Method for evaluating volatile components in compound licorice tablets through gas phase characteristic fingerprints

Abstract

The invention relates to the technical field of chromatographic instruments, and discloses a method for evaluating volatile components in a compound licorice tablet through gas phase characteristic fingerprints, and the method comprises the following steps: preparing a test solution of the compound licorice tablet, preparing a reference substance stock solution of the compound licorice tablet, and generating gas chromatographic conditions of a gas chromatograph; outputting a reference chromatogram of the mixed reference substance solution through a gas chromatograph, and outputting a test chromatogram and an internal standard chromatogram of the test substance solution and the internal standard solution through the gas chromatograph under a gas chromatography condition; determining a camphor peak and a trans-anethole peak in the to-be-tested chromatogram by using the control chromatogram and the internal standard chromatogram; analyzing the camphor content and the trans-anethole content in the compound liquorice tablet from the camphor characteristic spectrum and the trans-anethole characteristic spectrum, and quantifying the volatile components of the compound liquorice tablet by utilizing the camphor content and the trans-anethole content according to the internal standard chromatogram and the control chromatogram. The method can be used for evaluating the quality of the volatile components of the compound liquorice tablets.

Description

Technical Field

[0001] The invention relates to the technical field of chromatographs, and in particular to a method for evaluating volatile components in compound licorice tablets by using gas phase characteristic fingerprints. Background Art

[0002] Compound licorice tablets are prepared by drying licorice extract, grinding it, adding sodium benzoate and opium powder and evenly mixing it into granules, adding camphor and star anise oil dissolved in a small amount of ethanol, mixing them evenly and pressing them into tablets. Compound licorice tablets are antitussive and expectorant drugs, which have a strong protective effect on the nervous system.

[0003] Fingerprint technology is a comprehensive and quantifiable identification method. It is of great significance in the determination of components and authenticity of the quality of traditional Chinese medicine or natural medicine. With the continuous development of science and technology, people have gradually realized that the quality control method formed by only targeting a certain chemical component or using a certain detection method can no longer properly reflect the intrinsic quality of the product. The effective means to solve this problem is to establish innovative quality control methods and characteristic fingerprint control modes, and strengthen the scientific and standardized quality evaluation of traditional Chinese medicine. At present, the Chinese Pharmacopoeia does not control the volatile components in compound licorice tablets, and it is impossible to reflect its efficacy. Therefore, it is particularly important to evaluate the quality of volatile components of compound licorice tablets. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a method for evaluating volatile components in compound licorice tablets by using gas phase characteristic fingerprints, which can be used to evaluate the quality of volatile components in compound licorice tablets.

[0005] In a first aspect, the present invention provides a method for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprint, comprising:

[0006] preparing a test solution of compound licorice tablets, preparing an internal standard solution of the compound licorice tablets, preparing a reference substance stock solution of the compound licorice tablets, and preparing a mixed reference substance solution of the compound licorice tablets using the internal standard solution and the reference substance stock solution, wherein the reference substance stock solution includes a camphor reference solution and a trans-anethole reference solution;

[0007] Determine the gas chromatograph of the compound licorice tablets, and generate the gas chromatographic conditions of the gas chromatograph, wherein the gas chromatograph includes a chromatographic column, a stationary liquid, an injection port, a flame ionization detector and a carrier gas cylinder, and the gas chromatographic conditions include the liquid conditions of the stationary liquid, the injection conditions of the injection port, the detection conditions of the flame ionization detector and the carrier gas conditions of the carrier gas cylinder;

[0008] Inputting the mixed reference solution into the gas chromatograph to output a reference chromatogram of the mixed reference solution through the gas chromatograph under the gas chromatographic conditions, inputting the test solution and the internal standard solution into the gas chromatograph to output a test chromatogram and an internal standard chromatogram of the test solution and the internal standard solution through the gas chromatograph under the gas chromatographic conditions;

[0009] Determine the camphor peak and the trans-anethole peak in the test chromatogram by using the reference chromatogram and the internal standard chromatogram, and analyze the camphor characteristic spectrum and the trans-anethole characteristic spectrum of the camphor peak and the trans-anethole peak respectively;

[0010] The camphor content and the trans-anethole content in the compound licorice tablets are analyzed from the camphor characteristic spectrum and the trans-anethole characteristic spectrum, and the volatile components of the compound licorice tablets are quantified using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets.

[0011] In a possible implementation of the first aspect, the preparation of the test solution for the compound licorice tablets includes:

[0012] Select and reserve compound licorice tablets;

[0013] Grinding the reserved compound licorice tablets to obtain compound licorice powder;

[0014] Extracting a target compound licorice powder that meets a preset number of compound licorice tablets in the reserve compound licorice tablets from the compound licorice powder;

[0015] Adding the target compound licorice powder and a preset amount of water into a preset volumetric bottle to obtain a mixed powder solution;

[0016] Performing ultrasonic treatment on the mixed powder solution for a first preset time to obtain a powder solution;

[0017] Adding a preset amount of ethyl acetate into the powder solution to obtain a solution to be centrifuged;

[0018] Transferring the solution to be centrifuged into a centrifuge tube, and centrifuging the solution to be centrifuged at a preset speed of the centrifuge tube;

[0019] When the centrifugation time of the solution to be centrifuged at the preset speed of the centrifuge tube reaches a second preset time, removing a preset amount of supernatant and a preset amount of internal standard solution in the centrifuge tube into a small centrifuge tube;

[0020] After the preset amount of supernatant and the preset amount of internal standard solution are shaken in the small centrifuge tube, the test solution in the preset amount of supernatant and the preset amount of internal standard solution is determined by a filter membrane with a preset diameter.

