A characteristic chromatogram identification method of a Chinese medicine formula particle of agastache or wine agastache and a preparation method of the Chinese medicine formula particle of agastache or wine agastache

Abstract

The application provides a characteristic spectrum identification method of Chinese medicine formula granules of agastache or wine agastache and a preparation method of Chinese medicine formula granules of agastache or wine agastache, which comprises the following steps: adopting high performance liquid chromatography, taking acetonitrile as mobile phase A, taking 1% acetic acid solution as mobile phase B, performing gradient elution according to the regulations, the flow rate is 1.0 mL per minute, the column temperature is 30 DEG C, and the detection wavelength is 330 nm. In the process of establishing the characteristic spectrum of Chinese medicine formula granules of agastache, 9 common characteristic peaks are confirmed, 7 components are identified, and the relative retention time is studied, so that the chemical composition stability and use safety are ensured. The identification method has the advantages of good stability, high precision, good reproducibility, convenience and easy to master, and the preparation method of the Chinese medicine formula granules is beneficial to improving the identification precision and reproducibility.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine analysis and detection technology, specifically to a method for identifying patchouli or wine-processed patchouli traditional Chinese medicine formula granules using characteristic spectral data, and a method for preparing patchouli or wine-processed patchouli traditional Chinese medicine formula granules. Background Technology

[0002] Patchouli, or Agastache rugosa (Fisch. & C.A.Mey.) Kuntze, is a traditional Chinese herbal medicine widely used to treat summer-heat colds, chest tightness, abdominal pain, vomiting, and diarrhea. Patchouli contains a rich variety of chemical components, mainly terpenes, flavonoids, and phenolic acids. Its pharmacological effects are primarily focused on regulating the digestive system, resisting pathogenic microorganisms, anti-inflammation, and anti-oxidation. In traditional Chinese medicine theory, processing with wine can guide the medicine upwards and correct its odor and taste; therefore, processing with wine enhances the efficacy of patchouli. The specific method involves mixing yellow wine and patchouli in a 20:100 ratio, thoroughly soaking the mixture, placing it in a stir-frying container, stir-frying it over low heat until golden brown, removing it, cooling it, and then processing it into a wine-processed patchouli product.

[0003] CN 115887525 A relates to a method for preparing and detecting a patchouli extract, as well as a method for constructing a characteristic chromatogram. In this method, mobile phase A is a phosphoric acid solution containing 0.08-0.12 wt% phosphoric acid, and mobile phase B is acetonitrile. The resulting characteristic chromatogram has only 5 peaks, which is too few, resulting in less information that can be read, and it cannot identify the wine-processed patchouli.

[0004] The paper "Establishment of Characteristic Spectrum and Determination of Three Components of Jiawei Huoxiang Zhengqi Pill" published by Zhang Yichang, Fan Xiaolei, Song Defang, et al. involves a method for constructing a characteristic spectrum of Jiawei Huoxiang Zhengqi Pill, a quality detection method, and a content determination method. This method uses acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B for gradient elution. Although the method in this literature can obtain more peak information, the baseline is unstable, the information is noisy, the analysis time is long, the characteristic peak missing rate is high, the specificity coverage is incomplete, some medicinal ingredients have no corresponding characteristic peaks, and it also has the problem of not being able to identify the wine-processed agastache.

[0005] In conclusion, it is necessary to further improve and refine the identification methods for patchouli preparations, fill the gap in the identification of wine-processed patchouli preparations, ensure the quality control of patchouli or wine-processed patchouli preparations, provide a reference for clinical drug safety, and provide a basis for the quality evaluation and resource development and utilization of patchouli or wine-processed patchouli preparations. Summary of the Invention

[0006] In view of the problems existing in the prior art, the purpose of this invention is to provide a characteristic chromatographic identification method for patchouli or wine-processed patchouli traditional Chinese medicine formula granules. By using high performance liquid chromatography (HPLC), an identification method for patchouli or wine-processed patchouli traditional Chinese medicine formula granules and other types of preparations such as decoction pieces has been established. It has the characteristics of good stability, high precision, good reproducibility, convenience and ease of use.

[0007] Another objective of this invention is to provide a method for preparing granules of agastache or wine-processed agastache in traditional Chinese medicine formulations. The preparation method provided by this invention is beneficial to improving the accuracy of characteristic chromatogram identification and is highly compatible with the identification method provided by this invention.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A characteristic chromatographic identification method for a traditional Chinese medicine formula granule containing patchouli or wine-processed patchouli, including: A) The test sample is dissolved in methanol and extracted to obtain the test solution. The test sample is a traditional Chinese medicine formula granule of patchouli or wine-processed patchouli. B) The test solution was analyzed by high performance liquid chromatography to obtain the characteristic chromatogram of the test sample; C) The chromatographic peak with a relative retention time of 1.41 was used as the distinguishing point between patchouli preparations and wine-based patchouli preparations. The use of a chromatographic peak with a relative retention time of 1.41 as the identification point between patchouli and wine-processed patchouli traditional Chinese medicine formula granules means that if a chromatographic peak with a relative retention time of 1.41 is present in the characteristic chromatogram of the test sample preparation, it is identified as patchouli traditional Chinese medicine formula granules; if it is not present, it is identified as wine-processed patchouli traditional Chinese medicine formula granules. The chromatographic conditions for the high performance liquid chromatography method are as follows: the chromatographic column is a C18 column; mobile phase A is acetonitrile, mobile phase B is 1% acetic acid solution, and gradient elution is used. The gradient elution specifically refers to: 0–9 min, Phase A: 22% → 28%, Phase B: 78% → 72%; 9–14 min, Phase A: 28% → 30%, Phase B: 72% → 70%; 14–20 min, Phase A: 30% → 37%, Phase B: 70% → 63%; 20–35 min, Phase A: 37% → 75%, Phase B: 63% → 25%.

[0009] According to the present invention, unless otherwise specified, "%" as used herein refers to volume percentage.

