Keel authenticity identification method, system and equipment based on X-ray diffraction and medium

Abstract

The invention discloses a keel authenticity identification method, system and equipment based on X-ray diffraction and a medium, and relates to the technical field of keel detection. The method comprises the following steps: testing a keel sample to be tested by adopting an X-ray diffraction method to obtain a diffraction pattern; extracting diffraction peaks at a set diffraction angle in the diffraction pattern, matching each diffraction peak with 14 standard characteristic peaks of the genuine keel, and performing preliminary judgment according to the number of successful matching to obtain a preliminary judgment result; the preliminary judgment result comprises counterfeit products and to-be-determined products; setting the diffraction angle as the diffraction angle corresponding to the standard characteristic peak of the genuine keel; and calculating the crystallinity corresponding to the to-be-determined product according to the characteristic peak at the set diffraction angle, and comparing the calculated crystallinity with a set judgment standard to obtain a final judgment result. The method can combine phase analysis and crystallinity determination, and has the remarkable advantages of high precision, nondestructive detection, high repeatability and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of keel detection, and in particular to a keel authenticity identification method, system, equipment and medium based on X-ray diffraction. Background Art

[0003] Since dragon bones are non-renewable resources, there is adulteration in the market. Common counterfeits include products made from the processed bones of modern large mammals. Existing identification methods mainly rely on property observation and physical and chemical index testing, which are suitable for block or uncrushed samples. However, when the medicinal materials are ground into fine powder, the effectiveness of these conventional methods is significantly reduced, making it difficult to accurately identify the authenticity. Therefore, it is of great significance to scientifically identify dragon bones with the help of modern analytical instruments.

[0004] Although there are many technologies for the authenticity identification of dragon bones, including C 14 Dating method, near infrared spectroscopy, elemental analysis and thermal differential analysis, etc. However, the above technologies still have the following defects and shortcomings:

[0005] C 14 Dating method: It is mainly used to determine the age of carbon-containing materials such as animal and plant remains. Its application may be limited to materials such as dragon bones that may contain no or very low carbon. 14 The accuracy and sensitivity of dating methods are limited, and it may be difficult to accurately determine samples that are very old or have very low carbon content. In addition, the testing costs are high, there are few testing units, and it is very difficult to promote.

[0006] Near infrared spectroscopy analysis: Although the analysis speed is fast and efficient, there may be spectral interference or difficulty in analysis for some complex matrices or specific components of keels. And it mainly relies on the established calibration model for measurement, and may not be able to accurately analyze unknown or counterfeit keel samples.

[0007] Elemental analysis: Usually only the type and content of elements can be determined. The specific components or missing components of the keel may not be directly measured. In addition, the sensitivity and accuracy of the elemental analysis method may be interfered by other components or impurities in the sample. The elemental analysis method cannot fully reflect the overall properties or specific defects of the keel.

[0008] Differential thermal analysis: It is mainly used to measure the thermal effect changes of materials. It may not be able to detect keels that are not accompanied by thermal effect changes. At the same time, the quantitative analysis accuracy of differential thermal analysis is low, and it is mainly used for qualitative analysis. It cannot directly reflect the quality changes or specific defect types of keels, and is greatly affected by experimental conditions and sample parameters.

[0009] In summary, existing methods have certain limitations in terms of sensitivity, accuracy, cost control and ease of operation. Summary of the invention

[0010] The purpose of the present invention is to provide a method, system, equipment and medium for identifying the authenticity of dragon bones based on X-ray diffraction, which can combine phase analysis with crystallinity determination, has significant advantages such as high precision, non-destructive testing, and strong repeatability, and provides a new scientific and reliable way for identifying the authenticity of mineral medicines.

[0011] To achieve the above object, the present invention provides the following solutions:

[0012] A method for identifying the authenticity of dragon bones based on X-ray diffraction, comprising:

[0013] The keel sample to be tested is tested by an X-ray diffraction method to obtain a diffraction spectrum; the diffraction spectrum includes a plurality of diffraction peaks and corresponding peak intensity data;

[0014] Extract the diffraction peaks at the set diffraction angle in the diffraction spectrum, match each diffraction peak with the 14 standard characteristic peaks of the genuine keel, and make a preliminary judgment based on the number of successful matches to obtain a preliminary judgment result; the preliminary judgment result includes counterfeits and undetermined products; the set diffraction angle is the diffraction angle corresponding to the standard characteristic peak of the genuine keel;

[0015] The crystallinity of the sample to be determined is calculated according to the characteristic peak at the set diffraction angle, and the calculated crystallinity is compared with the set judgment standard to obtain the final judgment result.

