Method for detecting volatile components of liver-protecting traditional Chinese medicine preparation by using chromatography-mass spectrometry
By analyzing the distortion and correcting the errors in the chromatographic data curves of hepatoprotective traditional Chinese medicine preparations, the problem of inaccurate detection results of volatile components of traditional Chinese medicine was solved, and highly reliable detection results were achieved, ensuring the clinical efficacy of traditional Chinese medicine preparations.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHINA JAPAN FRIENDSHIP HOSPITAL
- Filing Date
- 2026-04-09
- Publication Date
- 2026-05-12
AI Technical Summary
Existing technologies have low accuracy in detecting volatile components of hepatoprotective traditional Chinese medicine preparations. This is mainly because the volatile components of traditional Chinese medicine are complex, some compounds have similar structures and are difficult to separate completely under conventional chromatographic conditions, and low-content components are easily masked by the signals of high-abundance components.
By collecting chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations, the target peaks were identified, the shape characteristics and intersections of adjacent peaks were analyzed, the degree of distortion was evaluated, the error degree value was used to correct the chromatographic data curves, and the matching degree was compared with a standard chromatographic database to ensure the accuracy of the detection results.
This improves the accuracy of detecting volatile components in hepatoprotective traditional Chinese medicine preparations, ensuring the stability and safety of clinical efficacy, and enabling accurate detection of the material composition of traditional Chinese medicine preparations.
Smart Images
Figure CN122017107A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chromatographic analysis technology, specifically to a method for detecting volatile components in hepatoprotective traditional Chinese medicine preparations using chromatographic-mass spectrometry. Background Technology
[0002] Traditional Chinese medicine (TCM) preparations for liver protection have a long history and significant clinical efficacy in the prevention and treatment of liver injury and the regulation of liver function. Research on their pharmacodynamic material basis is a key aspect of the modernization of TCM. Volatile components (such as terpenes and aromatic compounds) are important active components of hepatoprotective TCM, often exhibiting anti-inflammatory, antioxidant, and metabolic-promoting biological activities. However, their chemical composition is complex, their content is low, and they are easily volatile, making comprehensive identification and accurate quantification difficult using traditional analytical methods. Gas chromatography-mass spectrometry (GC-MS) combines the high separation efficiency of gas chromatography with the high sensitivity and selectivity of mass spectrometry, and has become the standard for the analysis of volatile components.
[0003] When detecting volatile components of hepatoprotective traditional Chinese medicine preparations using gas chromatography-mass spectrometry (GC-MS), the volatile components of traditional Chinese medicine are complex (such as terpenes, aldehydes, ketones, aromatic compounds, etc.), and some compounds have similar structures (such as isomers), making complete separation difficult under conventional chromatographic conditions. This results in co-elution peaks affecting the accuracy of qualitative and quantitative analysis. Furthermore, low-content components (such as trace active substances) are easily masked by high-abundance component signals due to their low ionization efficiency, thus leading to lower accuracy in the detection results of volatile components in hepatoprotective traditional Chinese medicine preparations. Summary of the Invention
[0004] To address the issue of low accuracy in existing methods for detecting volatile components in hepatoprotective traditional Chinese medicine preparations, this invention aims to provide a chromatography-mass spectrometry (LC-MS) method for detecting volatile components in hepatoprotective traditional Chinese medicine preparations. The specific technical solution adopted is as follows: This invention provides a method for detecting volatile components in hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry (PCMS), the method comprising the following steps: Chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations were collected; Based on the data distribution of the chromatographic data curves corresponding to each concentration, the chromatographic data curves are divided into multiple target peaks; the degree of distortion of the target peaks is obtained according to the shape characteristics of adjacent target peaks and the coordinates of their intersections. Based on the degree of distortion and the magnitude of the target peak in the chromatographic data curve corresponding to each concentration, the offset value of the chromatographic data curve corresponding to each concentration is determined; by combining the offset values of the chromatographic data curves corresponding to all concentrations, the error value of the chromatographic data is obtained. The chromatographic data curves corresponding to each concentration are corrected using the error level value, and the volatile components of the liver-protecting traditional Chinese medicine preparation are detected based on the correction results.