[0010] The inventors of this application discovered in their research that the above-mentioned determination method is beneficial for obtaining more effective chromatographic peaks, and the chromatographic peak baselines are stable and highly repeatable.

[0011] According to the present invention, the chromatographic peak with a relative retention time of 1.41 is peak 8 in the characteristic spectrum of patchouli. The similarity of the characteristic spectra of patchouli or its wine-processed preparations is evaluated using a similarity evaluation system for chromatographic fingerprints of traditional Chinese medicine. If the test sample is patchouli, a standard characteristic spectrum including 9 characteristic peaks is obtained. The peak corresponding to the reference peak of citronellol is peak S. The relative retention times of peaks 3-4, 6-9, and peak S are within ±10% of a specified value, where the specified values ​​are: 0.31 (peak 3), 0.58 (peak 4), 0.58 (peak 5), and 0.58 (peak 6). 4) 1.25 (peak 6), 1.31 (peak 7), 1.41 (peak 8), 1.65 (peak 9); If the test sample is *Pogostemon cablin*, a standard characteristic spectrum including 8 characteristic peaks is obtained, and the peak corresponding to the reference peak of piperidin is the S peak. The relative retention times of peaks 3-4, 6, 7 and 9 with the S peak are within ±10% of the specified values, where the specified values ​​are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), 1.65 (peak 8).

[0012] In some specific embodiments of the present invention, the peak trend of the citronella reference compound is used as a distinguishing point between the traditional Chinese medicine formula granules of patchouli and those made with wine.

[0013] In some specific embodiments of the present invention, the peak trend of the citronellol reference reference refers to the fact that, compared with the citronellol herbal formula granules, the peak area of ​​the citronellol herbal formula granules shows a decreasing trend. Therefore, compared with the characteristic spectrum of the identified citronellol herbal formula granules, if the peak area of ​​the citronellol reference reference peak of the test sample is smaller, it is identified as the citronellol herbal formula granules; otherwise, it is identified as the citronellol herbal formula granules.

[0014] According to the present invention, in principle, the chromatographic peak with a relative retention time of 1.41 is used as the identification point for the traditional Chinese medicine formula granules of patchouli and wine patchouli, which is consistent with the identification result of the peak trend of the reference glutenin.

[0015] According to the present invention, if the identification result of the chromatographic peak with a relative retention time of 1.41 as the identification point of the traditional Chinese medicine formula granules of patchouli and wine patchouli is inconsistent with the identification result of the peak trend of the reference compound citrinin, then the result of the chromatographic peak with a relative retention time of 1.41 as the identification point of the traditional Chinese medicine formula granules of patchouli and wine patchouli shall be taken as the standard.

[0016] In some specific embodiments of the present invention, the preparation of a reference solution is also included: chlorogenic acid reference standard, neochlorogenic acid reference standard, rosmarinic acid reference standard, caffeic acid reference standard, piracetamine reference standard, apigenin reference standard, and acacia glycoside reference standard are respectively dissolved in methanol to obtain a reference solution. The reference solution was analyzed by high performance liquid chromatography to obtain a chromatogram of the reference solution; and the components of the patchouli or wine-processed patchouli were identified based on the chromatogram of the reference solution.

[0017] In some specific embodiments of the present invention, the concentration of the reference solution is specifically 10~30 μg / mL, preferably 15~25 μg / mL; more preferably 25 μg / mL.

[0018] According to the present invention, when the concentration of the reference solution is within the above-mentioned range, it is advantageous to match the concentration of the test sample, thereby meeting the detection sensitivity requirements.

[0019] In some specific embodiments of the present invention, the chromatographic column is a C18 4.6×250mm 5μm column; the column temperature is 25℃~35℃, preferably 28℃~32℃, more preferably 30℃; the theoretical plate number calculated based on the citronellol peak should not be less than 5000.

[0020] According to the present invention, the chromatographic column conditions at 30°C are closer to the conventional room temperature, the column temperature is stable and easy to control, and the differences in the distribution behavior of different components on the stationary phase are more obvious, thereby improving the separation effect of characteristic peaks.

[0021] In some specific embodiments of the present invention, the flow rate of the mobile phase is 0.5 mL / min to 2 mL / min, preferably 0.8 mL / min to 1.5 mL / min, more preferably 0.9 mL / min to 1.2 mL / min, and even more preferably 1 mL / min; the injection volume is 5 to 15 μL, preferably 7 to 12 μL, and more preferably 10 μL.

[0022] According to the present invention, when the mobile phase flow rate and injection volume are within the above range, the resolution and peak shape are better, and the sensitivity and precision can be balanced. It is versatile and easy to operate.

[0023] In some specific embodiments of the present invention, the detection wavelength is 250nm~400nm, preferably 300nm~350nm, and more preferably 330nm.

[0024] According to the present invention, when the detection wavelength is within the above range, there is strong ultraviolet absorption and a large response signal, which can ensure that the characteristic spectrum has sufficient detection sensitivity to meet the quantitative requirements, and can significantly reduce background interference, reduce baseline noise, and make the measurement results more stable.

[0025] In some specific embodiments of the present invention, in step A), the extraction is ultrasonic extraction; the power of the ultrasound is 400W~800W, preferably 500W~700W, more preferably 550W~650W; the frequency is 10kHz~80kHz, preferably 20kHz~60kHz, more preferably 30kHz~50kHz; and the time is 10min~30min, preferably 15min~25min, more preferably 20min.

[0026] According to the present invention, when the ultrasonic conditions are within the above range, it is beneficial to obtain more chromatographic peaks, and the chromatographic peak baselines are stable and highly repeatable.

[0027] In some specific embodiments of the present invention, in step A), the ratio of the mass (g) of the test sample preparation to the volume (mL) of methanol is (0.1~1):10, preferably (0.1~0.5):10, more preferably 0.3:10; preferably, the sample weight of the test sample preparation is 0.3g, more preferably, the amount of methanol used relative to 0.3g of the test sample preparation is 5mL~15mL, more preferably 10mL.