[0021] In a possible implementation of the first aspect, the preparation of the reference substance stock solution of the compound licorice tablets comprises:

[0022] Selecting the camphor reference substance and trans-anethole reference substance of the compound licorice tablets;

[0023] Adding ethyl acetate to the camphor reference substance to obtain a first mixed solution between the camphor reference substance and the ethyl acetate;

[0024] When the first solution concentration of the first mixed solution meets the first preset concentration, using the first mixed solution as a camphor control solution of the compound licorice tablet;

[0025] adding ethyl acetate to the trans-anethole reference substance to obtain a second mixed solution between the trans-anethole reference substance and the ethyl acetate;

[0026] When the second solution concentration of the second mixed solution meets the second preset concentration, the second mixed solution is used as the trans-anethole control solution of the compound licorice tablets;

[0027] The camphor control solution and the trans-anethole control solution are used as the reference substance stock solutions.

[0028] In a possible implementation manner of the first aspect, generating the gas chromatography conditions of the gas chromatograph includes:

[0029] obtaining a sample material of the gas chromatograph and a real chromatogram corresponding to the sample material;

[0030] Inputting the sample material into the gas chromatograph so as to output a sample chromatogram corresponding to the sample material through the gas chromatograph;

[0031] calculating a chromatogram error between the true chromatogram and the sample chromatogram;

[0032] Constructing a linear mapping relationship between gas chromatographic parameters of the gas chromatograph and the sample chromatogram;

[0033] Based on the linear mapping relationship, performing parameter correction on the gas chromatography parameters to obtain correction parameters;

[0034] The correction parameters are used as the gas chromatography conditions.

[0035] In a possible implementation manner of the first aspect, calculating a chromatogram error between the true chromatogram and the sample chromatogram includes:

[0036] Constructing a ordinate matching string between the real chromatogram and the sample chromatogram;

[0037] Calculating the ordinate similarity between the ordinate in the real chromatogram and the ordinate in the sample chromatogram in the ordinate matching string;

[0038] Selecting the maximum similarity from the vertical coordinate similarities;

[0039] Obtaining a target matching string corresponding to the maximum similarity in the ordinate matching string;

[0040] Calculating a vertical coordinate loss value between a vertical coordinate in a real chromatogram and a vertical coordinate in a sample chromatogram in the target matching string;

[0041] The vertical axis loss value is taken as the chromatogram error.

[0042] In a possible implementation manner of the first aspect, constructing a linear mapping relationship between a gas chromatographic parameter of the gas chromatograph and the sample chromatogram includes:

[0043] constructing an initial linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram;

[0044] Solving the parameters to be solved in the initial linear mapping relationship to obtain constant parameters;

[0045] The initial linear mapping relationship is converted into a linear mapping relationship between the gas chromatography parameters of the gas chromatograph and the sample chromatogram based on the constant parameter.

[0046] In a possible implementation manner of the first aspect, performing parameter correction on the gas chromatography parameter based on the linear mapping relationship to obtain the corrected parameter includes:

[0047] Taking partial derivative of the ordinate loss value under the linear mapping relationship to obtain partial derivative parameters;

[0048] Using the partial derivative parameters to adjust the gas chromatography parameters to obtain adjustment parameters;

[0049] When the vertical coordinate loss value corresponding to the adjustment parameter is the minimum loss value, the adjustment parameter is used as the correction parameter.

[0050] In a possible implementation of the first aspect, the determining of the camphor peak and the trans-anethole peak in the test chromatogram using the reference chromatogram and the internal standard chromatogram comprises:

[0051] Taking the phenylpropanolamine peak in the internal standard chromatogram as the reference peak;

[0052] Collecting the relative retention time of the reference substance peak in the internal standard chromatogram;

[0053] Identifying a first target peak in the test chromatogram that is before the relative retention time, and identifying a second target peak in the control chromatogram that is before the relative retention time;

[0054] When the peak similarity between the first target peak and the second target peak is the largest, taking the first target peak as the camphor peak;

[0055] Identifying a third target peak in the test chromatogram that is after the relative retention time, and identifying a fourth target peak in the control chromatogram that is after the relative retention time;

[0056] When the peak similarity between the third target peak and the fourth target peak is the largest, the third target peak is used as the trans-anethole peak.

[0057] In a possible implementation of the first aspect, the volatile components of the compound licorice tablets are quantified using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets, including:

[0058] Calculating a first content ratio between the camphor content and the phenylpropanolamine content in the internal standard chromatogram;

[0059] Constructing a first regression model between the camphor content in the control chromatogram and the first content ratio;

[0060] Calculating a second content ratio between the trans-anethole content and the phenylpropanol content in the internal standard chromatogram;

[0061] constructing a second regression model between the trans-anethole content in the control chromatogram and the second content ratio;

[0062] Calculate a first correlation coefficient between the camphor content in the control chromatogram and the first content ratio;

[0063] Calculate a second correlation coefficient between the trans-anethole content in the control chromatogram and the second content ratio;

[0064] The first regression model, the second regression model, the first correlation coefficient and the second correlation coefficient are used to quantify the volatile components of the compound licorice tablets to obtain gas phase characteristic fingerprint evaluation results of the volatile components in the compound licorice tablets.

