Preparation method of charred schizonepeta spike decoction pieces and product thereof

Abstract

The invention provides a preparation method of schizonepeta spike charcoal decoction pieces and a product thereof, and the preparation method of the schizonepeta spike charcoal decoction pieces comprises the following steps: cleaning schizonepeta spikes, cutting into sections and frying charcoal to obtain the schizonepeta spike charcoal decoction pieces; the charcoal frying temperature is 200 to 320 DEG C, and the charcoal frying time is 5 to 30 minutes. The charring temperature and time are controlled, the surface of the charred schizonepeta spike decoction piece is black brown, and the interior of the charred schizonepeta spike decoction piece is burnt yellow, meanwhile, the content of luteolin in the charred schizonepeta spike decoction piece is further increased, the stability and safety of the prepared charred schizonepeta spike decoction piece are improved, and the method is suitable for popularization and application. The hemostasis and anti-inflammation effects of the charred schizonepeta spike decoction pieces are better exerted; meanwhile, the preparation method of the charred schizonepeta spike decoction piece is suitable for large-scale production.

Description

Technical Field

[0001] The invention relates to the field of traditional Chinese medicine preparations, and in particular to a preparation method of schizonepeta spicate charcoal slices and a product thereof. Background Art

[0002] Schizonepeta spicate has a long history of medicinal use in my country and is a famous traditional medicinal material. This product is slightly warm in nature and pungent in taste. It enters the lung and liver meridians and belongs to the category of Chinese herbal medicine for diaphoresis. Its functions and indications are diaphoresis, dispersing wind, clearing rashes, and eliminating sores. It is used for colds, headaches, measles, rubella, and the initial stage of sores.

[0003] Schizonepeta spicate charcoal is the product of Schizonepeta spicate roasted into charcoal. This method of roasting into charcoal aims to change the medicinal properties and effects of Schizonepeta spicate to meet the needs of specific disease treatment. Schizonepeta spicate roasted into charcoal becomes pungent, astringent and slightly warm. Its main function is to astringe and stop bleeding. It is used for bloody stool, metrorrhagia and postpartum fainting.

[0004] The main components of Nepeta charcoal are luteolin and rosmarinic acid. Luteolin, as a flavonoid compound, has anti-inflammatory and hemostatic effects. Rosmarinic acid, as a phenolic acid compound, has excellent antioxidant and antibacterial and anti-inflammatory effects.

[0005] The pharmacopoeia stipulates that the moisture content in Schizonepeta Spike charcoal should not exceed 9%. At the same time, studies have shown that the higher the luteolin content in Schizonepeta Spike charcoal slices, the better the hemostatic effect of the Schizonepeta Spike charcoal slices. During the process of charcoal frying of Schizonepeta Spike slices, the content of rosmarinic acid will show a downward trend as the charcoal frying temperature or time increases. If the rosmarinic acid content is too high, it indicates that the Schizonepeta Spike charcoal is not properly prepared; if the rosmarinic acid content is too low, the anti-inflammatory effect is reduced, thereby affecting the hemostatic effect of the slices. While increasing the luteolin content in Schizonepeta Spike charcoal slices, controlling the mass percentage of rosmarinic acid at 0.010% to 0.060% can better and comprehensively improve the hemostatic and anti-inflammatory effects of Schizonepeta Spike charcoal slices.

[0006] At present, the Chinese Pharmacopoeia (2020 edition) states that the charcoal method of schizonepeta spicate is as follows: Take schizonepeta spicate segments, fry them according to the charcoal method (General Rule 0213) until the surface is dark brown and the inside is burnt yellow, spray a little water, extinguish the sparks, take them out, and dry them. The charcoal method (General Rule 0213) states that the charcoal method is as follows: Take the product to be processed, place it in a hot pot, fry it with high heat until the surface is burnt black and the inside is burnt brown or to the specified degree, spray a little water, extinguish the sparks, take them out, and dry them.

[0007] However, in the prior art, the endpoint of charcoal roasting is controlled by the properties of Schizonepeta spicate charcoal, namely, "black-brown on the surface and burnt yellow on the inside". This method of judging the endpoint of charcoal roasting is highly subjective, and the Schizonepeta spicate charcoal roasted under different charcoal roasting parameters, which has "black-brown on the surface and burnt yellow on the inside", has large differences in the contents of luteolin and rosmarinic acid, poor stability, and uneven astringent and hemostatic effects.