[0028] According to the present invention, when the concentration of the test sample raw material is within the above range, it is beneficial to obtain more chromatographic peaks, and the chromatographic peak baseline is stable and has strong repeatability.

[0029] In some specific embodiments of the present invention, the identification results of the characteristic spectrum of the patchouli preparation include: peak 1: neochlorogenic acid; peak 2: chlorogenic acid; peak 3: caffeic acid; peak 4: rosmarinic acid; peak 5(S): citric acid; peak 6: apigenin; peak 9: acaciain.

[0030] In some specific embodiments of the present invention, the identification results of the characteristic spectrum of the herbal formula granules of *Pogostemon cablin* include: Peak 1: Neochlorogenic acid; Peak 2: Chlorogenic acid; Peak 3: Caffeic acid; Peak 4: Rosmarinic acid; Peak 5(S): Cirsium glycoside; Peak 6: Apigenin; Peak 8: Acacia glycoside.

[0031] A method for identifying the characteristic chromatogram of a patchouli or wine-processed patchouli preparation, characterized in that the above-mentioned method is used for detection and the detection results are analyzed, wherein the preparation form includes one or more of the following: medicinal materials, standard decoctions, and processed medicinal slices.

[0032] The quality judgment standard of this method is based on chlorogenic acid reference standard, neochlorogenic acid reference standard, rosmarinic acid reference standard, caffeic acid reference standard, piracetamine reference standard, apigenin reference standard, and fenestrated ginseng reference standard as references. The peak corresponding to the peak of the piracetamine reference standard is taken as the S peak. The relative retention time of each characteristic peak and the S peak is calculated, and it is stipulated that the relative retention time should be within ±10% of the specified value.

[0033] The specific quality judgment criteria are as follows: Take a sample of patchouli preparation, operate according to the same method as above, and obtain a characteristic chromatogram. The chromatogram of the test sample should show 9 characteristic peaks, which should correspond to the retention times of 7 characteristic peaks in the reference chromatogram of the reference medicinal material, namely chlorogenic acid reference standard, neochlorogenic acid reference standard, rosmarinic acid reference standard, caffeic acid reference standard, citronellol reference standard, apigenin reference standard, and acacia glycoside reference standard. The peak corresponding to the citronellol reference standard peak is the S peak. Calculate the relative retention times of peaks 3-4 and peaks 6-9 with the S peak. The relative retention times should all be within ±10% of the specified values, which are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), 1.41 (peak 8), and 1.65 (peak 9).

[0034] The specific quality judgment criteria are as follows: Take a sample of the *Pogostemon cablin* preparation, operate according to the same method described above, and obtain a characteristic chromatogram. The chromatogram of the test sample should show 8 characteristic peaks, which should correspond to the retention times of 7 characteristic peaks in the reference chromatogram of the reference medicinal material, namely chlorogenic acid, neochlorogenic acid, rosmarinic acid, caffeic acid, citronellol, apigenin, and acacia. The peak corresponding to the citronellol reference peak is the S peak. Calculate the relative retention times of peaks 3-4, 6, 7, and 9 with the S peak. The relative retention times should all be within ±10% of the specified values, which are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), and 1.65 (peak 8).

[0035] A method for preparing a traditional Chinese medicine formula granule containing patchouli or wine-processed patchouli, or the aforementioned traditional Chinese medicine formula granule containing patchouli or wine-processed patchouli, comprising: (1) Take agastache rugosa, remove impurities, wash, cut into sections, and dry to obtain agastache rugosa slices; (2) Take 600g of the agastache slices obtained in step (1), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, boil, and keep simmering for 20 minutes. For the second decoction, add 10 times the amount of water, boil, and keep simmering for 15 minutes. During the decoction process, the temperature is controlled at 94-100℃. Combine the water extracts. (3) The aqueous extract obtained in step (2) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated patchouli extract; (4) The concentrated agastache obtained in step (3) was spray-dried under the conditions of an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (5) Take 7.5 to 10.0 parts of the dried agastache powder from step (4), add 0.0 to 2.5 parts of maltodextrin, mix well, and perform dry granulation to obtain agastache medicinal formula granules; or (i) Take agastache rugosa, remove impurities, wash, cut into sections, and dry to obtain agastache rugosa slices; (ii) Take 400g of the agastache slices obtained in step (i), add rice wine and mix well according to the wine-processing method (General Chapter 0213 of Chinese Pharmacopoeia 2025 Edition) (the mass ratio of rice wine to agastache slices is 1:15); let it soak thoroughly, place it in a stir-frying container, and stir-fry at a temperature of 120-150℃ for 8-10 minutes. During the stir-frying process, the properties of the material need to be observed at all times. Stir-fry until dry, remove the material, spread it out to cool, and obtain wine-processed agastache slices. (iii) Take 350g of the wine-processed agastache slices obtained in step (ii), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, bring to a boil, and simmer for 20 minutes. For the second decoction, add 10 times the amount of water, bring to a boil, and simmer for 15 minutes. During the decoction process, the temperature should be controlled at 94-100℃. Combine the water extracts. (iv) The aqueous extract obtained in step (iii) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated extract of patchouli. (v) The concentrated agastache obtained in step (iv) is spray-dried under an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (vi) Take 7.1 to 10.0 parts of the dried agastache powder from step (v), add 0.0 to 2.9 parts of maltodextrin, mix well, and perform dry granulation to obtain agastache medicinal formula granules.

[0036] The beneficial effects of this invention are at least in the following aspects: Firstly, this invention is the first to establish a characteristic chromatographic method for distinguishing between patchouli granules and wine-processed patchouli granules using high-performance liquid chromatography (HPLC). This method identifies nine characteristic peaks as the distinguishing points between patchouli granules and wine-processed patchouli granules, enabling effective differentiation between them.

[0037] Secondly, in the process of establishing the characteristic spectrum of the patchouli Chinese medicine formula granules, this invention identified 9 common characteristic peaks, identified 7 components, and studied their relative retention times, thus ensuring the stability of its chemical composition and the safety of its use.