[0065] In a possible implementation manner of the first aspect, performing partial derivative of the ordinate loss value under the linear mapping relationship to obtain the partial derivative parameter includes:

[0066] The partial derivative of the ordinate loss value under the linear mapping relationship is obtained to obtain the partial derivative parameter.

[0067] Compared with the prior art, the technical principle and beneficial effects of this solution are:

[0068] The embodiment of the present invention generates the gas chromatographic conditions of the gas chromatograph to correct the instrument parameters of the gas chromatograph when the instrument parameters of the gas chromatograph affect the chromatogram, thereby improving the quality of the chromatogram and paving the way for the subsequent analysis of the component content in the chromatogram. Furthermore, the embodiment of the present invention quantifies the volatile components of the compound licorice tablets by using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram, so as to analyze whether the content of volatile components such as camphor and trans-anethole in the test solution meets the standard content, thereby achieving quality control of the compound licorice tablets corresponding to the test solution. Therefore, the method for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprints proposed in the embodiment of the present invention can evaluate the quality of volatile components in compound licorice tablets. BRIEF DESCRIPTION OF THE DRAWINGS

[0069] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and, together with the description, serve to explain the principles of the invention.

[0070] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0071] Figure 1 A schematic flow chart of a method for evaluating volatile components in compound licorice tablets by using gas phase characteristic fingerprints provided in one embodiment of the present invention;

[0072] Figure 2 A schematic diagram of a module of a system for evaluating volatile components in compound licorice tablets using gas phase characteristic fingerprints provided in one embodiment of the present invention. DETAILED DESCRIPTION

[0073] 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.

[0074] The embodiment of the present invention provides a method for evaluating volatile components in compound licorice tablets by gas-phase characteristic fingerprints, and the execution subject of the method for evaluating volatile components in compound licorice tablets by gas-phase characteristic fingerprints includes but is not limited to at least one of the electronic devices such as a server and a terminal that can be configured to execute the method provided by the embodiment of the present invention. In other words, the method for evaluating volatile components in compound licorice tablets by gas-phase characteristic fingerprints can be executed by software or hardware installed on a terminal device or a server device, and the software can be a blockchain platform. The server includes but is not limited to: a single server, a server cluster, a cloud server or a cloud server cluster, etc. The server can be an independent server, or it can be a cloud server that provides basic cloud computing services such as cloud services, cloud databases, cloud computing, cloud functions, cloud storage, network services, cloud communications, middleware services, domain name services, security services, content delivery networks (Content Delivery Network, CDN), and big data and artificial intelligence platforms.

[0075] See also Figure 1 FIG. 1 is a flow chart of a method for evaluating volatile components in compound licorice tablets by using gas phase characteristic fingerprints according to an embodiment of the present invention. Figure 1 The method described in the gas phase characteristic fingerprint evaluation of volatile components in compound licorice tablets includes:

[0076] S1. Prepare a test solution of compound licorice tablets, prepare an internal standard solution of the compound licorice tablets, prepare a reference substance stock solution of the compound licorice tablets, and use the internal standard solution and the reference substance stock solution to prepare a mixed reference substance solution of the compound licorice tablets, wherein the reference substance stock solution includes a camphor reference solution and a trans-anethole reference solution.

[0077] In one embodiment of the present invention, the preparation of the test solution of the compound licorice tablets includes: selecting a reserve compound licorice tablet; grinding the reserve compound licorice tablets to obtain a compound licorice powder; extracting a target compound licorice powder that meets a preset number of compound licorice tablets in the reserve compound licorice tablets from the compound licorice powder; adding the target compound licorice powder and a preset amount of water into a preset volumetric bottle to obtain a mixed powder solution; performing an ultrasonic treatment on the mixed powder solution for a first preset time to obtain a powder solution; adding a preset ethyl acetate to the powder solution; , obtaining a solution to be centrifuged; transferring the solution to be centrifuged into a centrifuge tube, and centrifuging the solution to be centrifuged at a preset speed of the centrifuge tube; when the centrifugation time of the solution to be centrifuged at the preset speed of the centrifuge tube reaches a second preset time, transferring a preset amount of supernatant and a preset amount of internal standard solution in the centrifuge tube into a small centrifuge tube; after shaking the preset amount of supernatant and the preset amount of internal standard solution in the small centrifuge tube, determining the test solution in the preset amount of supernatant and the preset amount of internal standard solution through a filter membrane of a preset diameter.