[0005] Preferably, the step of dividing the chromatographic data curve into multiple target peaks based on the data distribution of the chromatographic data curves corresponding to each concentration includes: For any concentration: Obtain the maximum and minimum values on the chromatographic data curve corresponding to any given concentration; On the chromatographic data curve, the curve segment between two adjacent minimum values is taken as a target spectral peak.
[0006] Preferably, obtaining the distortion degree of the target spectral peak based on the shape characteristics of adjacent target spectral peaks and the coordinates of their intersection includes: For any concentration: The degree of interference of each target peak is evaluated based on the difference between the vertical axis and the horizontal axis of the maximum point of each target peak and its adjacent next target peak on the chromatographic data curve corresponding to any concentration. The distortion degree of each target spectral peak is obtained based on the difference in the interference level of two adjacent target spectral peaks, the difference in the state value of two adjacent target spectral peaks, and the ordinate of the intersection point of two adjacent target spectral peaks. The state value is determined based on the peak width of the target spectral peak and the data value of the maximum point of the target spectral peak.
[0007] Preferably, the evaluation of the interference degree of each target peak based on the difference between the ordinate and the abscissa of the maximum point of each target peak on the chromatographic data curve corresponding to any concentration and the next adjacent target peak includes: Calculate the first normalized value of the difference between the ordinate of each target spectral peak and the maximum point of its next adjacent target spectral peak, and the second normalized value of the difference between the abscissa of each target spectral peak and the maximum point of its next adjacent target spectral peak. The product of the first normalized value and the second normalized value is taken as the degree of interference of each target spectral peak.
[0008] Preferably, the step of obtaining the distortion degree of each target spectral peak based on the difference in interference levels between two adjacent target spectral peaks, the difference in state values between two adjacent target spectral peaks, and the ordinate of the intersection point of two adjacent target spectral peaks includes: The ratio between the interference level of each target spectral peak and its adjacent next target spectral peak is denoted as the first ratio. The ratio between the state value of each target spectral peak and its adjacent next target spectral peak is denoted as the second ratio. Based on the first ratio, the second ratio, and the ordinate of the intersection point of each target spectral peak and its next adjacent target spectral peak, the distortion degree of each target spectral peak is obtained. The first ratio, the second ratio, and the ordinate of the intersection point are all positively correlated with the distortion degree.
[0009] Preferably, determining the offset value of the chromatographic data curve corresponding to each concentration based on the distortion degree and data value of the target peak in the chromatographic data curve corresponding to each concentration includes: For any concentration: Based on the distortion degree of the target peak and the data value of the maximum point of the target peak in the chromatographic data curve corresponding to any concentration, the offset value of the chromatographic data curve corresponding to any concentration is obtained, and the distortion degree and the data value of the maximum point are both positively correlated with the offset value.
[0010] Preferably, the step of obtaining the error value of the chromatographic data by combining the offset values of the chromatographic data curves corresponding to all concentrations includes: The error value of the chromatographic data is obtained based on the offset value of the chromatographic data curves corresponding to all concentrations and the corresponding concentrations; both the offset value and the concentration are positively correlated with the error value.
[0011] Preferably, obtaining the error value of the chromatographic data based on the offset values of the chromatographic data curves corresponding to all concentrations and the corresponding concentrations includes: The product of the normalized value of the offset of the chromatographic data curve corresponding to each concentration and the normalized value of the corresponding concentration is recorded as the first product corresponding to each concentration. The normalized result of the average of the first product corresponding to all concentrations is used as the error value of the chromatographic data.
[0012] Preferably, the step of correcting the chromatographic data curves corresponding to each concentration using the error level value includes: Calculate the first difference between the constant 1 and the normalized error value; The product of the first difference and the data value on the chromatographic data curve corresponding to each concentration is used as the correction result of the chromatographic data curve.