[0038] Third, the method of the present invention has good stability, high precision, good reproducibility, and is convenient and easy to master. Attached Figure Description

[0039] Figure 1 These are chromatograms of different wavelengths of the herbal formula granules containing patchouli.

[0040] Figure 2 This is the result of the investigation of the mobile phase.

[0041] Figure 3 This is the result of the investigation on the concentration of the mobile phase.

[0042] Figure 4 These are the results of investigations at different column temperatures and flow rates.

[0043] Figure 5 This is a result of delayed investigation.

[0044] Figure 6 This is the result of the extraction method examination.

[0045] Figure 7 This is the result of the investigation on the extraction solvent.

[0046] Figure 8 This refers to the results of the sample size survey.

[0047] Figure 9 This is a chromatographic peak identification diagram of the herbal formula granules containing patchouli.

[0048] Figure 10 This is the result of the specificity assessment.

[0049] Figure 11 This is the spectrum of piracetam.

[0050] Figure 12 It is particulate spectroscopy - piracetaminoside.

[0051] Figure 13 This is an intermediate precision chromatogram.

[0052] Figure 14 This is a test of column durability.

[0053] Figure 15 This is a characteristic spectrum of patchouli granules.

[0054] Figure 16 This is a characteristic spectrum of Huoxiang granules.

[0055] Figure 17 This is a characteristic spectrum of patchouli granules.

[0056] Figure 18 This is a comparison of the characteristic spectra of patchouli and wine-processed patchouli.

[0057] Figure 19 This is the feature map of Comparative Example 1.

[0058] Figure 20 This is the feature map of Comparative Example 2.

[0059] Figure 21 This is the feature map of Comparative Example 3.

[0060] Figure 22 This is the feature map of Comparative Example 4. Detailed Implementation

[0061] This invention provides a method for constructing characteristic spectra of patchouli or wine-processed patchouli preparations. Those skilled in the art can refer to the content of this document and appropriately modify the process parameters to achieve the desired result. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and fall within the scope of protection of this invention. The method and application of this invention have been described through preferred embodiments. Those skilled in the art can clearly modify or appropriately change and combine the method and application described herein without departing from the content, spirit, and scope of this invention to realize and apply the technology of this invention.

[0062] The present invention will be described in detail below through embodiments, but the scope of protection of the present invention is not limited to the following description.

[0063] Unless otherwise specified in the examples, the conditions shall be performed under conventional conditions or conditions recommended by the manufacturer. Raw materials, reagents, or instruments whose manufacturers are not specified are all commercially available products or prepared according to publicly disclosed methods.

[0064] The experimental instruments and materials used in the following embodiments are as follows: High performance liquid chromatograph: Waters E2695; Electronic balances: ME204E / 02, MS205DU, XP26 (Mettler-Toledo Instruments Ltd.); Ultrapure water system: Cellular type 1810A (Shanghai Moler Scientific Instruments Co., Ltd.); Ultrasonic cleaner: KQ-600DB model (600W, 40KHz; Kunshan Ultrasonic Instrument Co., Ltd.); Column: Agilent 5 TC-C18(2), 4.6 mm × 250 mm, 5 μm; Column: XBridge® C18, 4.6 mm × 250 mm, 5 μm; Column: ZORBAX SB-Aq, 4.6 mm × 250 mm, 5 μm; Acetonitrile, phosphoric acid, formic acid, and acetic acid were of chromatographic grade, water was ultrapure water, and all other reagents were of analytical grade.

[0065] Chlorogenic acid (China National Institutes for Food and Drug Control, batch number: 110753-202119, purity: 96.3%). Neochlorogenic acid (Chengdu Pusi Biotechnology Co., Ltd., batch number: PS020999, purity: 99.72%). Caffeic acid (China National Institutes for Food and Drug Control, batch number: 110885-201703, purity: 99.7%). Rosmarinic acid (China National Institutes for Food and Drug Control, batch number: 111871-201505, purity: 98.5%). Thistle glycoside (Sichuan Weikeqi Biotechnology Co., Ltd., batch number: wkq21071504, purity: 98.68%) Apigenin (China National Institutes for Food and Drug Control, batch number: 111901-202205, purity: 98.4%). Acacia extract (Chengdu Mansite Biotechnology Co., Ltd., batch number: MUST-19081008, purity: 99.07%).

[0066] The batch number of the herbal formula granules of patchouli is 2212021. Its preparation method is as follows: (1) Take patchouli, remove impurities, wash, cut into sections, and dry to obtain patchouli slices; (2) Take 600g of the agastache slices obtained in step (1), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, boil, and keep simmering for 20 minutes. For the second decoction, add 10 times the amount of water, boil, and keep simmering for 15 minutes. During the decoction process, the temperature is controlled at 94-100℃. Combine the water extracts. (3) The aqueous extract obtained in step (2) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated patchouli extract; (4) The concentrated agastache obtained in step (3) was spray-dried under the conditions of an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (5) Take the dried patchouli powder from step (4), add 1%-3% maltodextrin, mix well, and perform dry granulation to obtain patchouli formula granules.

[0067] The batch number of the herbal formula granules containing agastache is 2508001. The preparation method of the herbal formula granules containing agastache is as follows: (i) Take agastache, remove impurities, wash, cut into sections, and dry to obtain agastache slices. (ii) Take 400g of the agastache slices obtained in step (i), add rice wine and mix well according to the wine-processing method (General Chapter 0213 of Chinese Pharmacopoeia 2025 Edition) (the mass ratio of rice wine to agastache slices is 1:15); let it soak thoroughly, place it in a stir-frying container, and stir-fry at a temperature of 120-150℃ for 8-10 minutes. During the stir-frying process, the properties of the material need to be observed at all times. Stir-fry until dry, remove the material, spread it out to cool, and obtain wine-processed agastache slices. (iii) Take 350g of the wine-processed agastache slices obtained in step (ii), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, bring to a boil, and simmer for 20 minutes. For the second decoction, add 10 times the amount of water, bring to a boil, and simmer for 15 minutes. During the decoction process, the temperature should be controlled at 94-100℃. Combine the water extracts. (iv) The aqueous extract obtained in step (iii) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated extract of patchouli. (v) The concentrated agastache obtained in step (iv) is spray-dried under an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (vi) Take the dried agastache powder from step (v), add 1%-3% maltodextrin, mix well, and perform dry granulation to obtain agastache formula granules; according to the above method, select different batches of medicinal materials to prepare different batches of products.