[0078] Exemplarily, the process of preparing the test solution of the compound licorice tablets is as follows: selecting 5 compound licorice tablets; grinding the 5 compound licorice tablets to obtain compound licorice powder; extracting the target compound licorice powder that meets 2 of the 5 compound licorice tablets from the compound licorice powder; adding the target compound licorice powder and 10 mL of water to the 25 mL volumetric flask to obtain a mixed powder solution; subjecting the mixed powder solution to ultrasonic treatment for 10 minutes to obtain a powder solution; adding 10 mL of ethyl acetate to the powder solution to obtain a solution to be centrifuged. liquid; transferring the solution to be centrifuged into a centrifuge tube, and centrifuging the solution to be centrifuged at a speed of 2000r / min through the centrifuge tube; when the centrifugation time of the solution to be centrifuged at a speed of 2000r / min through the centrifuge tube reaches 5 minutes, transferring 3mL of supernatant and 1mL of internal standard solution in the centrifuge tube into a small centrifuge tube; after shaking the 3mL of supernatant and the 1mL of internal standard solution in the small centrifuge tube, determine the test solution in the 3mL of supernatant and the 1mL of internal standard solution through a 0.45μm filter membrane.

[0079] In one embodiment of the present invention, the preparation of the internal standard solution of the compound licorice tablets includes: adding ethyl acetate to phenylpropanolamine to obtain a mixed solution between the phenylpropanolamine and the ethyl acetate; when the solution concentration of the mixed solution meets the preset concentration, using the mixed solution as the internal standard solution.

[0080] Illustratively, the process of preparing the internal standard solution of the compound licorice tablets is as follows: take an appropriate amount of phenylpropanolamine, accurately weigh it, add ethyl acetate to dissolve and dilute it to make a solution containing 500 μg per 1 mL, shake well, and obtain it.

[0081] In one embodiment of the present invention, the preparation of the reference substance stock solution of the compound licorice tablets includes: selecting a camphor reference substance and a trans-anethole reference substance of the compound licorice tablets; adding ethyl acetate to the camphor reference substance to obtain a first mixed solution between the camphor reference substance and the ethyl acetate; when the first solution concentration of the first mixed solution meets the first preset concentration, the first mixed solution is used as the camphor reference solution of the compound licorice tablets; adding ethyl acetate to the trans-anethole reference substance to obtain a second mixed solution between the trans-anethole reference substance and the ethyl acetate; when the second solution concentration of the second mixed solution meets the second preset concentration, the second mixed solution is used as the trans-anethole reference solution of the compound licorice tablets; the camphor control solution and the trans-anethole control solution are used as the reference substance stock solutions.

[0082] Exemplarily, the process of preparing the reference stock solution of the compound licorice tablets is, for example: take appropriate amounts of camphor reference and trans-anethole reference, accurately weigh them, add ethyl acetate to dissolve and dilute them to prepare a camphor reference stock solution containing 2000 μg per 1 mL and a trans-anethole reference stock solution containing 400 μg per 1 mL, shake well, and obtain.

[0083] In one embodiment of the present invention, the method of preparing the mixed reference solution of the compound licorice tablets using the internal standard solution and the reference stock solution comprises: mixing the internal standard solution of the same concentration with the reference stock solutions of different concentrations to obtain the mixed reference solution of the compound licorice tablets.

[0084] Illustratively, the process of preparing the mixed reference solution of the compound licorice tablets using the internal standard solution and the reference stock solution is, for example: accurately measure appropriate amounts of camphor reference stock solution, trans-anethole reference stock solution and internal standard solution in a 10 mL volumetric flask, shake well, and prepare a series of mixed reference solutions (with the same internal standard concentration and different camphor and trans-anethole concentrations).

[0085] S2. Determine the gas chromatograph of the compound licorice tablets and generate gas chromatographic conditions of the gas chromatograph, wherein the gas chromatograph includes a chromatographic column, a stationary liquid, an injection port, a flame ionization detector and a carrier gas cylinder, and the gas chromatographic conditions include liquid conditions of the stationary liquid, injection conditions of the injection port, detection conditions of the flame ionization detector and carrier gas conditions of the carrier gas cylinder.

[0086] The embodiment of the present invention generates gas chromatographic conditions of the gas chromatograph to correct the instrument parameters of the gas chromatograph when the instrument parameters of the gas chromatograph affect the chromatogram, thereby improving the quality of the chromatogram and paving the way for subsequent analysis of the component content in the chromatogram.

[0087] In one embodiment of the present invention, the generating of the gas chromatography conditions of the gas chromatograph includes: obtaining a sample material of the gas chromatograph and a real chromatogram corresponding to the sample material; inputting the sample material into the gas chromatograph to output a sample chromatogram corresponding to the sample material through the gas chromatograph; calculating a chromatogram error between the real chromatogram and the sample chromatogram; constructing a linear mapping relationship between the gas chromatography parameters of the gas chromatograph and the sample chromatogram; based on the linear mapping relationship, performing parameter correction on the gas chromatography parameters to obtain correction parameters; and using the correction parameters as the gas chromatography conditions.

[0088] The sample material refers to a solution sample having a content consistent with that of the reference substance stock solution.

