Preparation process of standard herba houttuyniae decoction

Abstract

The invention discloses a preparation process of a standard herba houttuyniae decoction, and relates to the technical field of traditional Chinese medicine decoction preparation, and the preparation process comprises the following steps: weighing a proper amount of herba houttuyniae decoction pieces, placing in a marmite, decocting twice, adding 12 times of water for the first time, soaking for 30 minutes, boiling with strong fire, and decocting with slow fire for 30 minutes; adding 10 times of water for the second time, boiling with strong fire, then decocting with slow fire for 20 minutes, filtering the liquid medicine with 200 meshes, rapidly cooling the filtrate to room temperature in a water bath, mixing the two filtrates, carrying out vacuum concentration at the temperature of 50 DEG C until the weight ratio of the medicinal material to the fluid extract is about 1: 1, collecting the concentrated solution, and freeze-drying to obtain a sample. According to the invention, key quality indexes such as the main content, the characteristic spectrum and the extract of the herba houttuyniae after the decoction is prepared are stipulated, the transfer rate is investigated, and meanwhile, the transfer rate range of the main content of the herba houttuyniae is stipulated, so that the effectiveness of the herba houttuyniae decoction is kept according to a standard preparation method.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine decoction preparation technology, and in particular to the preparation process of Houttuynia cordata standard decoction. Background Technology

[0002] Houttuynia cordata is a medicinal herb listed in the literature. The herb is derived from the dried aerial parts of the plant Houttuynia cordata. Houttuynia cordata has a pungent taste and is cold in nature. It enters the lung meridian and can detoxify, reduce swelling and heal sores, promote diuresis and remove dampness, stop dysentery, and strengthen the stomach and aid digestion. It is used to treat lung abscess, carbuncles and boils, hematochezia, and spleen and stomach heat accumulation caused by excess heat, heat toxicity, dampness, and febrile diseases. Modern pharmacological experiments have shown that this product has the effects of improving immunity, etc.

[0003] Standard decoctions are single-herb Chinese medicinal decoctions prepared using standardized processes, guided by traditional Chinese medicine theory and based on clinical application, and referencing modern extraction methods. They are used for standardized clinical medication to ensure the accuracy of medication and the consistency of dosage. However, there are currently no quality studies or standards for Houttuynia cordata decoctions in China to measure the quality and efficacy of the decocted Houttuynia cordata decoction. Therefore, we propose a preparation process for standard Houttuynia cordata decoctions. Summary of the Invention

[0004] The main objective of this invention is to provide a preparation process for a standard decoction of Houttuynia cordata, specifying key quality indicators such as the main content, characteristic chromatogram, and extract of Houttuynia cordata after decoction preparation, in order to solve the problems raised in the background art.

[0005] To achieve the above objectives, the technical solution adopted by this invention is as follows: the preparation process of Houttuynia cordata standard decoction includes the following steps:

[0006] S1: Weigh out an appropriate amount of Houttuynia cordata slices, place them in a clay pot, and decoct twice.

[0007] S2: In the above operation, add 12 times the amount of water for the first time, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes to obtain a mixed medicinal liquid.

[0008] S3: In the above operation, add 10 times the amount of water for the second time, bring to a boil over high heat, then simmer over low heat for 20 minutes to obtain a further mixed medicinal liquid;

[0009] S4: Based on the above steps, filter the mixed solution through a 200-mesh filter, cool the filtrate to room temperature in a cold water bath, and combine the two filtrates;

[0010] S5: Vacuum concentration is carried out at a temperature of 50℃ until the weight ratio of medicinal material to fluid extract is approximately 1:1. The concentrated liquid is then collected and freeze-dried to obtain the sample.

[0011] In the S5 process, vacuum concentration is performed at a temperature of 50°C, with an absolute vacuum of 30-40 mbar.

[0012] In step S5, the extraction rate and extract indicators of traditional Chinese medicine in decoction are measured through concentration and freeze-drying operations.