[0013] Preferably, the volatile components of the hepatoprotective traditional Chinese medicine preparation are detected based on the correction results, including: The corrected chromatographic data curves were compared with the chromatographic data curves in the standard chromatographic database, and compounds with a matching degree greater than the preset matching degree were selected as candidate identification results.
[0014] The present invention has at least the following beneficial effects: This invention first collected chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations. Considering the complexity of volatile components in traditional Chinese medicine and the similarity of some compound structures, complete separation under conventional chromatographic conditions is difficult, leading to co-elution peaks affecting the accuracy of qualitative and quantitative analysis. Furthermore, low-content components are easily masked by high-abundance component signals due to low ionization efficiency. This invention analyzes the data distribution of chromatographic data curves corresponding to each concentration, extracting multiple target peaks from the chromatographic data curves. Then, based on the shape characteristics of adjacent target peaks and the distribution of intersection points, the distortion degree of the target peaks is evaluated. Next, based on the distortion degree and data value of the target peaks, the offset degree of the chromatographic data curve is quantified. Subsequently, the chromatographic data curve is corrected using the error degree value, providing highly reliable data for the subsequent detection of volatile components in hepatoprotective traditional Chinese medicine preparations. This results in higher accuracy of the subsequent detection results of volatile components in hepatoprotective traditional Chinese medicine preparations. The method provided by this invention can accurately detect the material composition of hepatoprotective traditional Chinese medicine preparations, ensuring the stability and safety of clinical efficacy. Attached Figure Description
[0015] To more clearly illustrate the technical solutions and advantages in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0016] Figure 1 This is a flowchart of a method for detecting volatile components in a hepatoprotective traditional Chinese medicine preparation using phase chromatography-mass spectrometry, provided as an embodiment of the present invention. Detailed Implementation
[0017] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the following detailed description, in conjunction with the accompanying drawings and preferred embodiments, describes a method for anomaly detection of multivariate time series data based on a multi-head graph attention network proposed in accordance with the present invention.
[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.
[0019] The following describes in detail, with reference to the accompanying drawings, a specific scheme for the detection of volatile components in a hepatoprotective traditional Chinese medicine preparation using phase chromatography-mass spectrometry provided by the present invention.
[0020] Example of a method for detecting volatile components in hepatoprotective traditional Chinese medicine preparations using chromatography-mass spectrometry: This embodiment proposes a method for detecting volatile components in hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry (PCMS), such as... Figure 1 As shown, the method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry in this embodiment includes the following steps: Step S1: Collect chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations.
[0021] The main objective of this embodiment is to detect the volatile components of hepatoprotective traditional Chinese medicine preparations using gas chromatography-mass spectrometry (GC-MS). Therefore, it is first necessary to collect chromatographic data of hepatoprotective traditional Chinese medicine preparations at different concentrations. In this embodiment, chromatographic data curves of three different concentrations of hepatoprotective traditional Chinese medicine preparations were collected. The specific process includes: First, the samples of hepatoprotective traditional Chinese medicine preparations undergo pretreatment. Specifically, solvent extraction is used, suitable for lipid-soluble or moderately polar volatile components (such as terpenes and phenylpropanoids). The herbal powder (approximately 1g) is soaked in an organic solvent (such as n-hexane, dichloromethane, or ether) or extracted by ultrasonication (30 min). After centrifugation (4000 rpm) for 10 min, the supernatant is collected and filtered through a 0.22μm organic filter membrane. The solution is then concentrated (by nitrogen blowing or rotary evaporation) to 100–200 μL for GC-MS injection. It should be noted that high-temperature concentration should be avoided to prevent component loss.
[0022] Then, headspace-solid phase microextraction is performed. This method is suitable for trace volatile components (to avoid solvent interference). Specifically, the sample (0.5g) of the hepatoprotective traditional Chinese medicine preparation is added to the headspace vial along with saturated saline (1:1). SPME fibers (recommended coating: PDMS / DVB / CAR or DVB / CAR / PDMS) are inserted. The sample is heated (60–80℃) for adsorption for 30–60 min, and then directly inserted into the GC inlet for desorption (250℃, 5 min).
