Preparation process of common selfheal fruit-spike standard decoction
By establishing a standard preparation process for Prunella vulgaris decoction, the problem of difficulty in measuring the quality of traditional Chinese medicine decoctions was solved, quality control indicators were established, and the quantifiable evaluation and effectiveness assurance of decoction components were achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-01
- Publication Date
- 2026-04-03
AI Technical Summary
The lack of standard regulations for the quality of traditional Chinese medicine decoctions in the current technology makes it difficult to measure the quality and efficacy after decoction.
The preparation process of the standard decoction of Prunella vulgaris was established, including weighing the Prunella vulgaris slices, decocting twice, filtering, vacuum concentration and freeze drying, and establishing quality control indicators such as extract yield, rosmarinic acid content, characteristic chromatograms, etc.
Objective quality standards are provided to ensure the transfer of components from Prunella vulgaris slices to decoction, thus ensuring the quality and effectiveness of the decoction.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of traditional Chinese medicine decoction processing technology, and in particular to the preparation process of standard decoction of Prunella vulgaris. Background Technology
[0002] Prunella vulgaris is a perennial herbaceous plant belonging to the Lamiaceae family and the Prunella genus. Its leaves are opposite, ovate or elliptic-lanceolate, and its verticillasters are arranged in spikes. The bracts are reniform, abruptly acuminate or caudate at the apex, and hairy on the outside and margins. The calyx is bilabiate; the corolla is purple; and the nutlets are brown. It flowers from April to June and fruits from July to October. Around the summer solstice, the plant withers and turns yellow.
[0003] Prunella vulgaris is distributed in all provinces and regions south of the Qinling Mountains in China, as well as Xinjiang. It is also widely distributed in Europe, North Africa, West Asia, and East Asia, and can be occasionally seen in Australia and North America. It grows mostly in wetlands along mountain streams, riverbanks, wastelands, and roadsides. The main varieties of Prunella vulgaris are the white-flowered variety and the narrow-leaved variety.
[0004] Prunella vulgaris has been used in China for over a thousand years as a traditional Chinese medicine. The "New Compendium of Materia Medica" calls it a holy medicine for treating sores. The whole plant can be used as medicine, and it has the effects of clearing liver fire, improving eyesight, and dispersing nodules and reducing swelling. In modern times, it is made into Prunella vulgaris decoction, oral liquid, granules, tablets, capsules, liniments and other prescriptions.
[0005] Since hospitals and the market currently lack quality research and standardization for traditional Chinese medicine decoctions to measure their quality and efficacy after preparation, this study takes Prunella vulgaris decoction as an example. It specifies key quality indicators such as the main content, characteristic spectrum, and extracts of Prunella vulgaris after decoction preparation, examines the transfer rate, and defines the range of transfer rates for the main content of Prunella vulgaris, ensuring the effectiveness of Prunella vulgaris decoction after standard preparation. Summary of the Invention
[0006] The main objective of this invention is to provide a preparation process for a standard decoction of Prunella vulgaris, in order to solve the problems mentioned in the background art.
[0007] In order to derive the preparation process of the standard decoction of Prunella vulgaris, the present invention conducted relevant pharmaceutical research, such as screening 15 batches of Prunella vulgaris herbs from major producing areas across the country for quality comparison research, and preparing 15 batches of standard decoctions in accordance with the "Management Standards for Traditional Chinese Medicine Decoction Rooms in Medical Institutions".
[0008] To achieve the above objectives, the technical solution adopted by this invention is as follows: The preparation process of the standard decoction of Prunella vulgaris involves first weighing an appropriate amount of Prunella vulgaris slices, placing them in a clay pot, and decocting them twice, including the following steps:
[0009] Step 1: Add 12 times the amount of water to the clay pot for the first time, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes.
[0010] Step 2: Add 10 times the amount of water to the clay pot for the second time, bring to a boil over high heat, then simmer over low heat for 20 minutes.
[0011] Step 3: Then filter the above medicine solution through a 200-mesh filter and cool the filtrate to room temperature in a cold water bath;
[0012] Step 4: Combine the two filtrates and concentrate them under vacuum at 50°C;
[0013] Step 5: Concentrate the extract to a 1:1 weight ratio of medicinal material to fluid extract, collect the concentrate, and freeze-dry to obtain the sample.
[0014] Preferably, in Step 4, vacuum concentration is performed under an absolute vacuum of 30–40 mbar.
[0015] The present invention has the following beneficial effects:
[0016] The preparation process of the standard decoction of Prunella vulgaris in this invention has objective quality standards to measure the component transfer of Prunella vulgaris slices into decoction, and to ensure the quality and effectiveness of the decoction.