[0068] Example 1: Method for Determining Characteristic Spectra Chromatographic conditions and system suitability tests were conducted using octadecylsilane-bonded silica gel as the packing material; acetonitrile as mobile phase A and 1% acetic acid solution as mobile phase B, with gradient elution performed according to the specifications in Table 1; the flow rate was 1.0 mL per minute; the column temperature was 30℃; the detection wavelength was 330 nm; and the theoretical plate number, calculated based on the piracetam glycoside peak, should not be less than 5000.

[0069] Table 1 Chromatographic conditions

[0070] Preparation of reference solution: Take an appropriate amount of piracetamine reference standard, accurately weigh it, and add methanol to prepare a solution containing 20 μg per 1 mL, which is used as the reference solution.

[0071] Preparation of the test solution: Take an appropriate amount of this product, grind it into a fine powder, take about 0.3g, weigh it accurately, place it in a stoppered conical flask, accurately add 10ml of methanol, stopper tightly, weigh it, sonicate (power 600W, frequency 40kHz) for 20 minutes, cool it, weigh it again, make up the weight loss with methanol, shake well, filter it, and take the filtrate to obtain the test solution.

[0072] The determination method involves precisely pipetting 10 μl of the reference solution and the test solution into the liquid chromatograph and measuring the results.

[0073] 1. Chromatographic conditions and system suitability test 1.1 Wavelength Selection Based on the above-planned experimental conditions, a diode array detector was used to perform a full-band scan of the test solution, and chromatograms of the test solution at wavelengths of 260 nm, 300 nm, and 330 nm were extracted. See... Figure 1 .

[0074] The results show that, under the experimental conditions of this invention, the wavelength of 330 nm provides a greater amount of chromatographic peak information and a more stable chromatographic baseline. Changing the wavelength will lead to a decrease in baseline stability, thus confirming the beneficial effect of this invention on wavelength selection.

[0075] 1.2 Wavelength Selection Based on the above-established experimental conditions, investigations were conducted on mobile phases of acetonitrile-1% phosphoric acid, acetonitrile-1% formic acid, and acetonitrile-1% acetic acid. The results are shown below. Figure 2 .

[0076] The results show that the sample has a better peak shape in the mobile phase of acetonitrile-1% acetic acid, and changing the mobile phase will not achieve the same technical effect as the present invention.

[0077] 1.3 Investigation of mobile phase concentration Based on the above-established experimental conditions, the concentration of mobile phase B was investigated using 0.1% acetic acid, 0.5% acetic acid, and 1% acetic acid solutions, respectively. The results are shown below. Figure 3 .

[0078] The results showed that the chromatogram peaks were relatively symmetrical only when the mobile phase B was a 1% acetic acid solution.

[0079] 1.4 Column Temperature and Flow Rate Investigation Based on the above-specified experimental conditions, the column temperature and flow rate were investigated, and the results are shown in the table below. Figure 4 .

[0080] Based on the analysis of the combined flow rate and column temperature results, the chromatogram peak shape was better and the baseline was more stable when the flow rate was 1.0 mL / min and the column temperature was 30℃. Other flow rates and column temperatures could not achieve the same technical effect as the present invention.

[0081] 1.5 Delayed Examination Based on the above-specified experimental conditions, a delay test was conducted. The results are shown below. Figure 5 .

[0082] The results showed that the sample had virtually no chromatographic peaks after 35 minutes, so the sample detection time was set at 35 minutes.

[0083] 1.6 Examination of Extraction Methods Take an appropriate amount of this product (Agastache rugosa granules), grind it into a fine powder, accurately weigh about 0.1g, place it in a stoppered conical flask, accurately add 10ml of methanol, seal tightly, weigh, and then sonicate (600W power, 40kHz frequency) and reflux for 20 minutes. Cool, weigh again, and replenish the lost weight with methanol. Shake well, filter, and collect the filtrate. See [link to product description]. Figure 6 .

[0084] The results showed that ultrasonic extraction and reflux extraction yielded consistent results for the test sample. Since ultrasonic extraction is simpler, it was chosen as the extraction method for the test sample.

[0085] 1.7 Investigation of Extraction Solvents Take an appropriate amount of this product (Agastache rugosa granules), grind it into a fine powder, take 0.1g, place it in a stoppered conical flask, add 10ml each of 30% methanol, 50% methanol, 80% methanol, and methanol, seal tightly, weigh, and sonicate (600W power, 40kHz frequency) for 20 minutes. Cool, weigh again, replenish the lost weight with the appropriate solvent, shake well, filter, and collect the filtrate. See [link to product description]. Figure 7 .

[0086] The results show that when methanol is used as the extraction solvent, the amount of chromatographic peak information is large and the chromatographic peak shape is good. Other concentrations of methanol solutions cannot achieve the same technical effect as the present invention.

[0087] 1.8 Sample Quantity Assessment Take an appropriate amount of this product (Agastache rugosa granules), grind it into a fine powder, and take 0.1g, 0.3g, and 0.5g respectively. Place them in a stoppered conical flask, add 10ml of methanol, seal tightly, weigh, and sonicate (600W power, 40kHz frequency) for 20 minutes. Cool, weigh again, and replenish the lost weight with methanol. Shake well, filter, and collect the filtrate. See [link to product description]. Figure 8 .

[0088] The results above show that the sample weight has no effect on the peak shape, and 0.3g was finally selected as the sample weight.

[0089] 2. Methodological Investigation 2.1 Chromatographic Peak Identification Preparation of the test solution: Prepare the test solution of the patchouli Chinese herbal medicine formula granules according to the experimental conditions proposed above.