[0013] The present invention has the following beneficial effects:

[0014] I. The present invention provides a Houttuynia cordata decoction that specifies key quality indicators such as the main content, characteristic spectrum, and extract of Houttuynia cordata after decoction preparation, and investigates the transfer rate and specifies the range of transfer rate of the main content of Houttuynia cordata, so as to maintain the effectiveness of the Houttuynia cordata decoction after preparation according to the standard method.

[0015] II. The preparation process of the standard decoction of Houttuynia cordata in this invention has objective quality standards to measure the component transfer of Houttuynia cordata slices into decoction, and to ensure the quality and effectiveness of the decoction.

[0016] 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

[0017] Figure 1 This is a flowchart illustrating the preparation process of the standard Houttuynia cordata decoction of this invention.

[0018] Figure 2 This is a characteristic peak-to-peak value comparison spectrum diagram of the present invention;

[0019] Figure 3 This is a comparative characteristic chromatogram of the standard decoction of Houttuynia cordata of the present invention. Detailed Implementation

[0020] 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.

[0021] like Figure 1 The preparation process of the standard decoction of Houttuynia cordata is as follows: Weigh an appropriate amount of Houttuynia cordata slices, place them in a clay pot, and decoct twice. For the first decoction, add 12 times the amount of water, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes. For the second decoction, add 10 times the amount of water, bring to a boil over high heat, then simmer over low heat for 20 minutes. Filter the decoction through a 200-mesh sieve, cool the filtrate to room temperature in a cold water bath, combine the two filtrates, and concentrate under vacuum at 50℃ and an absolute vacuum of 30–40 mbar until a fluid extract with a weight ratio of approximately 1:1 is obtained. Collect the concentrated liquid and freeze-dry to obtain the sample. Subsequent concentration and freeze-drying are necessary to measure the yield and extract content of the traditional Chinese medicine in the decoction.

[0022] The water extract of Houttuynia cordata was concentrated under vacuum, then freeze-dried to dryness. The dried extract powder was collected, weighed, and the yield was calculated. The formula for the yield is as follows:

[0023]

[0024] Ointment yield range: 15%–20%.

[0025] The extract was determined using ethanol as the solvent, following the hot extraction method as described in the "Determination of Alcohol-Soluble Extracts" section of the Chinese Pharmacopoeia 2020, Part IV, General Chapter 2201. The extract content of the standard decoction ranged from 12.5% ​​to 23.1%.

[0026] The content determination procedure includes determining quercetin by high performance liquid chromatography (General Chapter 0512, Chinese Pharmacopoeia 2020 Edition);

[0027] Chromatographic conditions and system suitability tests were conducted using octadecylsilane-bonded silica gel as the stationary phase; acetonitrile-0.1% phosphoric acid solution (23:77) as the mobile phase; and a detection wavelength of 254 nm. The theoretical plate number, calculated based on the quercetin peak, should be no less than 3000.

[0028] To prepare the reference solution, take an appropriate amount of quercetin reference standard, accurately weigh it, and add 50% methanol to prepare a solution containing 40 μg per ml.

[0029] To prepare the test solution, take an appropriate amount of this product, grind it into a fine powder, accurately weigh about 0.1 g, place it in a stoppered conical flask, accurately add 25 ml of 50% methanol, seal tightly, weigh, sonicate (power 250 W, frequency 40 kHz) for 30 minutes, cool, weigh again, replenish the lost weight with 50% methanol, shake well, filter, and collect the filtrate to obtain the test solution.

[0030] Determination method: Accurately pipette 10 μl of the reference solution and the test solution into the liquid chromatograph and determine the result.

[0031] Table 1 shows the calculation of the transfer rate of quercetin in the sample solution:

[0032]

[0033] The content of quercetin in each 1g of this product should be 5.2mg / g to 10.6mg / g;

[0034] The quercetin content transfer rate of medicinal materials to standard decoction ranged from 35.5% to 72.7%.