[0089] In another embodiment of the present invention, the calculating of the chromatogram error between the true chromatogram and the sample chromatogram includes: constructing a ordinate matching string between the true chromatogram and the sample chromatogram using the following format:

[0090]

[0091] Among them, A and B represent the vertical coordinate matching string, x1, x2, ..., x n Represents the ordinate in the real chromatogram, y1, y2, ..., y n-2 ,y n-1 ,y n represents the ordinate in the sample chromatogram, and n represents the number of ordinates in the real chromatogram;

[0092] Calculate the ordinate similarity between the ordinate in the real chromatogram and the ordinate in the sample chromatogram in the ordinate matching string; select the maximum similarity from the ordinate similarities; obtain the target matching string corresponding to the maximum similarity in the ordinate matching string; calculate the ordinate loss value between the ordinate in the real chromatogram and the ordinate in the sample chromatogram in the target matching string using the following formula:

[0093]

[0094] Among them, L(x,y) represents the vertical coordinate loss value, x i Represents the i-th ordinate in the real chromatogram, y irepresents the i-th ordinate in the sample chromatogram, and n represents the number of ordinates in the real chromatogram;

[0095] The vertical axis loss value is taken as the chromatogram error.

[0096] In another embodiment of the present invention, the constructing of the linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram includes: constructing an initial linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram using the following formula:

[0097] Z=(z1,z2,...,z m ) T

[0098] z j =(u1,u2,...,u d )

[0099] k=(k1,k2,...,z m ) T

[0100] y i =k T Z+b

[0101] Among them, y i =k T Z+b represents the initial linear mapping relationship, y i represents the i-th ordinate in the sample chromatogram, z1,z2,...,z m represents the gas chromatography parameter, z j With u1,u2,...,u d represents a series of parameters that change when the jth gas chromatography parameter changes in the gas chromatograph, d represents the number of the jth gas chromatography parameter, m represents the number of gas chromatography parameters, and Z represents z1, z2, ..., z m The transpose of k1, k2, ..., z m , b represents the parameters to be solved in the initial linear mapping relationship, k represents k1, k2, ..., z m The transpose of

[0102] Solving the parameters to be solved in the initial linear mapping relationship to obtain constant parameters; and converting the initial linear mapping relationship into a linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram based on the constant parameters.

[0103] It should be noted that when the liquid condition is a temperature condition, for example, the stationary liquid has an initial temperature of 80°C, maintained for 5 minutes, raised to 90°C at a rate of 2°C per minute, maintained for 5 minutes, then raised to 200°C at a rate of 20°C per minute, maintained for 2 minutes, and then raised to 220°C at a rate of 20°C per minute, then 80°C, 90°C, 200°C, and 220°C are used as a series of parameters in which the temperature parameter in the gas chromatograph changes, that is, z j With u1,u2,...,u d .

[0104] In another embodiment of the present invention, the gas chromatography parameters are corrected based on the linear mapping relationship to obtain the correction parameters, including: using the following formula to obtain the partial derivative of the ordinate loss value under the linear mapping relationship to obtain the partial derivative parameter:

[0105]

[0106] Among them, ΔZ represents the partial derivative parameter, L(x,y) represents the vertical coordinate loss value, and x i Represents the i-th ordinate in the real chromatogram, y i represents the i-th ordinate in the sample chromatogram, n represents the number of ordinates in the real chromatogram, y i =k T Z+b represents the initial linear mapping relationship, and Z represents z1,z2,...,z m The transpose of , k′, b′ represent the constant parameters corresponding to k and b;

[0107] The gas chromatography parameters are adjusted by using the partial derivative parameters to obtain adjustment parameters; when the vertical coordinate loss value corresponding to the adjustment parameters is the minimum loss value, the adjustment parameters are used as the correction parameters.

[0108] Optionally, the process of adjusting the gas chromatography parameters by using the partial derivative parameters to obtain the adjusted parameters is to add ΔZ to Z to obtain the adjusted value of Z, and then based on Z=(z1, z2, ..., z m ) T The gas chromatography parameters are adjusted to obtain adjustment parameters.

[0109] Further, in an embodiment of the present invention, the liquid condition is a temperature condition, for example, the starting temperature of the stationary liquid is 80°C, maintained for 5 minutes, heated to 90°C at a rate of 2°C per minute, maintained for 5 minutes, then heated to 200°C at a rate of 20°C per minute, maintained for 2 minutes, and then heated to 220°C at a rate of 20°C per minute. The injection conditions of the injection port are the injection port temperature, column head pressure and injection port flow rate, for example, the injection port temperature is 220°C, the column head pressure is 5.6psi, and the flow rate is 1.03mL·min-1. The detection condition of the flame ionization detector is the detection temperature, for example, the flame ionization detector detection temperature is 220°C, and the carrier gas condition of the carrier gas cylinder is the gas flow rate, for example, the air flow rate is 200.0mL·min-1, the hydrogen flow rate is 40.0mL·min-1, and the nitrogen flow rate is 20.0mL·min-1.

[0110] S3, inputting the mixed reference solution into the gas chromatograph, so as to output the reference chromatogram of the mixed reference solution through the gas chromatograph under the gas chromatographic conditions, inputting the test solution and the internal standard solution into the gas chromatograph, so as to output the test chromatogram and the internal standard chromatogram of the test solution and the internal standard solution through the gas chromatograph under the gas chromatographic conditions.

[0111] S4. Determine the camphor peak and trans-anethole peak in the test chromatogram using the control chromatogram and the internal standard chromatogram, and analyze the camphor characteristic spectra and trans-anethole characteristic spectra of the camphor peak and the trans-anethole peak, respectively.