[0017] Of course, any product implementing this invention does not necessarily need to achieve all of the advantages described above at the same time. Attached Figure Description
[0018] Figure 1 This is a flowchart illustrating the preparation process of the standard decoction of Prunella vulgaris according to the present invention.
[0019] Figure 2 This is a comparative characteristic chromatogram of the test solution of the standard decoction of Prunella vulgaris of the present invention;
[0020] Figure 3 This is a comparative characteristic spectrum of the standard decoction of Prunella vulgaris of the present invention. Detailed Implementation
[0021] The technical solutions in this utility model will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.
[0022] Example 1:
[0023] like Figure 1The preparation process of the standard decoction of Prunella vulgaris is as follows: First, weigh an appropriate amount of Prunella vulgaris slices and place them in a clay pot. Decoct twice, including the following steps: Step 1: First, add 12 times the amount of water to the clay pot containing the Prunella vulgaris slices, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes; Step 2: Second, add 10 times the amount of water to the clay pot containing the Prunella vulgaris slices, bring to a boil over high heat, then simmer over low heat for 20 minutes; Step 3: Then filter the above decoction through a 200-mesh sieve and cool the filtrate to room temperature in a cold water bath; Step 4: Combine the two filtrates and concentrate them under vacuum at 50℃; Step 5: Concentrate to a fluid extract with a weight ratio of 1:1 (medicinal material to fluid extract), collect the concentrate, and freeze-dry to obtain the sample.
[0024] Extract yield: After vacuum concentration of the Prunella vulgaris aqueous extract, the concentrate is freeze-dried to dryness. The dried extract powder is collected and weighed to calculate the extract yield. The formula for extract yield is as follows:
[0025]
[0026] Ointment yield range: 9.0% to 14.6%.
[0027] Extractives: Determined by hot extraction method according to the method for determination of alcohol-soluble extractives (Chinese Pharmacopoeia 2020 Edition, Part IV, General Chapter 2201) using ethanol as solvent. The extractives range of the standard decoction is 31.7%–58.9%.
[0028] Content determination
[0029] Rosmarinic acid was determined by high performance liquid chromatography (General Chapter 0512, Chinese Pharmacopoeia 2020).
[0030] Chromatographic conditions and system suitability test: Octadecylsilane-bonded silica gel was used as the stationary phase; methanol-0.1% phosphoric acid solution (42:58) was used as the mobile phase; the detection wavelength was 330 nm. The theoretical plate number, calculated based on the rosmarinic acid peak, should not be less than 6000.
[0031] Preparation of reference solution: Take an appropriate amount of rosmarinic acid reference standard, accurately weigh it, and add dilute ethanol to prepare a solution containing 0.1 mg per ml.
[0032] Preparation of the test solution: Take an appropriate amount of this product, grind it into a fine powder, take about 0.2g, weigh it accurately, place it in a stoppered conical flask, accurately add 25ml of dilute ethanol, weigh it, sonicate it (power 250W, frequency 40kHz) for 30 minutes, cool it, weigh it again, make up the weight loss with dilute ethanol, shake it well, filter it, and take the filtrate to obtain the test solution.
[0033] The assay involves precisely pipetting 10 μl each of the reference solution and the test solution into a liquid chromatograph and measuring the results.
[0034] Table 1 shows the transfer rate of rosmarinic acid content from medicinal materials to the standard decoction:
[0035]
[0036] This product contains 14.7 mg / g to 25.9 mg / g of rosmarinic acid per 1g.
[0037] The transfer rate of rosmarinic acid content in the decoction of medicinal materials ranged from 27.0% to 50.1%.
[0038] Characteristic chromatogram: determined by high performance liquid chromatography (Chinese Pharmacopoeia 2020 Edition, Part IV, General Chapter 0512).
[0039] Chromatographic conditions and system suitability test: Octadecylsilane-bonded silica gel was used as the packing material (column length 250 mm, inner diameter 4.6 mm, particle size 5 μm); acetonitrile was used as mobile phase A, and 0.1% phosphoric acid solution was used as mobile phase B, with gradient elution performed according to the specifications in the table below; the flow rate was 1.0 mL / min; the column temperature was 30 °C; and the detection wavelength was 280 nm. The theoretical plate number, calculated based on the rosmarinic acid peak, should be no less than 6000.
[0040] Table 2 shows the gradient elution table:
[0041]
[0042] Preparation of the reference solution: Take 1g of Prunella vulgaris reference material, add 25ml of water, heat under reflux for 45 minutes, filter, and take the filtrate as the reference solution. Separately, take appropriate amounts of caffeic acid reference standard and rosmarinic acid reference standard, accurately weigh them, and add dilute ethanol to prepare a mixed reference solution containing 20μg of caffeic acid and 40μg of rosmarinic acid per 1ml, as the reference solution.