[0023] Set the gas chromatography parameters as follows: Column: non-polar column (e.g., DB-5ms, 30m × 0.25mm × 0.25μm) or polar column (e.g., HP-INNOWax); Carrier gas: high-purity helium (1.0 mL / min constant flow mode); Temperature program: initial 50℃, hold for 2 min, then increase to 250℃ at 5–10℃ / min, and finally hold at 300℃ for 5 min; Injector temperature: 250℃ (split / splitless mode, split ratio 10:1). Set the mass spectrometry parameters as follows: Ion source: electron impact (EI, 70eV); Ion source temperature: 230℃; Scan mode: full scan (Scan, m / z 40–600) or selected ion monitoring (SIM, for target compound); Transfer line temperature: 280℃.
[0024] Next, chromatographic data acquisition was performed, with an injection volume of 1 μL liquid or headspace adsorption / desorption. A 2-minute solvent delay was used to avoid solvent peak interference. Each sample was repeated at least three times to improve reproducibility. Chromatographic data curves were obtained for each concentration of the hepatoprotective traditional Chinese medicine preparation. The x-axis of the chromatographic data curve represents retention time, and the y-axis represents retention volume. In specific applications, the implementer sets different concentrations according to the specific circumstances.
[0025] It should be noted that glass containers should be used during data collection to avoid the release of interfering substances from plastic.
[0026] Thus, this embodiment has obtained chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at various concentrations.
[0027] Step S2: Based on the data distribution of the chromatographic data curves corresponding to each concentration, the chromatographic data curves are divided into multiple target peaks; the distortion degree of the target peaks is obtained according to the shape characteristics of adjacent target peaks and the coordinates of their intersections.
[0028] Volatile components (such as terpenes and aromatic compounds) are the key pharmacodynamic basis of hepatoprotective traditional Chinese medicines, playing an important role in liver damage repair through their antioxidant, anti-inflammatory, and hepatocyte regeneration-promoting activities. However, these components are chemically unstable, present in low concentrations, and easily affected by extraction processes, making comprehensive identification and accurate quantification difficult using traditional analytical methods. Systematic detection of volatile components using gas chromatography-mass spectrometry (GC-MS) can not only elucidate the material composition of formulations and screen potential quality markers, but also provide a scientific basis for optimizing production processes and establishing quality control standards, thereby ensuring the stability and safety of clinical efficacy.
[0029] GC-MS offers significant advantages for the systematic detection of volatile components. First, it combines the high separation efficiency of gas chromatography with the high sensitivity and selectivity of mass spectrometry, enabling precise separation and identification of volatile components in complex matrices. This is particularly suitable for low-content, structurally similar compounds (such as terpenes, aldehydes, and ketones isomers) found in traditional Chinese medicine. Second, GC-MS allows for broad-spectrum screening and targeted quantification through full-scan mode and selected ion monitoring (SIM). Combined with chromatographic databases and retention index comparisons, it significantly improves the accuracy of component identification. Furthermore, this method offers flexible sample pretreatment options (such as headspace microextraction and solid-phase microextraction), reducing solvent interference and preserving information on thermally unstable components. However, because the volatile components of traditional Chinese medicine are complex (such as terpenes, aldehydes, ketones, aromatic compounds, etc.), and some compounds have similar structures (such as isomers), they are difficult to separate completely under conventional chromatographic conditions, which leads to co-elution peaks affecting the accuracy of qualitative and quantitative analysis. Furthermore, low-content components (such as trace active substances) are easily masked by the signals of high-abundance components due to their low ionization efficiency, resulting in missed detection.
[0030] Therefore, in order to solve the above problems, this embodiment analyzes the chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations to obtain the relationship between concentration and chromatographic peak changes, thereby accurately detecting the volatile concentration of hepatoprotective traditional Chinese medicine preparations.