[0035] Among them, the characteristic chromatograms were determined by high performance liquid chromatography (Chinese Pharmacopoeia 2020 Edition, Part IV, General Chapter 0512).

[0036] Chromatographic conditions and system suitability tests included: using octadecylsilane-bonded silica gel as the packing material (column length 250 mm, inner diameter 4.6 mm, particle size 5 μm); using acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, performing gradient elution as specified in the table below; flow rate 1.0 mL / min; column temperature 30 °C; detection wavelength 326 nm for 0–30 min and 254 nm for 30–80 min. The theoretical plate number, calculated based on the quercetin peak, should be no less than 3000.

[0037] Table 2 shows the gradient elution table for chromatographic conditions and system suitability testing:

[0038]

[0039] Preparation of reference solution: Take 0.5g of Houttuynia cordata reference material, place it in a stoppered conical flask, add 25ml of 50% methanol, sonicate (power 250W, frequency 40kHz) for 30 minutes, cool, shake well, filter, and take the filtrate as the reference solution. Separately, take appropriate amounts of chlorogenic acid reference standard, hyperoside reference standard, and quercetin reference standard, accurately weigh them, and add 50% methanol to prepare a mixed solution containing 100μg of each per ml, as the reference solution.

[0040] Determination method: Accurately pipette 10 μl each of the reference solution and the test solution into the liquid chromatograph and determine the result.

[0041] Among them, such as Figure 2 As shown, the chromatogram of the test sample should show 6 characteristic peaks, and the retention times should correspond to the 6 characteristic peaks in the chromatogram of the reference medicinal material; among them, 3 peaks should correspond to the retention times of the corresponding reference material peaks. The peak corresponding to the chlorogenic acid reference peak is the S peak. Calculate the relative retention times of peaks 1, 3, and 4 with peak S. The relative retention times should be within ±7% of the specified values, which are: 0.66 (peak 1), 1.03 (peak 3), and 1.13 (peak 4). Calculate the peak area ratio of peak 5 to peak 6. The peak area ratio should not be less than 0.300. Figure 2 In the sample, peak 1 is neochlorogenic acid; peak 2 (S) is chlorogenic acid; peak 3 is cryptochlorogenic acid; peak 5 is hyperoside; peak 6 is quercetin; each milligram of the test sample is approximately equivalent to 0.023 grams of medicinal slices.

[0042] In this plan, the selection of raw materials is based on 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. Houttuynia cordata is a cultivated product, distributed throughout my country. It is mainly produced in Sichuan and Hubei provinces, where its cultivation has reached a large scale and is also the main source of Houttuynia cordata for commercial use. 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 are Xuanhan County in Dazhou City, Sichuan Province; Cangxi County in Guangyuan City, Sichuan Province; Dangyang County and Enshi Prefecture in Hubei Province; and Shizhu County in Chongqing. Ultimately, 15 qualified batches will be selected for research on standard decoctions.

[0043] Specifically, Table 3 shows the transfer rate of 15 batches of Houttuynia cordata standard decoction:

[0044]

[0045]

[0046] In the table above, based on the content of 15 batches of Houttuynia cordata slices, the content of standard decoction, and the yield of extract, the average transfer rate of the standard decoction was calculated to be 54.1%. The range calculated using the mean plus or minus 3 times the SD is 35.5% to 72.7%. The range calculated using the mean of 70% to 130% is 37.9% to 70.3%. Considering the actual range of 47.4% to 69.8%, 35.5% to 72.7% is taken as the upper and lower limits of the transfer rate of the standard decoction.