[0112] In one embodiment of the present invention, the method of determining the camphor peak and the trans-anethole peak in the test chromatogram using the reference chromatogram and the internal standard chromatogram comprises: taking the phenylpropanol peak in the internal standard chromatogram as the reference peak; collecting the relative retention time of the reference peak in the internal standard chromatogram; identifying the first target peak in the test chromatogram before the relative retention time, and identifying the second target peak in the reference chromatogram before the relative retention time; when the peak similarity between the first target peak and the second target peak is the largest, taking the first target peak as the camphor peak; identifying the third target peak in the test chromatogram after the relative retention time, and identifying the fourth target peak in the reference chromatogram after the relative retention time; when the peak similarity between the third target peak and the fourth target peak is the largest, taking the third target peak as the trans-anethole peak.

[0113] Optionally, the process of respectively analyzing the camphor characteristic spectrum and the trans-anethole characteristic spectrum of the camphor peak and the trans-anethole peak is achieved by using traditional Chinese medicine quantitative fingerprint software.

[0114] S5. Analyze the camphor content and the trans-anethole content in the compound licorice tablets from the camphor characteristic spectrum and the trans-anethole characteristic spectrum, and quantify the volatile components of the compound licorice tablets using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets.

[0115] Optionally, the process of analyzing the camphor content and the trans-anethole content in the compound licorice tablets from the camphor characteristic spectrum and the trans-anethole characteristic spectrum is achieved by fingerprint technology, which refers to a quality control method based on multi-component analysis, which judges the quality and authenticity of the sample by analyzing the quality and relative content of multiple chemical components in the sample.

[0116] Furthermore, the embodiment of the present invention quantifies the volatile components of the compound licorice tablets by using the camphor content and the trans-anethole content according to the internal standard chromatogram and the control chromatogram, so as to analyze whether the content of volatile components such as camphor and trans-anethole in the test solution meets the standard content, thereby achieving quality control of the compound licorice tablets corresponding to the test solution.

[0117] In one embodiment of the present invention, the method of quantitatively analyzing the volatile components of the compound licorice tablets using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets includes: calculating a first content ratio between the camphor content and the phenylpropanol content in the internal standard chromatogram; constructing a first regression model between the camphor content and the first content ratio in the reference chromatogram; calculating a second content ratio between the trans-anethole content and the phenylpropanol content in the internal standard chromatogram; constructing a second regression model between the trans-anethole content and the second content ratio in the reference chromatogram; calculating a first correlation coefficient between the camphor content and the first content ratio in the reference chromatogram; calculating a second correlation coefficient between the trans-anethole content and the second content ratio in the reference chromatogram; and quantitatively analyzing the volatile components of the compound licorice tablets using the first regression model, the second regression model, the first correlation coefficient and the second correlation coefficient to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets.

[0118] Optionally, the process of using the first regression model, the second regression model, the first correlation coefficient and the second correlation coefficient to quantify the volatile components of the compound licorice tablets to obtain the gas phase characteristic fingerprint evaluation results of the volatile components in the compound licorice tablets refers to evaluating the similarity between volatile components such as camphor and trans-anethole in the mixed reference solution and volatile components such as camphor and trans-anethole in the test solution through regression models and correlation coefficients. The higher the similarity, the higher the consistency between the volatile components such as camphor and trans-anethole in the mixed reference solution and the volatile components such as camphor and trans-anethole in the test solution, and the more the content of volatile components such as camphor and trans-anethole in the test solution conforms to the standard content. Therefore, quality control of the compound licorice tablets corresponding to the test solution can be achieved.

[0119] It can be seen that the embodiment of the present invention generates the gas chromatographic conditions of the gas chromatograph to correct the instrument parameters of the gas chromatograph when the instrument parameters of the gas chromatograph affect the chromatogram, thereby improving the quality of the chromatogram and paving the way for the subsequent analysis of the component content in the chromatogram. Further, the embodiment of the present invention quantifies the volatile components of the compound licorice tablets by using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram, so as to analyze whether the content of volatile components such as camphor and trans-anethole in the test solution meets the standard content, thereby achieving quality control of the compound licorice tablets corresponding to the test solution. Therefore, the method for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprints proposed in the embodiment of the present invention can evaluate the quality of volatile components in compound licorice tablets.

[0120] like Figure 2 Shown is a system functional module diagram of the gas phase characteristic fingerprint evaluation of volatile components in compound licorice tablets of the present invention.

[0121] The system 200 for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprint of the present invention can be installed in an electronic device. According to the functions to be implemented, the system for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprint can include a solution preparation module 201, a condition generation module 202, a chromatogram output module 203, a characteristic analysis module 204 and a component quantification module 205. The module of the present invention can also be called a unit, which refers to a series of computer program segments that can be executed by an electronic device processor and can complete fixed functions, which are stored in the memory of the electronic device.