[0016] Optionally, the X-ray diffraction method is performed using an XRPD instrument, which uses CuKα radiation as the incident light source. The operating voltage of the X-ray tube in the instrument is 40 kV, the current is 40 mA, the aperture system is set to DS=SS=1°, and the scanning range is 3°~65°.

[0017] Optionally, the set diffraction angles include 25.82°, 28.14°, 29.18°, 32.02°, 33.16°, 34.16°, 40.10°, 42.40°, 46.94°, 48.26°, 49.64°, 51.68°, 53.08° and 63.98°.

[0018] Optionally, the successful matching criterion of the diffraction peak is: when the matching tolerance between any diffraction peak and the corresponding standard characteristic peak of the genuine keel is within ±0.2°, it is determined to be a successful match.

[0019] Optionally, the preliminary determination based on the number of successful matches specifically includes:

[0020] When the number of successful matches is less than 7, it is judged as a counterfeit;

[0021] When the number of successful matches is ≥ 7 peaks, it is determined to be a pending product.

[0022] Optionally, the calculation formula of the crystallinity is:

[0023] Optionally, comparing the calculated crystallinity with a set judgment standard specifically includes:

[0024] When the crystallinity of any diffraction peak is ≥30%, it is judged as a counterfeit;

[0025] When there are more than or equal to 3 diffraction peaks other than 32.02° and the crystallinity is greater than 10%, it is judged as a counterfeit;

[0026] When the crystallinity of the diffraction peak at 32.02° is ≤20%, and the other diffraction peaks are ≤10%, it is judged to be authentic;

[0027] When there is a diffraction peak and the crystallinity is between 10% and 15%, it is judged to be authentic and re-examination is recommended.

[0028] The present invention also provides a keel authenticity identification system based on X-ray diffraction, comprising:

[0029] A data acquisition unit is used to test the keel sample to be tested by using an X-ray diffraction method to obtain a diffraction spectrum; the diffraction spectrum includes a plurality of diffraction peaks and corresponding peak intensity data;

[0030] A preliminary determination unit is used to extract the diffraction peaks at the set diffraction angle in the diffraction spectrum, match each diffraction peak with the 14 standard characteristic peaks of the genuine keel, and make a preliminary determination according to the number of successful matches to obtain a preliminary determination result; the preliminary determination result includes counterfeits and undetermined products; the set diffraction angle is the diffraction angle corresponding to the standard characteristic peak of the genuine keel;

[0031] The final identification unit is used to calculate the crystallinity corresponding to the product to be determined according to the characteristic peak at the set diffraction angle, and compare the calculated crystallinity with the set judgment standard to obtain the final judgment result.

[0032] The present invention also provides an electronic device, including a memory and a processor, wherein the memory is used to store a computer program, and the processor runs the computer program to enable the electronic device to execute the above-mentioned dragon bone authenticity identification method based on X-ray diffraction.

[0033] The present invention also provides a computer-readable storage medium storing a computer program, which, when executed by a processor, implements the dragon bone authenticity identification method based on X-ray diffraction as described above.

[0034] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0035] The present invention discloses a method, system, equipment and medium for distinguishing the authenticity of keels based on X-ray diffraction, the method comprising testing a keel sample to be tested by an X-ray diffraction method to obtain a diffraction spectrum; extracting diffraction peaks at a set diffraction angle in the diffraction spectrum, matching each diffraction peak with 14 standard characteristic peaks of genuine keels, and making a preliminary judgment according to the number of successful matches to obtain a preliminary judgment result; the preliminary judgment result includes counterfeits and undetermined products; setting the diffraction angle to the diffraction angle corresponding to the standard characteristic peak of the genuine keel; calculating the crystallinity corresponding to the undetermined product according to the characteristic peak at the set diffraction angle, and comparing the calculated crystallinity with the set judgment standard to obtain the final judgment result. The present invention can combine phase analysis with crystallinity determination, has significant advantages such as high precision, non-destructive testing, and strong repeatability, and provides a scientific and reliable new way for distinguishing the authenticity of mineral medicines. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] 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 will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0037] Figure 1 This is a flowchart of keel sample preparation and specific testing in this embodiment;