[0090] Preparation of reference solutions: Take appropriate amounts of chlorogenic acid, neochlorogenic acid, rosmarinic acid, caffeic acid, piracetam, apigenin, and acetoxin reference standards respectively, accurately weigh them, and add methanol to prepare solutions containing 20 μg of each per ml, which are used as reference solutions.

[0091] The characteristic spectral peaks of the herbal formula granules containing patchouli were located, see [link / reference needed]. Figure 9 .

[0092] Depend on Figure 9 It can be seen that the test solution showed 8 peaks: peak 1 was neochlorogenic acid; peak 2 was chlorogenic acid; peak 3 was caffeic acid; peak 4 was rosmarinic acid; peak 5 was piracetaminoside; peak 6 was apigenin; and peak 9 was farnesin.

[0093] 2.2 Specificity Experiment Take the herbal formula granules of patchouli and prepare the test solution according to the method for preparing the test solution described in the characteristic spectrum determination method of Example 1 above.

[0094] Take maltodextrin and prepare a negative control solution according to the method for preparing the test solution described in the characteristic spectrum determination method of Example 1 above.

[0095] Take the piracetamine reference standard and prepare the reference solution according to the method for preparing the reference solution described in the characteristic spectrum determination method of Example 1 above.

[0096] Accurately pipette 10 µL each of the piperazine reference solution, negative control solution, and test solution into the liquid chromatograph, and determine the chromatographic conditions as described in the characteristic chromatogram determination method of Example 1. Results are shown below. Figure 10 .Depend on Figure 10 It can be seen that the characteristic curve of the patchouli herbal formula granules contains 9 chromatographic peaks (peaks 1, 2, 3, 4, 5, 6, 7, 8, and 9). Among them, the chromatographic peak of the citrinin reference standard corresponds to peak 5 in the characteristic curve of the patchouli herbal formula granules, and the spectrum is similar. Figure 1 To, see Figure 11-12 In addition, the negative control showed no interference.

[0097] 2.3 Precision Test Prepare one sample solution according to the proposed experimental method, inject it six times consecutively, and calculate the retention time of each characteristic peak. See Table 2.

[0098] Table 2 Precision test - retention time

[0099] The results showed that the RSD of the retention time of each characteristic peak in the precision study was 0.03% to 0.15%, indicating that the method had good precision.

[0100] 2.4 Repeatability Test Six test solutions were prepared according to the proposed experimental method, and the relative retention times of each characteristic peak were measured and calculated. See Table 3.

[0101] Table 3 Repeatability test - relative retention time ratio

[0102] The results show that the RSD of the relative retention time of the characteristic peak is between 0.00% and 0.15%, and the method has good repeatability.

[0103] 2.5 Intermediate Precision Examination Based on the above-planned experimental conditions, two portions of the Huo Xiang herbal formula granules were accurately weighed by different personnel (A1, A2) at different times (T1, T2) to prepare test solutions. These solutions were then analyzed using high-performance liquid chromatography (HPLC) on instruments of the same model but different serial numbers (C1: Waters022, C2: Waters023). See [link / details]. Figure 13 Table 4.

[0104] Table 4 Intermediate Precision Study - Relative Retention Time Ratio

[0105] The results showed that when the test solution was prepared by different personnel at different times and measured on different instruments, the RSD of the relative retention time of each characteristic peak was 0.00%-0.24%. Different instruments had little effect on the relative retention time of the characteristic peaks, and the method had good intermediate precision.

[0106] 2.6 Column robustness test The same test sample was investigated using three different C18 columns. See Table 5. Figure 14 .

[0107] Table 5. Column robustness study - relative retention time

[0108] As shown in the figure above, different chromatographic columns exhibit peak drift, resulting in a wide range of RSDs for the relative retention times of the remaining characteristic peaks, from 0.00% to 13.58%. However, the number and shape of the characteristic peaks remain unchanged, indicating that the column has good robustness.

[0109] 2.7 Stability Prepare a test solution according to the experimental conditions outlined above, and measure the results at 0h, 3h, 6h, 9h, 15h, and 24h. See Table 6.

[0110] Table 6 Stability Study - Retention Time

[0111] The results showed that the RSD of the corresponding characteristic peak retention time was 0.05-0.49%, and the sample solution was stable within 24 hours.

[0112] 3. Verification of the characteristic spectrum of patchouli granules The Huoxiang Granules were inspected, and the retention times were calculated. The results are shown in Figure 15 , Table 7.

[0113] Table 7 Characteristic Chromatogram of Huoxiang Granules - Relative Retention Time

[0114] According to the principle of stable retention time, all batches of samples can be detected, and the peaks are relatively high, a total of 9 peaks with good repeatability were selected as characteristic peaks.

[0115] According to the principle of stable relative retention time, all batches of samples can be detected, and the peaks are relatively high, a total of 9 peaks with good durability, namely Peak 1, Peak 2, Peak 3, Peak 4, Peak 5, Peak 6, Peak 7, Peak 8, and Peak 9, were selected as characteristic peaks. Since the relative retention times of Peak 1 and Peak 2 are relatively small and the specified value range is relatively narrow, reference substances of reference standards were used for the determination of Peak 1 and Peak 2. The relative retention times of the remaining characteristic peaks are stable and within the range of the average value ± 10%. The RSD values of the relative retention times of each characteristic peak are relatively small. Therefore, only the specified values of the relative retention times are considered, and the specified value range of the relative retention time of each peak is tentatively set at ± 10%.

[0116] Using the Similarity Evaluation System for Traditional Chinese Medicine Chromatographic Fingerprints (2012 Edition), 4 batches of Huoxiang Granules were synthesized to establish a reference characteristic chromatogram of the characteristic chromatogram of Huoxiang Granules. See Figure 16 .

[0117] Verification of the Characteristic Chromatogram of Wine-processed Huoxiang Granules The Wine-processed Huoxiang Granules were inspected, and the retention times were calculated. The results are shown in Figure 17 , Table 8.

