment is extended based on the comparison result of the speed reduction amount with the preset speed reduction amount, and the extension of the replacement period is proportional to the speed reduction amount.

[0101] Specifically, in this embodiment, the speed reduction is the difference between the initial value of the conveying speed and the speed obtained after adjustment. The conveying speed is reduced, and the loss of the filter device is also reduced accordingly; the preset speed reduction V0 can be divided into a first preset speed reduction V1 and a second preset speed reduction V2, and the preset speed reduction standard V3=0.3 ml / min, V1=0.5×V3, V2=1.1×V3 is set. It should be noted that the value of V3 is related to the type and inner diameter of the chromatographic column, the pore size of the chromatographic column filling material, the liquid phase viscosity, etc., and the value of V3 can be adjusted according to the actual situation of the above parameters. The same is true for V1 and V2. The comparison process based on the speed reduction V and V1 and V2 is as follows:

[0102] If the speed reduction amount V is less than or equal to the first preset speed reduction amount V1, it is determined that the replacement cycle of the filter device is extended by one month on the original basis; if the speed reduction amount V is greater than the first preset speed reduction amount V1 and less than or equal to the second preset speed reduction amount V2, it is determined that the replacement cycle of the filter device is extended by two months on the original basis; if the speed reduction amount V is greater than the second preset speed reduction amount V2, it is determined that the replacement cycle of the filter device is extended by three months on the original basis. It should be noted that the extension period can be set according to actual needs without specific limitation; by extending the replacement period, the equipment use cost required for chromatographic detection can be saved, and a balance between the conveying speed and the replacement period of the filter device can be achieved.

[0103] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0104] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A chromatographic detection method for a compound Eucommia ulmoides leaf preparation, characterized in that: include: Preparing a preparation sample according to the proportion of each component in the prescription, and pre-treating the preparation sample to obtain a sample solution to be tested; Placing the sample solution to be tested into a chromatographic column, and performing chromatographic separation on the sample solution to be tested to obtain separated components; placing the separated components into a detector, and performing chromatographic analysis on the separated components to obtain a chromatogram; Analyzing the chromatogram to obtain the ratios of several components in the preparation sample, and sequentially comparing the ratios of several components with the ratios of several components in the comparison table to determine the difference in the ratios of the components; Determining whether the chromatographic detection process meets the standard based on the comparison results of the difference values ​​of the component ratios and the corresponding preset values, and generating corresponding instructions when it does not meet the standard; The length of the chromatographic column, the illumination wavelength of the detector, or the transport speed of the sample solution entering the chromatographic column is determined based on the instruction.

2. A chromatographic detection method for a compound Eucommia ulmoides leaf preparation according to claim 1, characterized in that: The process of determining whether the chromatographic detection process meets the standard based on the comparison results of the difference values ​​of the component ratios and the corresponding preset values ​​includes: Calculate the average of the differences in the proportions of the components and record it as the average difference in proportions; Based on the comparison result of the mean difference of the ratio with the preset mean difference of the ratio, or based on the number of components in the preparation sample, determining whether the chromatographic detection process meets the standard; When it is determined that the chromatographic detection process does not meet the standard, the reason why the chromatographic detection process does not meet the standard is determined according to the difference between the proportional average difference and the preset proportional average difference.

3. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 2, characterized in that: The process of determining whether the chromatographic testing process meets the standards based on the number of components in the preparation sample includes: Counting the amount of the components in the preparation sample; Whether to increase the length of the chromatographic column is determined based on a comparison result of the component quantity with a preset component quantity.

4. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 3, characterized in that: The process of determining whether to increase the length of the chromatographic column based on the comparison result of the number of components and the preset number of components comprises: Calculating the difference between the number of components and the preset number of components, and recording the difference as the difference in the number of components; Based on the comparison result of the component quantity difference and the preset component quantity difference, it is determined that the length of the chromatographic column is increased, and the increase in the length is proportional to the component quantity difference.

5. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 2, characterized in that: The process of determining the reason why the chromatographic detection process does not meet the standard according to the difference between the ratio average difference and the preset ratio average difference comprises: Calculate the difference between the proportional mean difference and the preset proportional mean difference, and record it as the second-order proportional mean difference; Determining the reason why the chromatographic detection process does not meet the standard based on the comparison result of the second-order ratio average difference and the preset second-order ratio average difference; Determining corresponding treatment based on the cause includes: determining the irradiation wavelength of the detector, the transport speed of the sample solution to be tested into the chromatographic column, or calculating the component variance based on the difference in several component proportions and re-determining the cause of non-compliance with the standard based on the component variance.

6. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 5, characterized in that: The process of determining the illumination wavelength of the detector includes: Based on the comparison result of the light reflectance average value and the preset light reflectance average value, it is determined that the irradiation wavelength is increased, and the increase amplitude of the irradiation wavelength is inversely proportional to the light reflectance average value; When the detector illuminates the separated components, it obtains the light reflectance corresponding to each component, calculates the average value of several light reflectances, and records it as the light reflectance average value.

7. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 6, characterized in that: When the irradiation wavelength adjustment is completed, based on the comparison result of the component quantity ratio and the preset component quantity ratio, it is determined that the light source intensity of the detector is increased, and the increase range of the light source intensity is inversely proportional to the component quantity ratio; The ratio between the preset component quantity and the component quantity is calculated and recorded as the component quantity ratio.

8. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 5, characterized in that: The process of calculating the component variance according to the difference in the component proportions and re-determining the reasons for non-compliance with the standard based on the component variance includes: Based on the comparison result of the component variance and the preset component variance, the irradiation wavelength of the detector is determined, the conveying speed of the sample solution to be tested into the chromatographic column is adjusted, or the preparation sample is remade.

9. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 8, characterized in that: The process of determining the transport speed of the sample solution to be tested into the chromatographic column comprises: Determining to reduce the conveying speed based on a comparison result of the component variance difference and a preset component variance difference, and the reduction range of the conveying speed is proportional to the component variance difference; The difference between the component variance and the preset component variance is calculated and recorded as the component variance difference.

10. The chromatographic detection method for the compound Eucommia ulmoides leaf preparation according to claim 9, characterized in that: When the conveying speed is reduced, the replacement period of the filter device in the pretreatment is extended based on the comparison result of the speed reduction amount and the preset speed reduction amount, and the extension of the replacement period is proportional to the speed reduction amount.

Images