[0122] In the embodiment of the present invention, the functions of each module / unit are as follows:

[0123] The solution preparation module 201 is used to prepare a test solution of the compound licorice tablets, prepare an internal standard solution of the compound licorice tablets, prepare a reference substance stock solution of the compound licorice tablets, and prepare a mixed reference substance solution of the compound licorice tablets using the internal standard solution and the reference substance stock solution, wherein the reference substance stock solution includes a camphor reference solution and a trans-anethole reference solution;

[0124] The condition generation module 202 is used to determine the gas chromatograph of the compound licorice tablets and generate the gas chromatographic conditions of the gas chromatograph, wherein the gas chromatograph includes a chromatographic column, a stationary liquid, an injection port, a flame ionization detector and a carrier gas cylinder, and the gas chromatographic conditions include the liquid conditions of the stationary liquid, the injection conditions of the injection port, the detection conditions of the flame ionization detector and the carrier gas conditions of the carrier gas cylinder;

[0125] The chromatogram output module 203 is used for inputting the mixed reference solution into the gas chromatograph to output the reference chromatogram of the mixed reference solution through the gas chromatograph under the gas chromatographic conditions, and inputting the test solution and the internal standard solution into the gas chromatograph to output the test chromatogram and the internal standard chromatogram of the test solution and the internal standard solution through the gas chromatograph under the gas chromatographic conditions;

[0126] The characteristic analysis module 204 is used to determine the camphor peak and the trans-anethole peak in the test chromatogram by using the reference chromatogram and the internal standard chromatogram, and analyze the camphor characteristic spectrum and the trans-anethole characteristic spectrum of the camphor peak and the trans-anethole peak respectively;

[0127] The component quantification module 205 is used to analyze the camphor content and the trans-anethole content in the compound licorice tablets from the camphor characteristic spectrum and the trans-anethole characteristic spectrum, and quantify the volatile components of the compound licorice tablets using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain the gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets.

[0128] In detail, the modules in the system 200 for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprints in the embodiment of the present invention are used in the same manner as described above. Figure 1 The method of evaluating the volatile components in compound licorice tablets by gas phase characteristic fingerprint described in is the same technical means and can produce the same technical effect, so it will not be repeated here.

[0129] In addition, each functional module in each embodiment of the present invention may be integrated into one processing unit, each unit may exist physically separately, or two or more units may be integrated into one unit. The above-mentioned integrated unit may be implemented in the form of hardware or in the form of hardware plus software functional modules.

[0130] The above description is only a specific embodiment of the present invention, so that those skilled in the art can understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but should conform to the widest scope consistent with the principles and novel features invented herein.

Claims

1. A method for evaluating volatile components in compound licorice tablets by gas phase characteristic fingerprint, characterized in that: The method comprises: preparing a test solution of compound licorice tablets, preparing an internal standard solution of the compound licorice tablets, preparing a reference substance stock solution of the compound licorice tablets, and preparing a mixed reference substance solution of the compound licorice tablets using the internal standard solution and the reference substance stock solution, wherein the reference substance stock solution includes a camphor reference solution and a trans-anethole reference solution; Determine the gas chromatograph of the compound licorice tablets, and generate the gas chromatographic conditions of the gas chromatograph, wherein the gas chromatograph includes a chromatographic column, a stationary liquid, an injection port, a flame ionization detector and a carrier gas cylinder, and the gas chromatographic conditions include the liquid conditions of the stationary liquid, the injection conditions of the injection port, the detection conditions of the flame ionization detector and the carrier gas conditions of the carrier gas cylinder; Inputting the mixed reference solution into the gas chromatograph to output a reference chromatogram of the mixed reference solution through the gas chromatograph under the gas chromatographic conditions, inputting the test solution and the internal standard solution into the gas chromatograph to output a test chromatogram and an internal standard chromatogram of the test solution and the internal standard solution through the gas chromatograph under the gas chromatographic conditions; Determine the camphor peak and the trans-anethole peak in the test chromatogram by using the reference chromatogram and the internal standard chromatogram, and analyze the camphor characteristic spectrum and the trans-anethole characteristic spectrum of the camphor peak and the trans-anethole peak respectively; The camphor content and the trans-anethole content in the compound licorice tablets are analyzed from the camphor characteristic spectrum and the trans-anethole characteristic spectrum, and the volatile components of the compound licorice tablets are quantified using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain a gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets.

2. The method according to claim 1, characterized in that The test solution for preparing the compound licorice tablets comprises: Select and reserve compound licorice tablets; Grinding the reserved compound licorice tablets to obtain compound licorice powder; Extracting a target compound licorice powder that meets a preset number of compound licorice tablets in the reserve compound licorice tablets from the compound licorice powder; Adding the target compound licorice powder and a preset amount of water into a preset volumetric bottle to obtain a mixed powder solution; Performing ultrasonic treatment on the mixed powder solution for a first preset time to obtain a powder solution; Adding a preset amount of ethyl acetate into the powder solution to obtain a solution to be centrifuged; Transferring the solution to be centrifuged into a centrifuge tube, and centrifuging the solution to be centrifuged at a preset speed of the centrifuge tube; When the centrifugation time of the solution to be centrifuged at the preset speed of the centrifuge tube reaches a second preset time, removing a preset amount of supernatant and a preset amount of internal standard solution in the centrifuge tube into a small centrifuge tube; After the preset amount of supernatant and the preset amount of internal standard solution are shaken in the small centrifuge tube, the test solution in the preset amount of supernatant and the preset amount of internal standard solution is determined by a filter membrane with a preset diameter.