[0038] Figure 2 This is the X-ray diffraction fingerprint of 9 batches of authentic dragon bones in this example;

[0039] Figure 3 It is the average X-ray diffraction fingerprint of 9 batches of authentic dragon bones in this example;

[0040] Figure 4 The X-ray diffraction fingerprints of two batches of five-flowered keel in this example;

[0041] Figure 5 The X-ray diffraction fingerprints of 4 batches of counterfeit dragon bones in this example;

[0042] Figure 6 The X-ray diffraction fingerprints of 8 batches of counterfeit dragon bones in this example;

[0043] Figure 7 This is the principal component analysis diagram of the dragon bone X-ray diffraction fingerprint in this embodiment;

[0044] Figure 8This is the X-ray diffraction comparison characteristic spectrum of the keel in this embodiment;

[0045] Fig. 9 This is the X-ray diffraction pattern of 4 batches of counterfeit keel in this example;

[0046] Fig.10 This is the X-ray diffraction pattern of 5 batches of counterfeit keel in this example;

[0047] Fig.11 The following are the X-ray diffraction patterns of three batches of counterfeit dragon bones in this example. DETAILED DESCRIPTION

[0048] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0049] The purpose of the present invention is to provide a method, system, equipment and medium for identifying the authenticity of dragon bones based on X-ray diffraction, which can combine phase analysis with crystallinity determination, has significant advantages such as high precision, non-destructive testing, and strong repeatability, and provides a new scientific and reliable way for identifying the authenticity of mineral medicines.

[0050] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0051] like Figure 1 As shown, the present invention provides a method for identifying the authenticity of dragon bones based on X-ray diffraction, comprising:

[0052] Step 100: Using an X-ray diffraction method to test the keel sample to obtain a diffraction pattern; the diffraction pattern includes a plurality of diffraction peaks and corresponding peak intensity data.

[0053] Step 200: extract the diffraction peaks at the set diffraction angle in the diffraction pattern, match each diffraction peak with the 14 standard characteristic peaks of the authentic dragon bone, and make a preliminary judgment based on the number of successful matches to obtain a preliminary judgment result; the preliminary judgment result includes counterfeits and undetermined products; the set diffraction angle is the diffraction angle corresponding to the standard characteristic peak of the authentic dragon bone.

[0054] Step 300: Calculate the crystallinity corresponding to the product to be determined according to the characteristic peak at the set diffraction angle, and compare the calculated crystallinity with the set judgment standard to obtain the final judgment result.

[0055] As a specific implementation method, it is necessary to first determine the 14 standard characteristic peaks of the genuine keel, and the detailed process is as follows.

[0056] 1. Sample preparation and specific test process: Take the dragon bone and grind it in an agate mortar and pass it through a 200-mesh sieve. All experimental samples were tested at the Anhui Provincial Food and Drug Inspection Institute. Put the fine powder into the groove of the glass plate and press the fine powder with a glass slide. The incident light source is CuKα radiation; Ni filter; the X-ray tube working voltage is 40kV; the current is 40mA; the aperture system is DS=SS=1°; RS=0.3mm. Use continuous scanning mode, the scanning rate is 8° / min; the 2θ resolution is 0.02°; the scanning range is 3°~65°; and a super energy detector is used. Collect experimental data, export RAW format and ASC format files, use MDIJade9.0 analysis software to process the data, and obtain each batch of X-ray diffraction patterns.

[0057] 2. Sample source: The 23 batches of dragon bone samples in the present invention were all provided by Anhui Provincial Food and Drug Inspection Institute, including 9 batches of authentic dragon bones, 2 batches of five-flowered dragon bones, and 12 batches of counterfeit dragon bones.