[0043] The preparation of the test solution is the same as in the [Assay] section.
[0044] The determination method involves precisely pipetting 10 μl of the reference solution and the test solution into the liquid chromatograph and measuring the results.
[0045] The chromatogram of the test sample should show five characteristic peaks, and their retention times should correspond to the five characteristic peaks in the chromatogram of the reference medicinal material. Peaks 3 and 4 should correspond to the retention times of the reference peaks for caffeic acid and rosmarinic acid, respectively. The peak corresponding to the rosmarinic acid reference peak is designated as the S peak. The relative retention times of each characteristic peak and the S peak should be calculated and should be within ±8% of the specified values. The specified values are: 0.18 (peak 1), 0.38 (peak 2), and 1.60 (peak 5).
[0046] Example 2:
[0047] 1. Raw material selection
[0048] According to the "Technical Requirements for Quality Control and Standardization of Traditional Chinese Medicine Formula Granules," the samples used in the research should be representative, covering the main producing areas or authentic production areas of the medicinal materials to be harvested, with no fewer than three batches from each producing area. Prunella vulgaris is a cultivated product, distributed throughout my country. It is mainly produced in Henan and Anhui provinces, where its cultivation has reached a large scale and is the main source of commercial Prunella vulgaris. Based on a comprehensive evaluation of raw material quality, sustainable resource supply, and other factors, the preliminary production areas for raw materials used in large-scale production were determined to be Queshan County in Zhumadian City, Henan Province; Wuling City in Jiaozuo City, Henan Province; Sheqi County in Nanyang City, Henan Province; Yangtong County in Henan Province; and Wangjiang County in Qing'an City, Anhui Province. Ultimately, 15 qualified batches were selected for research on standard decoctions.
[0049] 2. Research and standard setting on extract yield and transfer rate
[0050] Table 3 shows the glycoside content of 18 batches of standard licorice decoction.
[0051]
[0052]
[0053] Based on the content of 15 batches of Prunella vulgaris slices, the content of standard decoction, and the yield of extract, the average content transfer rate of standard decoction was calculated to be 20.3%.
[0054] The range calculated using the mean plus or minus 3 times the SD is 32.1% to 45.0%.
[0055] The range calculated using 70% to 130% of the mean is 27.0% to 50.1%.
[0056] Based on the actual range, it is 35.6% to 43.5%;
[0057] It is recommended to take 27.0% to 50.1% as the upper and lower limits of the standard decoction transfer rate.
[0058] 3. Content research and standard setting
[0059] Modern research shows that Prunella vulgaris contains various components, such as polysaccharides (including galactose, glucose, mannose, xylose, arabinose, and rhamnose), organic acids (rosmarinic acid), flavonoids, triterpenes and their glycosides, and sterols. Prunella vulgaris possesses various pharmacological activities, including anti-tumor, anti-thyroid cancer, anti-breast cancer, anti-lymphoma, anti-inflammatory, antibacterial, antioxidant, and antihypertensive effects. The 2020 edition of the Chinese Pharmacopoeia lists rosmarinic acid as an indicator component for the quality control of Prunella vulgaris. Combined with the fact that the national drug standard YBZ-PFKL-2021128 for Prunella vulgaris formula granules uses rosmarinic acid as a quality control component under the "Content Determination" section, this study selected rosmarinic acid as the quality control indicator component for the standard Prunella vulgaris decoction.
[0060] Based on the "Technical Requirements for Quality Control and Standard Formulation of Traditional Chinese Medicine Formula Granules", and combined with data from 15 batches of Prunella vulgaris standard decoction, the content limits and upper and lower limits of the standard decoction were calculated.
[0061] The range calculated using the mean plus or minus 3 times the SD is: 14.7 mg to 25.9 mg;
[0062] The range calculated using 70%–130% of the mean is 14.2 mg–26.4 mg.
[0063] Based on the actual range of 16.9mg to 23.1mg, it is recommended to use the average value of 70% to 130%, i.e., 14.7mg to 25.9mg, as the upper and lower limits of the standard decoction content.
[0064] Based on the content of 15 batches of Prunella vulgaris slices, the content of standard decoction, and the yield of extract, the average content transfer rate of standard decoction was calculated to be 20.3%.
[0065] The range calculated using the mean plus or minus 3 times the SD is 32.1% to 45.0%.
[0066] The range calculated using 70% to 130% of the mean is 27.0% to 50.1%.
[0067] Based on the actual range, it is 35.6% to 43.5%;
[0068] It is recommended to take 27.0% to 50.1% as the upper and lower limits of the standard decoction transfer rate.