[0008] The existing technology lacks precise control over the preparation method of Schizonepeta Spike charcoal. Therefore, providing a stable and accurate preparation process of Schizonepeta Spike charcoal and improving the hemostatic effect and stability of the prepared Schizonepeta Spike charcoal slices have become technical problems that need to be solved urgently. Summary of the invention

[0009] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for preparing charcoal slices of Schizonepeta Spike and its products. The present invention can further increase the content of luteolin in the charcoal slices of Schizonepeta Spike by controlling the temperature and time of charcoal frying, improve the stability and safety of the prepared charcoal slices of Schizonepeta Spike, and better exert the hemostatic and anti-inflammatory effects of the charcoal slices of Schizonepeta Spike.

[0010] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0011] In a first aspect, the present invention provides a method for preparing charcoal slices of Schizonepeta spicate, the preparation method comprising: cleaning, cutting and charcoal-frying Schizonepeta spicate to obtain charcoal slices of Schizonepeta spicate.

[0012] The charcoal-roasting temperature is 200-320° C., and the charcoal-roasting time is 5-30 minutes.

[0013] Among them, the specific point values ​​in 200-320°C can be selected from 200°C, 220°C, 240°C, 260°C, 280°C, 300°C, 320°C, etc., and the specific point values ​​in 5-30min can be selected from 5min, 10min, 15min, 20min, 25min, 30min, etc.

[0014] The present invention controls the temperature and time of charcoal frying, while ensuring that the properties of the schizonepeta spicate charcoal slices are "black brown on the surface and burnt yellow on the inside", further increases the content of luteolin in the schizonepeta spicate charcoal slices, improves the stability and safety of the prepared schizonepeta spicate charcoal slices, and better exerts the hemostatic and anti-inflammatory effects of the schizonepeta spicate charcoal slices.

[0015] Preferably, said cleaning comprises removing impurities.

[0016] Preferably, the cutting comprises cutting the cleaned Nepeta spicate into Nepeta spicate segments with a length of 1 to 2 cm.

[0017] Among them, the specific point values ​​in 1 to 2 cm can be selected as 1 cm, 1.2 cm, 1.4 cm, 1.6 cm, 1.8 cm, 2 cm, etc.

[0018] Preferably, the cutting method includes dry cutting or wet cutting, preferably dry cutting.

[0019] The pharmacopoeia stipulates that the charcoal slices of Schizonepeta Spike need to be prepared from Schizonepeta Spike segments (Schizonepeta Spike slices). Therefore, during the segmentation process, it is necessary to ensure the stability of the medicinal properties of Schizonepeta Spike to avoid uncontrollable component changes during the segmentation process. Controlling the product quality of Schizonepeta Spike slices is crucial for the further preparation of Schizonepeta Spike charcoal slices.

[0020] In the present invention, the dry cutting method has the least effect on the components in the herbal medicine of Schizonepeta spicate, and can better ensure the stability of the herbal medicine before and after cutting, thereby improving the product quality of the herbal medicine of Schizonepeta spicate charcoal slices. At the same time, the dry cutting method greatly reduces the process difficulty and improves the preparation efficiency of the herbal medicine of Schizonepeta spicate charcoal slices.

[0021] Preferably, the charcoal roasting temperature is 290-310° C., and the charcoal roasting time is 8-13 minutes.

[0022] Among them, the specific point values ​​in 290-310℃ can be selected from 290℃, 293℃, 296℃, 299℃, 302℃, 305℃, 308℃, 310℃, etc., and the specific point values ​​in 8-13min can be selected from 8min, 8.5min, 9min, 9.5min, 10min, 10.5min, 11min, 11.5min, 12min, 12.5min, 13min, etc.

[0023] Furthermore, in the present invention, when the charcoal roasting temperature is controlled within the range of 290 to 310° C. and the charcoal roasting time is controlled within the range of 8 to 13 min, the content of luteolin in the charcoal slices of Schizonepeta spicata can be further increased.

[0024] Preferably, the preparation method further comprises cooling the schizonepeta spicate charcoal after charcoal roasting.

[0025] Preferably, the cooling temperature is 20-40°C, for example, 20°C, 25°C, 30°C, 35°C, 40°C, etc.