[0031] The following explanation uses one concentration as an example; other concentrations can be processed using the method provided in this embodiment.
[0032] Specifically, for any concentration: Obtain the maximum and minimum points on the chromatographic data curve corresponding to this concentration.
[0033] On the chromatographic data curve, the curve segment between two adjacent minimum points is taken as a target spectral peak. That is, in order of increasing x-axis, the curve segment between the first minimum point and the second minimum point is taken as a target spectral peak, the curve segment between the third minimum point and the fourth minimum point is taken as a target spectral peak, the curve segment between the fifth minimum point and the sixth minimum point is taken as a target spectral peak, and so on, to obtain multiple target spectral peaks.
[0034] Because compounds with similar compositions can interfere with each other when measured by chromatography, and the higher the concentration of one substance, the more it will affect the peaks of another substance with similar composition; therefore, the degree of interference of the target peaks is first determined based on the positional relationship between the target peaks.
[0035] Specifically, firstly, the absolute value of the difference between the ordinate of each target spectral peak and the ordinate of the next adjacent target spectral peak's maximum point is calculated. This absolute value represents the difference between the data values of the two maximum points. This absolute value is then normalized, and the normalized result is recorded as the first normalized value. Next, the absolute value of the difference between the abscissa of each target spectral peak and the ordinate of the next adjacent target spectral peak's maximum point is calculated. This absolute value represents the distance between the abscissas of the two maximum points. This absolute value is then normalized, and the normalized result is recorded as the second normalized value. There are many data normalization methods; in this embodiment, linear normalization is used to normalize the data, ensuring that both the first and second normalized values fall within the range of (0, 1). Alternatively, other existing data normalization methods can also be used. It should be noted that if the normalized data may have a value of 0, a zero-prevention parameter needs to be added in the subsequent calculation of the state value to prevent the denominator of the formula from being 0 when calculating the degree of distortion. The zero-prevention parameter should be small enough to reduce the impact on the calculation result, for example, it can be 0.0001.
[0036] The product of each first normalized value and its corresponding second normalized value is used as the interference level of each target spectral peak. The closer two target spectral peaks are, the more similar their components are, and the greater the degree of mutual interference in the spectrum. Furthermore, the greater the peak difference between adjacent target spectral peaks, the greater the degree of interference. Therefore, this embodiment uses the peak height difference between two adjacent target spectral peaks and the distance between their horizontal axes to represent the interference level of the target spectral peaks.
[0037] Based on the interference level of the target spectral peak obtained from the above calculation, different spectral peaks are then analyzed to obtain the differences in the interference level of each spectral peak in the same agent. Different components have different chemical compositions, and their sensitivity to the spectrum and light absorption capacity are different. Therefore, in the same agent, the interference level of the target spectral peak at different positions is different. Therefore, the degree of shift of the current agent spectral peak is evaluated based on the differences between the target spectral peaks.
[0038] Specifically, firstly, the product of the normalized result of the data value of the maximum point of each target spectral peak and the normalized value of the peak width of each target spectral peak is used as the state value of each target spectral peak. The peak width of the target spectral peak is obtained by taking the difference between the x-coordinate of the last point and the x-coordinate of the first point of the target spectral peak as the peak width. In this embodiment, linear normalization is used to normalize the data. Then, the ratio between the interference degree of each target spectral peak and its next adjacent target spectral peak is recorded as the first ratio; the ratio between the state value of each target spectral peak and its next adjacent target spectral peak is recorded as the second ratio. Next, based on the first ratio, the second ratio, and the ordinate of the intersection point of each target spectral peak and its next adjacent target spectral peak, the distortion degree of each target spectral peak is obtained. The first ratio, the second ratio, and the ordinate of the intersection point are all positively correlated with the distortion degree.
[0039] Among them, a positive correlation means that the dependent variable increases as the independent variable increases, and the dependent variable decreases as the independent variable decreases. It can be an additive relationship, a multiplicative relationship, etc., which is determined by the actual application.