[0047] Modern research shows that Houttuynia cordata contains various chemical components, mainly volatile oils, flavonoids (quercetin), organic acids, alkaloids, and vitamins. Its main active ingredients are volatile oils and flavonoids. Houttuynia cordata possesses a variety of pharmacological activities, including antipyretic, anti-inflammatory, antibacterial, antiviral, immune-enhancing, anti-allergic, antitussive, antidepressant, insulin-resistant, hypoglycemic, and ventricular remodeling-improving effects. The national standard YBZ-PFKL-202145, "Houttuynia cordata Formula Granules," designates quercetin as a quality control indicator component for Houttuynia cordata. Therefore, this study selected quercetin as the quality control indicator component for the standard Houttuynia cordata decoction.

[0048] Among them, based on the "Technical Requirements for Quality Control and Standard Formulation of Traditional Chinese Medicine Formula Granules", and combined with the data of 15 batches of Houttuynia cordata standard decoction, the content limits and upper and lower limits of the standard decoction were calculated.

[0049] The range calculated using the mean plus or minus 3 times the SD is 5.2 mg to 10.6 mg.

[0050] The range calculated using 70%–130% of the mean is 5.5 mg–10.3 mg.

[0051] Based on the actual range of 6.6mg to 8.6mg, it is recommended to use the mean plus or minus 3 times the SD, i.e., 5.2mg to 10.6mg, as the upper and lower limits of the standard decoction content.

[0052] Based on the content of 15 batches of Houttuynia cordata slices, the content of standard decoction, and the yield of extract, the average transfer rate of standard decoction content was calculated to be 54.1%.

[0053] The range calculated using the mean plus or minus 3 times the SD is 35.5% to 72.7%.

[0054] The range calculated using 70% to 130% of the mean is 37.9% to 70.3%.

[0055] Based on the actual range, it is 47.4% to 69.8%;

[0056] The upper and lower limits of the standard decoction transfer rate were set at 35.5% to 72.7%.

[0057] The research and standardization of characteristic maps are as follows:

[0058] like Figure 3 As shown, the chromatogram of the Houttuynia cordata standard decoction with experimental batch number BT(YXC)211201 was selected as the reference chromatogram to establish a control characteristic chromatogram. Based on the data analysis results, six common peaks were finally selected as characteristic peaks. The generated standard chromatograms are shown in Table 5. Chlorogenic acid was selected as the reference peak, and the relative retention times of the characteristic peaks in the chromatogram were calculated. By comparing with the reference chromatogram, it can be seen that among the six characteristic peaks in the Houttuynia cordata standard decoction characteristic chromatogram, peak 2 (S) is chlorogenic acid. According to the national drug standard YBZ-PFKL-2021145 for "Houttuynia cordata Formula Granules", peak 1: neochlorogenic acid; peak 2 (S): chlorogenic acid; peak 3: cryptochlorogenic acid; peak 5: hyperoside; peak 6: quercetin.

[0059] Table 4 shows a comparison of the retention times of 15 batches of Houttuynia cordata standard decoction:

[0060]

[0061]

[0062] Table 5 shows the relative retention times (peak areas) of 15 batches of Houttuynia cordata standard decoction:

[0063]

[0064]

[0065] The results showed that the characteristic chromatograms of 15 batches of Houttuynia cordata standard decoction samples all showed chromatographic peaks corresponding to the retention times of the six main characteristic peaks in the control herb. The relative retention time RSD of peaks 1-6 was less than 2%, indicating that the elution times of each peak were consistent among the batches.

[0066] The relative peak area RSD of peaks 5 and 6 is less than 3%, indicating that the relative peak area of ​​each peak is basically the same across batches. Therefore, it is stipulated that the peak area ratio of peak 5 to peak 6 shall not be less than 0.300.