[0026] In a second aspect, the present invention provides a charcoal slice of Schizonepeta Spicae prepared by the preparation method of the charcoal slice of Schizonepeta Spicae as described in the first aspect.

[0027] Preferably, the mass percentage of luteolin in the dry product of the schizonepeta spicate charcoal slices is above 0.0025%, and the mass percentage of rosmarinic acid is between 0.010% and 0.060%.

[0028] Among them, the specific point values ​​above 0.0025% can be selected from 0.0025%, 0.0030%, 0.0035%, 0.0040%, 0.0045%, 0.0050%, 0.0055%, 0.0060%, etc., and the specific point values ​​between 0.010% and 0.060% can be selected from 0.010%, 0.020%, 0.030%, 0.040%, 0.050%, 0.060%, etc.

[0029] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] The present invention controls the temperature and time of charcoal frying, while ensuring that the properties of the schizonepeta spicate charcoal slices are "black brown on the surface and burnt yellow on the inside", further increases the content of luteolin in the schizonepeta spicate charcoal slices, improves the stability and safety of the prepared schizonepeta spicate charcoal slices, and better exerts the hemostatic and anti-inflammatory effects of the schizonepeta spicate charcoal slices; at the same time, the preparation method of the schizonepeta spicate charcoal slices provided by the present invention is suitable for large-scale production.

[0032] Furthermore, the dry cutting method can better ensure the stability of the medicinal material before and after cutting, avoid uncontrollable component changes during the cutting process, and thus improve the product quality of Schizonepeta Spike charcoal slices; at the same time, the dry cutting method greatly reduces the difficulty of the process and improves the preparation efficiency of Schizonepeta Spike charcoal slices. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a comparison of the liquid chromatography of the charcoal slices of Schizonepeta Spica before and after charcoal frying;

[0034] Figure 2 This is a comparison chart of the properties of three batches of Schizonepeta charcoal slices in Test Example 5. DETAILED DESCRIPTION

[0035] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0036] Example 1

[0037] This embodiment provides a method for preparing schizonepeta spicate decoction pieces, comprising the following steps:

[0038] (1) Purification: 500 g of Nepeta spicata medicinal material was placed on the unpacking table, and after manual selection, impurities were removed and soil was sieved off;

[0039] (2) Cutting into segments: Cut the dried Nepeta spicate into 1.5 cm Nepeta spicate segments (i.e. Nepeta spicate decoction pieces);

[0040] (3) Charcoal Stir-frying: Preheat the stir-frying pot to 300°C in advance, place the cut pieces of Schizonepeta Spike in the stir-frying pot and stir-fry continuously. The temperature for charcoal stir-frying is 300°C and the time is 10 min. If there are sparks during the stir-frying process, spray a little water to extinguish the sparks. After the set time is reached, discharge the material, cool it to 25°C, and add the material to obtain Schizonepeta Spike charcoal slices.

[0041] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0042] Example 2

[0043] This embodiment provides a method for preparing schizonepeta spicate decoction pieces, comprising the following steps:

[0044] (1) Cleaning: 500 g of the same batch of Nepeta spicata medicinal materials as in Example 1 were placed on an unpacking table, and after manual selection, impurities were removed and soil was sieved out;

[0045] (2) Cutting into segments: Cut the dried Nepeta spicate into 1.5 cm Nepeta spicate segments (i.e. Nepeta spicate decoction pieces);

[0046] (3) Stir-frying charcoal: preheat the stir-frying pot to 310°C in advance, place the cut pieces of Schizonepeta spicata in the stir-frying pot and stir-fry continuously. The temperature for charcoal stir-frying is 310°C and the time is 8 min. If there are sparks during the stir-frying process, spray a little water to extinguish the sparks. After the set time is reached, discharge the material, cool it to 25°C, and add the material to obtain the Schizonepeta spicata charcoal slices.

[0047] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0048] Example 3

[0049] This embodiment provides a method for preparing schizonepeta spicate decoction pieces, comprising the following steps:

[0050] (1) Cleaning: 500 g of the same batch of Nepeta spicata medicinal materials as in Example 1 were placed on an unpacking table, and after manual selection, impurities were removed and soil was sieved out;

[0051] (2) Cutting into segments: Cut the dried Nepeta spicate into 1.5 cm Nepeta spicate segments (i.e. Nepeta spicate decoction pieces);

[0052] (3) Stir-frying charcoal: preheat the stir-frying pot to 290°C in advance, place the cut pieces of Schizonepeta spicata in the stir-frying pot and stir-fry continuously. The temperature for charcoal stir-frying is 290°C and the time is 11 minutes. If there are sparks during the stir-frying process, spray a little water to extinguish the sparks. After the set time is reached, discharge the material, cool it to 25°C, and add the material to obtain the Schizonepeta spicata charcoal slices.