[0058] 3. Spectrum comparison

[0059] 3.1 The authentic keel samples were processed using Origin2024 software to draw the X-ray diffraction common pattern diagram of 9 batches of authentic keel samples from LG1 to LG9, see Figure 2 . Using JADE9.0 digital signal processing technology, we searched for peaks and phases in these spectra, and consulted the "Powder Diffraction Card PDF Card" edited and published by the International Federation of Powder Diffraction Standards. It was preliminarily determined that the X-ray diffraction data were basically consistent with PDF#01-086-0740 (hydroxylapatite) and PDF#01-075-9356, indicating that these genuine dragon bone samples mainly contain Ca5(PO4)3(OH) (hydroxylapatite) and calcite (CaCO3), which is consistent with the literature reports. In addition, compared with other samples, sample LG2 has an additional peak at 2θ=26.444°, which is the characteristic peak of CsCuGd2Te4, consistent with PDF#97-038-0381; sample LG3 has an additional peak at 2θ=26.689°, which is consistent with PDF#97-000-1271 and is the characteristic peak of Pb(SeO3); this indicates that there are other components in some samples, which may be related to the geological antiquity of the keel. The peaks in the X-ray diffraction patterns of these nine batches of genuine keel bones are superimposed and averaged to obtain the average spectrum, which is used as the reference spectrum of the keel, see Figure 3 .

[0060] 3.2 Wuhua keel map: Wuhua keel was processed by Origin2024 software to draw the X-ray diffraction common pattern map of two batches of Wuhua keel samples, LG10~LG11, see Figure 4 The results of the physical phase search showed that the two batches of dragon bone samples mainly contained hydroxyapatite and calcite, and their physical phase compositions were found to be completely consistent with those of LG1 to LG9, which means that both were genuine dragon bones.

[0061] 3.3 Spectral analysis of keel counterfeit: A keel counterfeit was detected through the fingerprint information established experimentally. Its X-ray diffraction spectrum is shown in Figure 5 and Figure 6 , it can be seen that the characteristics of the spectrum are far from the authentic dragon bone. Through the physical phase search, it was found that Figure 5 These four batches of samples all contain hydroxyapatite and calcite, which are the main components of authentic dragon bones. They also contain a large amount of gypsum, whose diffraction intensity is greater than that of the main components. Therefore, they are fake dragon bones. Through phase retrieval, it was found that Figure 6 The samples LG12, LG13, LG14, LG22, and LG23 only contain a large amount of CaCO3 and a small amount of quartz, but no calcium hydroxyphosphate. Therefore, they are fake dragon bones. The samples LG17, LG18, and LG19 only contain calcium hydroxyphosphate, but no calcium carbonate. According to relevant literature, the main inorganic component in modern mammal bones is hydroxyapatite (Ca5(PO4)3(OH)). It is speculated that modern mammal bones may have been used for adulteration.

[0062] 4. Principal component analysis of fingerprints

[0063] According to the peak intensity of 23 batches of dragon bone X-ray diffraction fingerprints, PCA principal component analysis was performed on the dragon bone X-ray diffraction fingerprints using Maiwei Cloud social science statistics software. Figure 7 As shown. From the principal component analysis of the dragon bone X-ray diffraction fingerprint, it can be seen that the genuine dragon bones and counterfeit dragon bones are in a dispersed state. Among them, two batches of counterfeit dragon bones are also gathered in the genuine and five-flowered dragon bones. Because these two batches of counterfeit dragon bones have been adulterated, they will also retain the characteristics of genuine dragon bones. Combined with 1.3, it can be seen that LG18 only contains calcium hydroxyphosphate and no calcium carbonate. According to the literature, the main inorganic component in the bones of modern mammals is hydroxyapatite (Ca5(PO4)3(OH)). It is speculated that modern mammal bones may be used for adulteration; LG21 contains hydroxyapatite and calcite, which are the main components of genuine dragon bones. At the same time, they all contain a large amount of gypsum, whose diffraction intensity is greater than the main component, so it is a counterfeit dragon bone. We can see that modern adulteration methods are complex in form, and the adulteration technology of counterfeit dragon bones is superb. It is feasible to use X-ray diffraction fingerprints to identify the authenticity of dragon bones.