[0118] Table 8 Characteristic Chromatogram of Wine-processed Huoxiang Granules - Relative Retention Time

[0119] According to the present invention, in the characteristic chromatogram of the Wine-processed Huoxiang Granules, the peak at a relative retention time of 1.65 is named Peak No. 8 in the re-numbering order, without following the naming method of the peak at a relative retention time of 1.65 in the characteristic chromatogram of the Huoxiang Granules, and it is named Peak No. 9.

[0120] Comparison of the characteristic chromatograms of Huoxiang Granules and Wine-processed Huoxiang Granules is shown in Figure 18 .

[0121] The final specification stipulates that the chromatogram of the patchouli herbal formula granules should show 9 characteristic peaks. The peak corresponding to the reference peak of piracetam is designated as peak S (peak 5). The relative retention times of peaks 3-4, 6-9, and peak S should be calculated and should be within ±10% of the specified values. The specified values ​​are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), 1.41 (peak 8), and 1.65 (peak 9).

[0122] The results showed that only 8 chromatographic peaks with good stability and repeatability could be detected in the granules of the herbal formula of *Pogostemon cablin*. Among them, the 8 peaks that could be detected in the *Pogostemon cablin* granules, that is, the peaks with a relative retention time of 1.27, were all obvious and well separated. However, no obvious chromatographic peaks were detected in the granules of the herbal formula of *Pogostemon cablin*.

[0123] Meanwhile, compared with the processed product granules, the peak area of ​​the processed product generally showed a decreasing trend. In conclusion, the chromatographic peak with a relative retention time of 1.27 and the trend of the S peak can both be used as identification points for the traditional Chinese medicine formula granules of patchouli and wine-processed patchouli, which is of great significance for studying the identification of the authenticity of patchouli and wine-processed patchouli granules.

[0124] Comparative Examples 1-4 The results were essentially the same as in Example 1, except that elution was performed according to the elution conditions listed in Table 9 (Comparative Example 1), Table 10 (Comparative Example 2), Table 11 (Comparative Example 3), and Table 12 (Comparative Example 4), respectively. The results are shown in the table below. Figure 19-22 This indicates that the elution procedure in Example 1 provides richer chromatographic peak information, optimal peak resolution, and a more stable baseline.

[0125] Table 9 Gradient elution conditions

[0126] Table 10 Gradient elution conditions

[0127] Table 11 Gradient elution conditions

[0128] Table 12 Gradient elution conditions

[0129] Based on the comparison between this application and Comparative Examples 1-4, it can be seen that the gradient elution time in this application is shorter, which is significantly better than that in Examples 1-4. At the same time, the mobile phase ratio is gradually adjusted according to the elution ability of different polar components, so that multiple components such as araliain, rosmarinic acid, and araliain can be well separated, with sharp peaks and no obvious tailing. It also avoids the difficulty of eluting certain components, residual contamination, or baseline drift under isocratic elution, making the baseline more stable and the interference of impurities less.

[0130] It should be noted that the embodiments described above are only for explaining the present invention and do not constitute any limitation on the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to the present invention within the scope of the claims, and revisions can be made to the present invention without departing from the scope and spirit of the present invention. Although the present invention described herein relates to specific methods, materials, and embodiments, it does not mean that the present invention is limited to the specific examples disclosed herein; on the contrary, the present invention can be extended to all other methods and applications with the same function.

[0131] It should be noted that the endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

Claims

1. A method for identifying the characteristic chromatograms of agastache or wine-processed agastache granules in a traditional Chinese medicine formula, comprising: A) The test sample is dissolved in methanol and extracted to obtain the test solution. The test sample is a traditional Chinese medicine formula granule of patchouli or wine-processed patchouli. B) The test solution was analyzed by high performance liquid chromatography to obtain the characteristic chromatogram of the test sample; C) The chromatographic peak with a relative retention time of 1.41 was used as the identification point between patchouli and wine-processed patchouli granules in traditional Chinese medicine formulas. The use of a chromatographic peak with a relative retention time of 1.41 as the identification point between patchouli and wine-processed patchouli traditional Chinese medicine formula granules means that if a chromatographic peak with a relative retention time of 1.41 is present in the characteristic chromatogram of the test sample preparation, it is identified as patchouli traditional Chinese medicine formula granules; if it is not present, it is identified as wine-processed patchouli traditional Chinese medicine formula granules. The chromatographic conditions for the high performance liquid chromatography method are as follows: the chromatographic column is a C18 column; mobile phase A is acetonitrile, mobile phase B is 1% acetic acid solution, and gradient elution is used. The gradient elution specifically refers to: 0–9 min, Phase A: 22% → 28%, Phase B: 78% → 72%; 9–14 min, Phase A: 28% → 30%, Phase B: 72% → 70%; 14–20 min, Phase A: 30% → 37%, Phase B: 70% → 63%; 20–35 min, Phase A: 37% → 75%, Phase B: 63% → 25%.

2. The method according to claim 1, characterized in that, The peak trend of the citronellol reference granule is used as a distinguishing point between agastache and wine-processed agastache granules. Preferably, the peak trend of the citronellol reference granule indicates that the peak area of ​​the wine-processed agastache granules decreases compared to the agastache granules. Therefore, if the peak area of ​​the citronellol reference granule in the test sample is smaller than that in the characteristic spectrum of the identified agastache granules, it is identified as wine-processed agastache granules; otherwise, it is identified as agastache granules.

3. The method according to claim 2, characterized in that, It also includes the preparation of reference solutions: chlorogenic acid reference standard, neochlorogenic acid reference standard, rosmarinic acid reference standard, caffeic acid reference standard, piracetamine reference standard, apigenin reference standard, and acacia glycoside reference standard are respectively dissolved in methanol to obtain reference solution; The reference solution was analyzed by high performance liquid chromatography to obtain a chromatogram of the reference solution; and the components of the patchouli or wine-processed patchouli were identified based on the chromatogram of the reference solution. Preferably, the concentration of the reference solution is 10~30 μg / mL, more preferably 15~25 μg / mL; and more preferably 25 μg / mL.