[0069] 4. Characteristic spectrum research and standard setting
[0070] The chromatogram of the standard decoction of Prunella vulgaris with experimental batch number BT(XKC)220301 was selected as the reference chromatogram to establish a control characteristic chromatogram. Based on the data analysis results, five common peaks were finally selected as characteristic peaks, and the generated standard chromatogram is shown in Figure 4-11. Rosmarinic acid was selected as the reference peak, and the relative retention times of the characteristic peaks in the chromatogram were calculated. According to the national drug standard YBZ-PFKL-2021128 "Prunella vulgaris Formula Granules", among the five characteristic peaks in the characteristic chromatogram of the standard decoction of Prunella vulgaris, peak 1 is tanshinone, peak 2 is protocatechuic aldehyde, peak 3 is caffeic acid, and peak 4(S) is rosmarinic acid.
[0071] Table 4 shows the retention time of 15 batches of Prunella vulgaris standard decoction.
[0072]
[0073]
[0074] The results showed that the characteristic chromatograms of five randomly selected batches of Prunella vulgaris standard decoction samples all showed chromatographic peaks corresponding to the retention times of the five main characteristic peaks in the control herb. The relative retention time RSD of peaks 1, 2, and 5 was less than 2%, indicating that the elution times of each peak were consistent across batches. (Note: The batch number of the standard decoction was selected to correspond to the batch of the medicinal slices to prove that the prepared sample had almost no effect on the characteristic chromatogram of the medicinal slices.)
[0075] The national standard YBZ-PFKL-2021128, "Prunella vulgaris Formula Granules," stipulates that peaks 3 and 4 should correspond to the retention times of caffeic acid and rosmarinic acid reference peaks, respectively; the retention times of peaks 1-5 should correspond to the retention times of the reference decoction pieces; and the relative retention times of peaks 1, 2, and 5 are specified. Based on the results of five batches of Prunella vulgaris standard decoctions and the retention time data from the repeatability and precision tests in the methodology, it can be seen that the retention times of peaks 3 and 4 are stable and correspond to the retention times of caffeic acid and rosmarinic acid reference peaks. The relative peak drift of peaks 1, 2, and 5 is very small, basically within ±6%, indicating that the retention times of each characteristic peak are stable. Therefore, it is stipulated that the chromatogram of the test sample should show five characteristic peaks, and their retention times should correspond to the five characteristic peaks in the chromatogram of the reference medicinal material, with peaks 3 and 4 corresponding to the retention times of caffeic acid and rosmarinic acid reference peaks, respectively. The peak corresponding to the rosmarinic acid reference peak is designated as the S peak. The relative retention times of each characteristic peak and the S peak are calculated, and these relative retention times should be within ±8% of the specified values. The specified values are: 0.18 (peak 1), 0.38 (peak 2), and 1.60 (peak 5).
[0076] 5. Leachate research and standard setting
[0077] Grind the product into a fine powder, take approximately 2g, accurately weigh it, and accurately add 100ml of ethanol. Determine the soluble extract using the hot extraction method as described in the General Chapter 2201 of the Chinese Pharmacopoeia 2020. The test results for 15 batches of Prunella vulgaris standard decoction are shown in Table 5.
[0078] Table 5 shows the results of extract determination of 15 batches of Prunella vulgaris.
[0079]
[0080]
[0081] The average value of the alcohol-soluble extract from 15 batches of standard decoction was 26.5%.
[0082] The range calculated using the mean plus or minus 3 times the SD is 15.8% to 37.2%.
[0083] The range calculated using 70% to 130% of the mean is 18.5% to 34.5%.
[0084] Based on the actual range of 21.2% to 31.4%;
[0085] It is recommended to take 31.7% to 58.9% as the upper and lower limits of the standard decoction extract.
[0086] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0087] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to any specific implementation. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. The preparation process of the standard decoction of Prunella vulgaris, firstly, weigh the Prunella vulgaris slices, place them in a clay pot, and decoct twice, characterized in that... Includes the following steps: Step 1: Add 12 times the amount of water to the clay pot for the first time, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes. Step 2: Add 10 times the amount of water to the clay pot for the second time, bring to a boil over high heat, then simmer over low heat for 20 minutes. Step 3: Then filter the above medicine solution through a 200-mesh filter and cool the filtrate to room temperature in a cold water bath; Step 4: Combine the two filtrates and concentrate them under vacuum at 50°C; Step 5: Concentrate the extract to a 1:1 weight ratio of medicinal material to fluid extract, collect the concentrate, and freeze-dry to obtain the sample.
2. The preparation process of the standard decoction of Prunella vulgaris according to claim 1, characterized in that, In Step 4, vacuum concentration is carried out under an absolute vacuum of 30–40 mbar.