[0053] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0054] Example 4

[0055] This embodiment provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as in Embodiment 1. The only difference between this method and Embodiment 1 is that the charcoal-frying time in step (3) is adjusted to 15 min.

[0056] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0057] Example 5

[0058] This embodiment provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as in Embodiment 1. The only difference between this method and Embodiment 1 is that the charcoal-frying time in step (3) is adjusted to 5 min.

[0059] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0060] Example 6

[0061] The present embodiment provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as in Example 1. The method differs from Example 1 only in that the frying pan in step (3) is preheated to 250° C., the charcoal frying temperature is adjusted to 250° C., and the charcoal frying time remains at 10 min.

[0062] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0063] Example 7

[0064] The present embodiment provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as in Example 1. The method differs from Example 1 only in that the frying pan in step (3) is preheated to 315° C., the charcoal frying temperature is adjusted to 315° C., and the charcoal frying time remains at 10 min.

[0065] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0066] Example 8

[0067] The present embodiment provides a method for preparing charcoal slices of Schizonepeta spicate, which uses 500 g of Schizonepeta spicate medicinal materials from the same batch as in Example 1. The method differs from Example 1 only in that the cutting method in step (2) is adjusted to wet cutting, that is, the Schizonepeta spicate is soaked in water for 0.5 h, cut into 1.5 cm long segments, and then the cut Schizonepeta spicate is dried at 40° C. for 5 h to obtain Schizonepeta spicate segments.

[0068] Example 9

[0069] The present embodiment provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as in Example 1. The only difference between the present embodiment and Example 1 is that the cutting method in step (2) is adjusted to wet cutting, that is, the Schizonepeta spicata is sprayed with water 3 times the amount of the medicinal material, cut into 1.5 cm long segments, and then the cut Schizonepeta spicata is dried in the shade to obtain Schizonepeta spicata segments.

[0070] Comparative Example 1

[0071] This comparative example provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as Example 1. The difference between this method and Example 1 is that the frying pan in step (3) is preheated to 190°C, the charcoal frying temperature is adjusted to 190°C, and the charcoal frying time is adjusted to 23 minutes.

[0072] Before charcoal frying, the appearance of the Schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the Schizonepeta spicate charcoal was observed to be dark brown on the surface and burnt yellow on the inside.

[0073] Comparative Example 2

[0074] This comparative example provides a method for preparing charcoal slices of Schizonepeta spicata, which uses 500 g of Schizonepeta spicata medicinal materials from the same batch as Example 1. The difference between this method and Example 1 is that the frying pan in step (3) is preheated to 350°C, the charcoal frying temperature is adjusted to 350°C, and the charcoal frying time is adjusted to 2 min.

[0075] Before charcoal frying, the appearance of the schizonepeta spicate was observed to be yellow-green; after charcoal frying, the appearance of the schizonepeta spicate charcoal was observed to be dark brown both on the surface and inside.

[0076] Test Example 1

[0077] The contents of moisture, pulegone, luteolin and rosmarinic acid in the Schizonepeta spicate medicinal materials, Schizonepeta spicate segments and Schizonepeta spicate charcoal before and after cutting and charcoal frying were tested in accordance with the "Chinese Pharmacopoeia" 2020 edition, Part I, the "Schizonepeta spicate Segment Enterprise Internal Control Standards" and the "Schizonepeta spicate charcoal Enterprise Internal Control Standards".

[0078] (1) Content determination method:

[0079] (I) Moisture determination: The moisture content of Schizonepeta spicata charcoal was determined according to the second method of 0832 of the fourth volume of the 2020 edition of the Chinese Pharmacopoeia.

[0080] (II) Determination of pulegone content: refer to the method for determination of pulegone content under the item of content determination of Schizonepeta spicata medicinal materials in the 2020 edition of the Chinese Pharmacopoeia.