4. The method according to any one of claims 1-3, characterized in that, The chromatographic column is a C18 4.6×250mm 5μm column; the column temperature is 25℃~35℃, preferably 28℃~32℃, more preferably 30℃; the theoretical plate number calculated based on the citronellol peak should be no less than 5000; and / or The flow rate of the mobile phase is 0.5 mL / min to 2 mL / min, preferably 0.8 mL / min to 1.5 mL / min, more preferably 0.9 mL / min to 1.2 mL / min, and even more preferably 1 mL / min; the injection volume is 5 to 15 μL, preferably 7 to 12 μL, and more preferably 10 μL.

5. The method according to any one of claims 1-3, characterized in that, The detection wavelength is 250nm~400nm, preferably 300nm~350nm, and more preferably 330nm.

6. The method according to any one of claims 1-3, characterized in that, In step A), the extraction is ultrasonic extraction; the power of the ultrasound is 400W~800W, preferably 500W~700W, more preferably 550W~650W; the frequency is 10kHz~80kHz, preferably 20kHz~60kHz, more preferably 30kHz~50kHz; the time is 10min~30min, preferably 15min~25min, more preferably 20min.

7. The method according to any one of claims 1-3, characterized in that, In step A), the ratio of the mass (g) of the test sample to the volume (mL) of methanol is (0.1~1):10, preferably (0.1~0.5):10, more preferably 0.3:10; preferably the sample weight is 0.3g, more preferably the amount of methanol used relative to 0.3g of test sample is 5mL~15mL, more preferably 10mL.

8. The method according to any one of claims 1-3, characterized in that, The similarity of characteristic chromatograms of *Agastache rugosa* or *Agastache rugosa* granules was evaluated using a chromatographic fingerprint similarity evaluation system for traditional Chinese medicine. If the test sample is *Agastache rugosa* granules, a standard characteristic chromatogram with 9 characteristic peaks is obtained, with the peak corresponding to the *Cirsium japonicum* reference peak being the S peak. The relative retention times of peaks 3-4, 6-9, and the S peak are within ±10% of the specified values, which are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), 1.41 (peak 8), and 1.65 (peak 9). If the test sample is *Agastache rugosa* granules, a standard characteristic chromatogram with 8 characteristic peaks is obtained, with the peak corresponding to the *Cirsium japonicum* reference peak being the S peak. The relative retention times of peaks 3 to 4, 6, 7, and 9 with peak S are within ±10% of the specified values, where the specified values ​​are: 0.31 (peak 3), 0.58 (peak 4), 1.25 (peak 6), 1.31 (peak 7), and 1.65 (peak 8); and / or the identification results of the characteristic chromatograms of Huoxiang herbal medicine granules include: peak 1: neochlorogenic acid; peak 2: chlorogenic acid; peak 3: caffeic acid; peak 4: rosmarinic acid; peak 5 (S): citric acid; peak 6: apigenin; peak 9: acaciain; and / or the identification results of the characteristic chromatograms of wine-processed Huoxiang herbal medicine granules include: peak 1: neochlorogenic acid; peak 2: chlorogenic acid; peak 3: caffeic acid; peak 4: rosmarinic acid; peak 5 (S): citric acid; peak 6: apigenin; peak 8: acaciain.

9. A method for identifying the characteristic chromatograms of patchouli and wine-processed patchouli preparations, characterized in that, The method described in any one of claims 1 to 8 is used for detection, and the detection results are analyzed. The preparation form includes one or more of medicinal materials, standard decoctions, and processed medicinal slices.

10. A method for preparing a traditional Chinese medicine formula granule of patchouli or wine-processed patchouli, or the traditional Chinese medicine formula granule of patchouli or wine-processed patchouli according to any one of claims 1-8, comprising: (1) Take agastache rugosa, remove impurities, wash, cut into sections, and dry to obtain agastache rugosa slices; (2) Take 600g of the agastache slices obtained in step (1), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, boil, and keep simmering for 20 minutes. For the second decoction, add 10 times the amount of water, boil, and keep simmering for 15 minutes. During the decoction process, the temperature is controlled at 94-100℃. Combine the water extracts. (3) The aqueous extract obtained in step (2) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated patchouli extract; (4) The concentrated agastache obtained in step (3) was spray-dried under the conditions of an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (5) Take 7.5 to 10.0 parts of the dried agastache powder from step (4), add 0.0 to 2.5 parts of maltodextrin, mix well, and perform dry granulation to obtain agastache medicinal formula granules; or (i) Take agastache rugosa, remove impurities, wash, cut into sections, and dry to obtain agastache rugosa slices; (ii) Take 400g of the agastache slices obtained in step (i), add rice wine and mix well according to the wine-processing method (General Chapter 0213 of Chinese Pharmacopoeia 2025 Edition) (the mass ratio of rice wine to agastache slices is 1:15); let it soak thoroughly, place it in a stir-frying container, and stir-fry at a temperature of 120-150℃ for 8-10 minutes. During the stir-frying process, the properties of the material need to be observed at all times. Stir-fry until dry, remove the material, spread it out to cool, and obtain wine-processed agastache slices. (iii) Take 350g of the wine-processed agastache slices obtained in step (ii), add water and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, bring to a boil, and simmer for 20 minutes. For the second decoction, add 10 times the amount of water, bring to a boil, and simmer for 15 minutes. During the decoction process, the temperature should be controlled at 94-100℃. Combine the water extracts. (iv) The aqueous extract obtained in step (iii) is concentrated under reduced pressure to a density of 1.08 to 1.10 at a temperature of 60 to 80°C and a vacuum degree of -0.050 to -0.080 MPa to obtain a concentrated extract of patchouli. (v) The concentrated agastache obtained in step (iv) is spray-dried under an inlet air temperature of 190±5℃ and an outlet air temperature of 95±5℃ to obtain agastache spray-dried powder. (vi) Take 7.1 to 10.0 parts of the dried agastache powder from step (v), add 0.0 to 2.9 parts of maltodextrin, mix well, and perform dry granulation to obtain agastache medicinal formula granules.

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