[0067] According to the national standard YBZ-PFKL-202145 for Houttuynia cordata formula granules, only the retention times of peaks 2 (chlorogenic acid), 5 (hyperoside), and 6 (quercetin) should correspond to the retention times of the reference standard, as well as the relative retention times of peaks 1, 3, and 4, and the peak area ratio of peak 5 to peak 6. Based on the determination results of 15 batches of Houttuynia cordata standard decoctions and the retention time data from the repeatability and precision tests in the methodology (see Table 6), it can be seen that the retention times of peaks 2 (chlorogenic acid), 5 (hyperoside), and 6 (quercetin) are stable and correspond to the retention times of the corresponding reference standards. The relative peak drift of peaks 1 and 5-6 is very small, basically within ±7%. The relative peak area RSD of characteristic peaks 5 and 6 is less than 3%, indicating that the difference in the relative peak area of ​​peaks 7 and 8 between batches is small. Therefore, it is stipulated that: the chromatogram of the test sample should show 6 characteristic peaks, and the retention times should correspond to the 6 characteristic peaks in the chromatogram of the reference medicinal material; among them, 3 peaks should correspond to the retention times of the corresponding reference material peaks. The peak corresponding to the chlorogenic acid reference peak is the S peak. The relative retention times of peaks 1, 3, and 4 with the S peak should be calculated, and their relative retention times should be within ±7% of the specified values, which are: 0.66 (peak 1), 1.03 (peak 3), and 1.13 (peak 4); the peak area ratio of peak 5 to peak 6 should be calculated, and its peak area ratio should not be less than 0.300.

[0068] In this plan, the research and standard setting of leachate are as follows:

[0069] The determination of alcohol-soluble extracts was performed using the hot extraction method as specified in the General Chapter 2201 of Part IV of the Chinese Pharmacopoeia 2020. The test results of 15 batches of Houttuynia cordata standard decoction are shown in the table below.

[0070] Table 6 is a comparison table of the extract results of 18 batches of Platycladus orientalis leaves:

[0071]

[0072] The average value of the alcohol-soluble extract from 15 batches of standard decoction was 17.8%.

[0073] The range calculated using the mean plus or minus 3 times the SD is 12.8% to 22.8%.

[0074] The range calculated using 70% to 130% of the mean is 12.5% ​​to 23.1%.

[0075] Based on the actual range, it is 14.8% to 19.9%;

[0076] The upper and lower limits of the standard decoction extract were set at 12.5% ​​to 23.1%.

[0077] In this invention, taking Houttuynia cordata decoction as an example, the key quality indicators such as the main content, characteristic spectrum and extract of Houttuynia cordata after decoction preparation are specified, and the transfer rate is investigated. The range of transfer rate of the main content of Houttuynia cordata is specified to ensure the effectiveness of Houttuynia cordata decoction after standard preparation method.

[0078] 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.

[0079] 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 Houttuynia cordata standard decoction, characterized in that, Includes the following steps: S1: Weigh out the slices of Houttuynia cordata, place them in a clay pot, and decoct twice. S2: In the above operation, add 12 times the amount of water for the first time, soak for 30 minutes, bring to a boil over high heat, then simmer over low heat for 30 minutes to obtain a mixed medicinal liquid. S3: In the above operation, add 10 times the amount of water for the second time, bring to a boil over high heat, then simmer over low heat for 20 minutes to obtain a further mixed medicinal liquid; S4: Based on the above steps, filter the mixed solution through a 200-mesh filter, cool the filtrate to room temperature in a cold water bath, and combine the two filtrates; S5: Vacuum concentration is carried out at a temperature of 50℃ until the weight ratio of medicinal material to fluid extract is 1:

1. The concentrated liquid is then collected and freeze-dried to obtain the sample.

2. The preparation process of the Houttuynia cordata standard decoction according to claim 1, characterized in that, In the S5 process, vacuum concentration is performed at a temperature of 50°C, with an absolute vacuum of 30-40 mbar.

3. The preparation process of the Houttuynia cordata standard decoction according to claim 1, characterized in that, In step S5, the extraction rate and extract indicators of houttuynia cordata in decoction are measured through concentration and freeze-drying operations.

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