[0040] As a concrete example, the specific formula for calculating the degree of distortion is given, the first... The degree of distortion of each target spectral peak can be expressed as: in, Indicates the first The degree of distortion of each target spectral peak, Indicates the first The degree of interference of each target spectral peak Indicates the first The degree of interference of each target spectral peak Indicates the first The target spectral peak and the first The ordinate of the intersection point of the target spectral peaks Indicates the first The data values of the maximum points of each target spectral peak, i.e., the ordinate; Indicates the first The peak width of each target spectral peak Indicates the first The data values of the maximum points of each target spectral peak. Indicates the first The peak width of each target spectral peak Represents the normalization function. This represents the hyperbolic tangent function.
[0041] This represents the first ratio; a ratio greater than 1 indicates that the first ratio... The interference experienced by the first target spectral peak is greater than that of the second. The greater the interference to a target spectral peak, the greater the distortion of its spectral peak. The height of the intersection point of two target spectral peaks indicates the degree of overlap of the spectral peaks. The higher the degree of overlap of the target spectral peaks, the greater the interference to the weaker target spectral peak, and therefore the greater the distortion. Indicates the first The state values of each target spectral peak. Indicates the first The state values of each target spectral peak. This ratio is used to describe the difference between two target spectral peaks. The larger the ratio, the greater the interference to the current spectral peak, and the greater the degree of distortion.
[0042] Using the above method, the degree of distortion of the target peak in the chromatographic data curve corresponding to each concentration can be obtained.
[0043] Step S3: Based on the distortion degree and data value of the target peak in the chromatographic data curve corresponding to each concentration, determine the offset value of the chromatographic data curve corresponding to each concentration; combine the offset values of the chromatographic data curves corresponding to all concentrations to obtain the error value of the chromatographic data.
[0044] The content of substances in traditional Chinese medicine preparations varies at different concentrations. When different substance contents are measured, the degree of expression of the spectral peaks is different. Therefore, the degree of influence between target spectral peaks is also different. Thus, the influence of substances with the same composition on the chromatographic data can be obtained by measuring the differences in spectral peaks at different concentrations. This allows for the correction of the target spectral peaks and the acquisition of accurate spectral peaks, thereby enabling the detection of volatile components in liver-protecting traditional Chinese medicine preparations.
[0045] The following example will be used to illustrate the concept of a single concentration.
[0046] For any concentration: Based on the degree of distortion of the target peak and the data value of the maximum point of the target peak in the chromatographic data curve corresponding to the concentration, the offset value of the chromatographic data curve corresponding to the concentration is obtained. The degree of distortion and the data value of the maximum point are both positively correlated with the offset value.
[0047] In this embodiment, a specific formula for calculating the offset value is given. The offset value of the chromatographic data curve corresponding to this concentration can be expressed as: in, This indicates the degree of deviation of the chromatographic data curve corresponding to this concentration. This indicates the number of target peaks on the chromatographic data curve corresponding to that concentration. This indicates the number of chromatographic data curves corresponding to that concentration. The data values of the maximum points of each target spectral peak. This indicates the number of chromatographic data curves corresponding to that concentration. The degree of distortion of each target spectral peak, This represents the normalization function.
[0048] Indicates the first The higher the height of the target spectral peak and the greater the degree of distortion, the greater the degree of distortion in the current data.
[0049] Using the above method, the offset value of the chromatographic data curve corresponding to each concentration can be obtained.
[0050] Next, the error level of the chromatographic data is evaluated based on the offset values of the chromatographic data curves corresponding to all concentrations and the corresponding concentrations; both the offset values and the concentrations are positively correlated with the error level.
[0051] Specifically, the deviation values of the chromatographic data curves corresponding to each concentration are normalized, and the values of each concentration are also normalized. The product of the normalized deviation value of the chromatographic data curve corresponding to each concentration and the normalized value of the corresponding concentration is recorded as the first product for each concentration. The normalized result of the average of the first products corresponding to all concentrations is taken as the error value of the chromatographic data. The higher the concentration and the greater the distortion, the larger the error value.