[0081] (III) Determination of luteolin and rosmarinic acid content: Determined by referring to the high performance liquid chromatography method (General Rule 0512 of the 2020 edition of the Chinese Pharmacopoeia):

[0082] ①Chromatographic conditions:

[0083] Octadecylsilane bonded silica gel was used as filler (particle size was 1.6 μm), the column length was 150 mm, the inner diameter was 2.1 mm. Acetonitrile was used as mobile phase A, 0.1% phosphoric acid water was used as mobile phase B, gradient elution was performed according to the provisions in the following table, the flow rate was 0.3 ml per minute, the column temperature was 40°C, the detection wavelength was 348 nm, and the theoretical plate number was calculated based on the luteolin peak and should be no less than 10,000.

[0084] Time (minutes) Mobile phase A (%) Mobile phase B (%) 0～2 7→18 93→82 2～15 18→25 82→75 15～19 25→32 75→68 19～21 32→7 68→93

[0085] ② Preparation of reference solution: Take appropriate amount of luteolin reference substance and rosmarinic acid reference substance, weigh accurately, add 70% ethanol to make a mixed solution containing 2μg luteolin and 40μg rosmarinic acid per 1ml, shake well, and obtain.

[0086] ③ Preparation of test solution: Take the Nepeta spicata decoction pieces and Nepeta spicata charcoal decoction pieces prepared in each embodiment and comparative example, crush and pass through a No. 3 sieve to obtain a powder; accurately weigh 2 g of the powder and place it in a stoppered conical flask, accurately add 25 ml of 70% ethanol, weigh the weight, ultrasonically treat (power 500 W, frequency 40 kHz) for 30 minutes, take out, cool, weigh again, make up the lost weight with 70% ethanol, shake well, filter, and take the filtrate to obtain.

[0087] ④ Accurately pipette 2 μl of the reference solution and the test solution respectively, inject them into the liquid chromatograph, and determine the contents of luteolin and rosmarinic acid in the test solution.

[0088] (2) Determination of the difference in component content before and after cutting

[0089] The contents of water, pulegone, luteolin and rosmarinic acid in the original medicinal material (Schizonepeta spicate) before cutting, and the contents of water, pulegone, luteolin and rosmarinic acid in the Schizonepeta spicate slices after cutting in Example 1, Example 8 and Example 9 were tested. The results are shown in the following table:

[0090]

[0091] By measuring the contents of Schizonepeta spicate and Schizonepeta spicate segments (Schizonepeta spicate decoction pieces) before and after cutting, it can be seen that the dry cutting method of Example 1 has the least effect on the components in the Schizonepeta spicate medicinal material, thus ensuring the stability of the medicinal material before and after cutting.

[0092] (3) Determination of the difference in component content before and after charcoal roasting

[0093] The changes in the contents of water, luteolin and rosmarinic acid before and after charcoal roasting of Examples 1 to 9 and Comparative Examples 1 to 2 were tested, and the results are shown in the following table:

[0094]

[0095] It can be seen from the data of Example 1 and Comparative Examples 1 to 2 that when the charcoal frying temperature is lowered to 190°C and the time is increased to 23 minutes, the appearance of the Schizonepeta Spike charcoal slices can also reach "black brown on the surface and burnt yellow on the inside", but the luteolin content in the Schizonepeta Spike charcoal slices is too low, which leads to a decrease in the hemostatic ability of the Schizonepeta Spike charcoal slices; when the charcoal frying temperature is increased to 350°C, the properties of the product change after 2 minutes, the surface and the inside are both black brown, and the carbonization is severe, which no longer meets the requirements for Schizonepeta Spike charcoal slices in the pharmacopoeia, and the luteolin content is severely reduced.

[0096] It can be seen from the data of Examples 1 and 4 to 7 that the appearance of the charcoal slices of Schizonepeta spicata is also ensured to be "dark brown on the surface and burnt yellow on the inside", and the charcoal frying temperature is controlled at 290 to 310°C and the time is controlled at 8 to 13 minutes, which can better increase the content of luteolin.

[0097] From the data of Examples 1, 8 and 9, it can be seen that charcoal roasting after dry cutting can further increase the content of luteolin in the charcoal slices of Schizonepeta Spike, which is beneficial for the charcoal slices of Schizonepeta Spike to exert their hemostatic effect.