[0064] 5. Crystallinity analysis

[0065] Determining the crystallinity of keel bones by X-ray diffraction (XRPD) technology can provide a strong basis for identifying its authenticity. Authentic keel bones, due to their specific composition and structure, will show specific crystallinity characteristics. However, counterfeit keel bones, due to differences in their composition and structure, often have significantly different crystallinity from the authentic ones. Since most mineral medicines are crystalline substances, in the application of identifying the authenticity of keel bones, X-ray diffraction technology may measure the X-ray diffraction pattern of keel samples. In the XRPD spectrum, the crystalline material will show a series of diffraction peaks, which correspond to specific crystal planes of the material. The higher the crystallinity, the sharper the diffraction peak and the higher the peak intensity; the lower the crystallinity, the wider the diffraction peak and the lower the peak intensity. This is because the grain size of the high-crystallinity material is larger, and the half-width at half-maximum (FWHM) of the diffraction peak is smaller, while the grain size of the low-crystallinity material is smaller, and the half-width at half-maximum (FWHM) of the diffraction peak is larger. By comparison Figure 2 and Figure 5 , Figure 2 and Figure 6 It was found that the diffraction peak of the genuine keel is relatively wide and the intensity of the diffraction peak is relatively low; the diffraction peak of the counterfeit keel is relatively narrow and the intensity of the diffraction peak is relatively high. By comparing the ratio of the diffraction peak intensity to the total intensity of the entire diffraction peak, the crystallinity of the keel can be calculated. The crystallinity of the genuine keel should be within a certain range and is significantly different from that of the counterfeit keel. It is feasible to use the degree of crystallinity to identify the authenticity of keels.

[0066] 6. Establishment of dragon bone fingerprint

[0067] 6.1 X-ray diffraction spectrum peak search: Using JADE 9.0 software, the spectrum of 11 batches of genuine dragon bones was searched for peaks. After analysis and comparison, 14 common characteristic peaks with larger intensities were selected ( Figure 8 ) as the characteristic fingerprint peak of dragon bones. Then, peak searching was performed on other samples to obtain the peak position values ​​(2θ / °) and diffraction peak intensities (I). The X-ray diffraction pattern of dragon bones should have characteristic diffraction peaks at diffraction angles (2θ) of 25.82°, 28.14°, 29.18°, 32.02°, 33.16°, 34.16°, 40.10°, 42.40°, 46.94°, 48.26°, 49.64°, 51.68°, 53.08° and 63.98° (the error range is ±0.2°). The spectra of 4 batches of fake keels, 5 batches of fake keels and 3 batches of fake keels were peak-searched respectively, and the diffraction patterns of the 3 types of fake keels were obtained as follows: Fig. 9 , Fig.10 , Fig.11. By comparing the diffraction patterns of genuine keels and counterfeit keels, the differences in the number, position and intensity of diffraction peaks can be clearly seen. The diffraction peaks of genuine keels are relatively clear and have specific intensity patterns, while the diffraction peaks of counterfeits may present different forms or completely lack certain characteristic peaks. By analyzing the half-width at half maximum (FWHM) and intensity of the diffraction peaks, the crystallinity of the sample can be calculated. The diffraction angles of the 14 characteristic peaks of genuine keels correspond to different diffraction peak intensities, and the crystallinity calculation is shown in formula (1):

[0068]

[0069] The calculation results of crystallinity show that the characteristic peaks of 11 batches of genuine keels have a crystallinity between 6% and 11% when the diffraction angle (2θ) is 25.82°; the crystallinity is between 4% and 6% when the diffraction angle (2θ) is 28.14°; the crystallinity is between 5% and 7% when the diffraction angle (2θ) is 29.18°; the crystallinity is between 13% and 19% when the diffraction angle (2θ) is 32.02°; the crystallinity is between 7% and 10% when the diffraction angle (2θ) is 33.16°; the crystallinity is between 7% and 10% when the diffraction angle (2θ) is 34.16°; the crystallinity is between 5% and 7% when the diffraction angle (2θ) is 40.10°. When the diffraction angle (2θ) is 42.40°, the crystallinity is between 3% and 4%; when the diffraction angle (2θ) is 46.94°, the crystallinity is between 4% and 6%; when the diffraction angle (2θ) is 48.26°, the crystallinity is between 3% and 5%; when the diffraction angle (2θ) is 49.64°, the crystallinity is between 4% and 6%; when the diffraction angle (2θ) is 51.68°, the crystallinity is between 3% and 5%; when the diffraction angle (2θ) is 53.08°, the crystallinity is between 3% and 5%; when the diffraction angle (2θ) is 63.98°, the crystallinity is between 2% and 3%. The calculation results of the crystallinity of 11 batches of genuine keels are shown in Table 1. Similarly, JADE 9.0 software was used to perform peak search on the spectra of 4 batches of fake keels, 5 batches of fake keels, and 3 batches of fake keels. After analysis and comparison, 8, 13, and 23 common characteristic peaks with greater intensity were selected. Then, peak search was performed on other samples to obtain the peak position value (2θ / °) and diffraction peak intensity (I). The crystallinity of the fake keels was calculated using the formula of crystallinity (1). The calculation results of the crystallinity of 4 batches of fake keels, 5 batches of fake keels, and 3 batches of fake keels are shown in Table 2, Table 3, and Table 4, respectively.