[0052] Thus, this embodiment has obtained the error level value of the chromatographic data.
[0053] Step S4: Correct the chromatographic data curves corresponding to each concentration using the error level value, and detect the volatile components of the liver-protecting traditional Chinese medicine preparation based on the correction results.
[0054] In this embodiment, the error level value of the chromatographic data is obtained in step S3, and the chromatographic data curve will be corrected based on the error level value.
[0055] Specifically, the error values of the chromatographic data are normalized, and the normalized error values are (0, 1). The difference between the constant 1 and the normalized error values is recorded as the first difference. The product of the first difference and the data values on the chromatographic data curves corresponding to each concentration is used as the corrected data values for the corresponding data points on the chromatographic data curves, thus obtaining the corrected results of the chromatographic data curves.
[0056] After correcting the chromatographic data curves, the corrected chromatographic data curves are first compared with the chromatographic data curves in the standard chromatographic database. Compounds with a matching degree greater than the preset matching degree are usually selected as candidate identification results. The calculation method of the matching degree between curves is existing technology and will not be described in detail in this embodiment. The preset matching degree is set by the implementer according to the specific situation and will not be described in detail here.
[0057] Simultaneously, retention indices are used for auxiliary verification to improve identification accuracy. For important components, further confirmation through standard comparison experiments is also required. This multi-parameter comparison method can reliably identify the chemical structures of various volatile components such as monoterpenes, sesquiterpenes, and aromatic compounds in traditional Chinese medicine preparations, providing a scientific basis for elucidating the pharmacodynamic material basis of traditional Chinese medicine preparations.
[0058] Thus, the method provided in this embodiment has been used to complete the detection of volatile components in hepatoprotective traditional Chinese medicine preparations.
[0059] This embodiment first collected chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations. Considering the complexity of volatile components in traditional Chinese medicine and the similarity of some compound structures, complete separation under conventional chromatographic conditions is difficult, leading to co-elution peaks affecting the accuracy of qualitative and quantitative analysis. Furthermore, low-content components are easily masked by high-abundance component signals due to low ionization efficiency. This embodiment analyzed the data distribution of chromatographic data curves corresponding to each concentration, extracted multiple target peaks from the chromatographic data curves, and then evaluated the distortion degree of the target peaks based on the shape characteristics and intersection distribution of adjacent target peaks. Next, the offset degree of the chromatographic data curves was quantified based on the distortion degree and data value of the target peaks, and then the chromatographic data curves were corrected using the error degree value. This provides highly reliable data for the subsequent detection of volatile components in hepatoprotective traditional Chinese medicine preparations, making the detection results of volatile components in hepatoprotective traditional Chinese medicine preparations more accurate. The method provided in this embodiment can accurately detect the material composition of hepatoprotective traditional Chinese medicine preparations, ensuring the stability and safety of clinical efficacy.
[0060] It should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for detecting volatile components in a hepatoprotective traditional Chinese medicine preparation using phase chromatography-mass spectrometry, characterized in that, The method includes the following steps: Chromatographic data curves of hepatoprotective traditional Chinese medicine preparations at different concentrations were collected; Based on the data distribution of the chromatographic data curves corresponding to each concentration, the chromatographic data curves are divided into multiple target peaks; the degree of distortion of the target peaks is obtained according to the shape characteristics of adjacent target peaks and the coordinates of their intersections. Based on the degree of distortion and the magnitude of the target peak in the chromatographic data curve corresponding to each concentration, the offset value of the chromatographic data curve corresponding to each concentration is determined; by combining the offset values of the chromatographic data curves corresponding to all concentrations, the error value of the chromatographic data is obtained. The chromatographic data curves corresponding to each concentration are corrected using the error level value, and the volatile components of the liver-protecting traditional Chinese medicine preparation are detected based on the correction results.
2. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, Based on the data distribution of the chromatographic data curves corresponding to each concentration, the chromatographic data curves are divided into multiple target peaks, including: For any concentration: Obtain the maximum and minimum values on the chromatographic data curve corresponding to any given concentration; On the chromatographic data curve, the curve segment between two adjacent minimum values is taken as a target spectral peak.
3. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, The step of obtaining the distortion degree of the target spectral peak based on the shape characteristics of adjacent target spectral peaks and the coordinates of their intersection points includes: For any concentration: The degree of interference of each target peak is evaluated based on the difference between the vertical axis and the horizontal axis of the maximum point of each target peak and its adjacent next target peak on the chromatographic data curve corresponding to any concentration. The distortion degree of each target spectral peak is obtained based on the difference in the interference level of two adjacent target spectral peaks, the difference in the state value of two adjacent target spectral peaks, and the ordinate of the intersection point of two adjacent target spectral peaks. The state value is determined based on the peak width of the target spectral peak and the data value of the maximum point of the target spectral peak.
4. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 3, characterized in that, The evaluation of the interference degree of each target peak based on the differences in the ordinate and the abscissa of the maximum point of each target peak on the chromatographic data curve corresponding to any concentration and the next adjacent target peak includes: Calculate the first normalized value of the difference between the ordinate of each target spectral peak and the maximum point of its next adjacent target spectral peak, and the second normalized value of the difference between the abscissa of each target spectral peak and the maximum point of its next adjacent target spectral peak. The product of the first normalized value and the second normalized value is taken as the degree of interference of each target spectral peak.
5. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 3, characterized in that, The distortion degree of each target spectral peak is obtained based on the difference in interference levels between two adjacent target spectral peaks, the difference in state values between two adjacent target spectral peaks, and the ordinate of the intersection point of two adjacent target spectral peaks, including: The ratio between the interference level of each target spectral peak and its adjacent next target spectral peak is denoted as the first ratio. The ratio between the state value of each target spectral peak and its adjacent next target spectral peak is denoted as the second ratio. Based on the first ratio, the second ratio, and the ordinate of the intersection point of each target spectral peak and its next adjacent target spectral peak, the distortion degree of each target spectral peak is obtained. The first ratio, the second ratio, and the ordinate of the intersection point are all positively correlated with the distortion degree.
6. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, The step of determining the offset value of the chromatographic data curve corresponding to each concentration based on the distortion degree and data value of the target peak in the chromatographic data curve corresponding to each concentration includes: For any concentration: Based on the distortion degree of the target peak and the data value of the maximum point of the target peak in the chromatographic data curve corresponding to any concentration, the offset value of the chromatographic data curve corresponding to any concentration is obtained, and the distortion degree and the data value of the maximum point are both positively correlated with the offset value.
7. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, The deviation values of the chromatographic data curves corresponding to all concentrations are used to obtain the error value of the chromatographic data, including: The error value of the chromatographic data is obtained based on the offset value of the chromatographic data curves corresponding to all concentrations and the corresponding concentrations; both the offset value and the concentration are positively correlated with the error value.
8. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 7, characterized in that, The step of obtaining the error value of the chromatographic data based on the offset value of the chromatographic data curves corresponding to all concentrations and the corresponding concentrations includes: The product of the normalized value of the offset of the chromatographic data curve corresponding to each concentration and the normalized value of the corresponding concentration is recorded as the first product corresponding to each concentration. The normalized result of the average of the first product corresponding to all concentrations is used as the error value of the chromatographic data.
9. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, The step of correcting the chromatographic data curves corresponding to each concentration using the error level value includes: Calculate the first difference between the constant 1 and the normalized error value; The product of the first difference and the data value on the chromatographic data curve corresponding to each concentration is used as the correction result of the chromatographic data curve.
10. The method for detecting volatile components of hepatoprotective traditional Chinese medicine preparations using phase chromatography-mass spectrometry according to claim 1, characterized in that, Based on the corrected results, the volatile components of the hepatoprotective traditional Chinese medicine preparation were detected, including: The corrected chromatographic data curves were compared with the chromatographic data curves in the standard chromatographic database, and compounds with a matching degree greater than the preset matching degree were selected as candidate identification results.