3. The method according to claim 1, characterized in that: The preparation of the reference substance stock solution of the compound licorice tablets comprises: Selecting the camphor reference substance and trans-anethole reference substance of the compound licorice tablets; Adding ethyl acetate to the camphor reference substance to obtain a first mixed solution between the camphor reference substance and the ethyl acetate; When the first solution concentration of the first mixed solution meets the first preset concentration, using the first mixed solution as a camphor control solution of the compound licorice tablet; adding ethyl acetate to the trans-anethole reference substance to obtain a second mixed solution between the trans-anethole reference substance and the ethyl acetate; When the second solution concentration of the second mixed solution meets the second preset concentration, the second mixed solution is used as the trans-anethole control solution of the compound licorice tablets; The camphor control solution and the trans-anethole control solution are used as the reference substance stock solutions.

4. The method according to claim 1, characterized in that: The gas chromatographic conditions for generating the gas chromatograph include: obtaining a sample material of the gas chromatograph and a real chromatogram corresponding to the sample material; Inputting the sample material into the gas chromatograph so as to output a sample chromatogram corresponding to the sample material through the gas chromatograph; calculating a chromatogram error between the true chromatogram and the sample chromatogram; Constructing a linear mapping relationship between gas chromatographic parameters of the gas chromatograph and the sample chromatogram; Based on the linear mapping relationship, performing parameter correction on the gas chromatography parameters to obtain correction parameters; The correction parameters are used as the gas chromatography conditions.

5. The method according to claim 4, characterized in that The calculating the chromatogram error between the true chromatogram and the sample chromatogram comprises: Constructing a ordinate matching string between the real chromatogram and the sample chromatogram; Calculating the ordinate similarity between the ordinate in the real chromatogram and the ordinate in the sample chromatogram in the ordinate matching string; Selecting the maximum similarity from the vertical coordinate similarities; Obtaining a target matching string corresponding to the maximum similarity in the ordinate matching string; Calculating a vertical coordinate loss value between a vertical coordinate in a real chromatogram and a vertical coordinate in a sample chromatogram in the target matching string; The vertical axis loss value is taken as the chromatogram error.

6. The method according to claim 4, characterized in that The step of constructing a linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram comprises: constructing an initial linear mapping relationship between the gas chromatographic parameters of the gas chromatograph and the sample chromatogram; Solving the parameters to be solved in the initial linear mapping relationship to obtain constant parameters; The initial linear mapping relationship is converted into a linear mapping relationship between the gas chromatography parameters of the gas chromatograph and the sample chromatogram based on the constant parameter.

7. The method according to claim 4, characterized in that The method of performing parameter correction on the gas chromatography parameters based on the linear mapping relationship to obtain the corrected parameters includes: Taking partial derivative of the ordinate loss value under the linear mapping relationship to obtain partial derivative parameters; Using the partial derivative parameters to adjust the gas chromatography parameters to obtain adjustment parameters; When the vertical coordinate loss value corresponding to the adjustment parameter is the minimum loss value, the adjustment parameter is used as the correction parameter.

8. The method according to claim 1, characterized in that The method of using the reference chromatogram and the internal standard chromatogram to determine the camphor peak and the trans-anethole peak in the test chromatogram comprises: Taking the phenylpropanolamine peak in the internal standard chromatogram as the reference peak; Collecting the relative retention time of the reference substance peak in the internal standard chromatogram; Identifying a first target peak in the test chromatogram that is before the relative retention time, and identifying a second target peak in the control chromatogram that is before the relative retention time; When the peak similarity between the first target peak and the second target peak is the largest, taking the first target peak as the camphor peak; Identifying a third target peak in the test chromatogram that is after the relative retention time, and identifying a fourth target peak in the control chromatogram that is after the relative retention time; When the peak similarity between the third target peak and the fourth target peak is the largest, the third target peak is used as the trans-anethole peak.

9. The method according to claim 1, characterized in that: The method of quantifying the volatile components of the compound licorice tablets by using the camphor content and the trans-anethole content according to the internal standard chromatogram and the reference chromatogram to obtain the gas phase characteristic fingerprint evaluation result of the volatile components in the compound licorice tablets comprises: Calculating a first content ratio between the camphor content and the phenylpropanolamine content in the internal standard chromatogram; Constructing a first regression model between the camphor content in the control chromatogram and the first content ratio; Calculating a second content ratio between the trans-anethole content and the phenylpropanol content in the internal standard chromatogram; constructing a second regression model between the trans-anethole content in the control chromatogram and the second content ratio; Calculate a first correlation coefficient between the camphor content in the control chromatogram and the first content ratio; Calculate a second correlation coefficient between the trans-anethole content in the control chromatogram and the second content ratio; The first regression model, the second regression model, the first correlation coefficient and the second correlation coefficient are used to quantify the volatile components of the compound licorice tablets to obtain gas phase characteristic fingerprint evaluation results of the volatile components in the compound licorice tablets.

10. The method according to claim 7, characterized in that The partial derivative of the ordinate loss value under the linear mapping relationship is obtained to obtain the partial derivative parameter, including: The partial derivative of the ordinate loss value under the linear mapping relationship is obtained to obtain the partial derivative parameter.

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