[0070] Table 1 Peak positions and crystallinity of 14 common characteristic peaks of a batch of genuine keels

[0071]

[0072] Table 2 Peak positions and crystallinity of 8 common characteristic peaks of fake keels

[0073]

[0074] Table 3 Peak positions and crystallinity of 13 common characteristic peaks of fake keels

[0075]

[0076] Table 4 Peak positions and crystallinity of 23 common characteristic peaks of fake keels

[0077]

[0078] The authentic keel should be at the angle of the common peak of the characteristic spectrum, and the crystallinity should be within the corresponding range, which is the authentic keel. The peak intensity exceeding or below this range is the counterfeit keel. And through analysis and comparison Figure 8 , Fig. 9 , Fig.10 and Fig.11 , Table 1, Table 2, Table 3 and Table 4 show that genuine keels usually have lower crystallinity, which is manifested as wider diffraction peaks and lower peak intensity. While fake keels usually show sharper and stronger diffraction peaks, and higher crystallinity.

[0079] Based on the above experimental data, the specific identification method of this embodiment is:

[0080] 1. Data collection: XRD is used to test the sample to obtain the diffraction angle (2θ) and peak intensity data.

[0081] 2. Characteristic peak matching determination:

[0082] The diffraction peaks of the sample are matched with the 14 standard characteristic peaks of the genuine keel, and the matching tolerance is set to ±0.2°. A preliminary judgment is made based on the number of matching peaks:

[0083] If the number of matching peaks is less than 7, the sample is directly judged as a fake. If the number of matching peaks is greater than or equal to 7, the sample proceeds to crystallinity determination.

[0084] 3. Calculation and determination of crystallinity:

[0085] The criteria are:

[0086] Any peak crystallinity ≥ 30% → judged as a counterfeit;

[0087] ≥3 characteristic peaks with crystallinity >10% (except 32.02°) → judged as counterfeit;

[0088] 32.02° peak crystallinity ≤ 20%, other peaks ≤ 10% → judged as authentic;

[0089] The crystallinity of individual peaks slightly exceeds 10% (but ≤ 15%) → tends to be genuine, and re-examination is recommended.

[0090] Comprehensive judgment: Combine the characteristic peak matching results with the crystallinity analysis to finally determine whether the sample is genuine or counterfeit.

[0091] Therefore, it can be seen from this embodiment that the present technical solution has the following beneficial effects:

[0092] 1. High precision and high reliability: Based on X-ray powder diffraction (XRPD) technology combined with crystallinity analysis, this invention can simultaneously obtain the sample's phase information and crystal structure integrity, ensuring the scientificity and accuracy of the identification results. Compared with traditional methods, it can not only identify composition differences, but also capture subtle changes in crystal structure, thereby improving the sensitivity of counterfeit identification.

[0093] 2. Combination of qualitative and quantitative analysis: Different from the traditional method that relies on empirical judgment, XRPD technology uses diffraction peak position and intensity for qualitative analysis, while crystallinity calculation provides a quantitative basis. This dual analysis method can effectively reduce human errors and make the identification results more objective and repeatable.

[0094] 3. Non-destructive testing, high sample integrity: This method does not require any chemical treatment of the sample, avoiding sample damage, and is particularly suitable for the testing of precious medicinal materials such as dragon bones. At the same time, sample preparation is simple and fast, and only a small amount of powder is needed to complete the test, which is suitable for rapid screening of large-scale samples.

[0095] 4. Standardized fingerprint database: Through a large number of sample tests, the X-ray diffraction fingerprint database of dragon bones is established, which can be used as a standard reference. Combined with multivariate statistical methods such as principal component analysis (PCA), it can realize automated and batch identification, improve identification efficiency and consistency, and has good prospects for promotion and application.

[0096] 5. Wide applicability: This method is applicable to dragon bone samples of different sources and forms, and is not limited by the physical state of the sample (such as powder, block, etc.). In addition to dragon bones, it can also be applied to the authenticity identification and quality evaluation of other mineral Chinese medicinal materials, and has wide applicability.

[0097] 6. Economical, efficient and easy to promote: The equipment required for XRPD combined with crystallinity analysis is universal, the detection cost is low, and the test speed is fast. It is suitable for routine applications in different fields such as drug supervision, enterprise quality control and scientific research institutions.

[0098] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0099] This article uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the core idea of ​​the present invention. At the same time, for those skilled in the art, according to the idea of ​​the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A method for identifying the authenticity of keels based on X-ray diffraction, characterized in that: include: The keel sample to be tested is tested by an X-ray diffraction method to obtain a diffraction spectrum; the diffraction spectrum includes a plurality of diffraction peaks and corresponding peak intensity data; Extract the diffraction peaks at the set diffraction angle in the diffraction spectrum, match each diffraction peak with the 14 standard characteristic peaks of the genuine keel, and make a preliminary judgment based on the number of successful matches to obtain a preliminary judgment result; the preliminary judgment result includes counterfeits and undetermined products; the set diffraction angle is the diffraction angle corresponding to the standard characteristic peak of the genuine keel; The crystallinity of the sample to be determined is calculated according to the characteristic peak at the set diffraction angle, and the calculated crystallinity is compared with the set judgment standard to obtain the final judgment result.

2. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The X-ray diffraction method is performed using an XRPD instrument, which uses CuKα radiation as the incident light source. The operating voltage of the X-ray tube in the instrument is 40 kV, the current is 40 mA, the aperture system is set to DS=SS=1°, and the scanning range is 3°~65°.

3. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The set diffraction angles include 25.82°, 28.14°, 29.18°, 32.02°, 33.16°, 34.16°, 40.10°, 42.40°, 46.94°, 48.26°, 49.64°, 51.68°, 53.08° and 63.98°.

4. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The successful matching standard of the diffraction peak is: when the matching tolerance between any diffraction peak and the corresponding standard characteristic peak of the genuine keel is within ±0.2°, it is determined to be a successful match.

5. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The preliminary determination based on the number of successful matches specifically includes: When the number of successful matches is less than 7, it is judged as a counterfeit; When the number of successful matches is ≥ 7 peaks, it is determined to be a pending product.

6. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The calculation formula of the crystallinity is:

7. The method for identifying the authenticity of keels based on X-ray diffraction according to claim 1, characterized in that: The step of comparing the calculated crystallinity with the set judgment criteria specifically includes: When the crystallinity of any diffraction peak is ≥30%, it is judged as a counterfeit; When there are more than or equal to 3 diffraction peaks other than 32.02° and the crystallinity is greater than 10%, it is judged as a counterfeit; When the crystallinity of the diffraction peak at 32.02° is ≤20%, and the other diffraction peaks are ≤10%, it is judged to be authentic; When there is a diffraction peak with a crystallinity between 10% and 15%, it is judged to be authentic and a review is recommended.

8. A keel authenticity identification system based on X-ray diffraction, characterized in that: include: A data acquisition unit is used to test the keel sample to be tested by using an X-ray diffraction method to obtain a diffraction spectrum; The diffraction spectrum includes a plurality of diffraction peaks and corresponding peak intensity data; A preliminary determination unit is used to extract the diffraction peaks at the set diffraction angle in the diffraction spectrum, match each diffraction peak with the 14 standard characteristic peaks of the genuine keel, and make a preliminary determination according to the number of successful matches to obtain a preliminary determination result; the preliminary determination result includes counterfeit products and undetermined products; The set diffraction angle is the diffraction angle corresponding to the standard characteristic peak of the genuine keel; The final identification unit is used to calculate the crystallinity corresponding to the product to be determined according to the characteristic peak at the set diffraction angle, and compare the calculated crystallinity with the set judgment standard to obtain the final judgment result.

9. An electronic device, characterized in that: It comprises a memory and a processor, wherein the memory is used to store a computer program, and the processor runs the computer program to enable the electronic device to execute the keel authenticity identification method based on X-ray diffraction according to any one of claims 1-7.

10. A computer-readable storage medium, characterized in that: It stores a computer program, which, when executed by a processor, implements the method for identifying the authenticity of dragon bones based on X-ray diffraction as described in any one of claims 1 to 7.

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