[0098] (4) Comparison of liquid chromatograms before and after charcoal roasting

[0099] The spectra of the prepared charcoal slices of Schizonepeta spicata before and after charcoal frying are as follows: Figure 1 As shown, peak 1, peak 4, and peak 6 were identified as luteolin, rosmarinic acid, and luteolin by reference substances, respectively. By comparing the spectra obtained before and after charcoal frying, there were obvious differences in the components of the medicinal pieces before and after frying, with the luteolin content increasing and the rosmarinic acid content decreasing.

[0100] Test Example 2

[0101] The schizonepeta charcoal slices prepared in the embodiment and the comparative example were subjected to an accelerated 6-month conditional investigation at a temperature of 40°C ± 2°C and a relative humidity of 75% ± 5%. Samples were taken at 0 and 6 months, respectively, and the mass percentage of luteolin in the schizonepeta charcoal slices was detected using the same detection method as in Test Example 1. The results are shown in the following table:

[0102]

[0103]

[0104] It can be seen from the data of Example 1 and Comparative Examples 1 to 2 that when the charcoal roasting temperature is outside the range of 200 to 320°C, or the charcoal roasting time is outside the range of 5 to 30 min, the content of the active ingredient in the prepared Schizonepeta Spike charcoal slices will further decrease after being placed for 6 months.

[0105] It can be seen from the data of Examples 1 and 4 to 7 that the charcoal-frying temperature is controlled at 290 to 310° C. and the time is controlled at 8 to 13 min. The prepared charcoal slices of Schizonepeta spicata can be stored for a long time with good stability. After 6 months, the luteolin content still remains at a high level.

[0106] From the data of Examples 1 and 8 to 9, it can be seen that the content of luteolin in the charcoal slices of Schizonepeta spicata obtained by charcoal frying after wet cutting will further decrease after 6 months, indicating that the charcoal slices of Schizonepeta spicata prepared by this method have poor stability.

[0107] Test Example 3

[0108] In order to confirm the safety of the charcoal slices of Schizonepeta spicate prepared in different embodiments and comparative examples, this test example tested the cytotoxicity of the charcoal slices of Schizonepeta spicate prepared in each embodiment and comparative example, and determined the cell survival rate by MTT analysis.

[0109] (1) Preparation of Chinese herbal decoction: The pieces prepared in Examples 1 to 9 and Comparative Examples 1 to 2 were crushed respectively, and water 10 times the total mass of the Chinese herbal powder was added, and the mixture was soaked at room temperature for 6 h. After soaking, the mixture was heated to boiling, and the boiling was maintained for 1 h. The heating was stopped, the mixture was cooled, and the mixture was filtered with a filter cloth. The filtrate was collected to obtain the Chinese herbal decoction of the pieces prepared in Examples 1 to 9 and Comparative Examples 1 to 2.

[0110] (2) MTT analysis of each Chinese herbal decoction: HUVEC cells were used with 5×10 4The above cells were inoculated in a 96-well plate, with 4 replicate wells in each group, and the cells were cultured for 24 hours. Each treatment group was treated with the Chinese medicine decoction further prepared by Examples 1 to 9 and Comparative Examples 1 to 2 after 20 times dilution, and the control group was set to add the same volume of culture medium. After continuing to culture for 24 hours, 20 μL MTT at a concentration of 5 mg / ml was added to each well and continued to incubate for 4 hours. After terminating the culture, the culture supernatant in the well was carefully aspirated and discarded, 150 μL DMSO was added to each well, and the crystals were fully dissolved. A wavelength of 490 nm was selected to measure the light absorption value of each well on an enzyme-linked immunosorbent assay. Cell survival rate % = OD value of treatment group / OD value of control group × 100%. The survival rate of cells after treatment in each test group is shown in the following table:

[0111] sample Cell survival rate (%) Example 1 99.1 Example 2 98.3 Example 3 96.9 Example 4 95.4 Example 5 96.5 Example 6 95.8 Example 7 96.4 Example 8 94.3 Example 9 93.6 Comparative Example 1 96.2 Comparative Example 2 78.8

[0112] It can be seen from the above table that the charcoal slices of Schizonepeta Spike prepared by the preparation method of the charcoal slices of Schizonepeta Spike of the present invention are highly safe; the charcoal slices of Schizonepeta Spike obtained by charcoal frying at 350°C for 2 min in comparative example 2 have a dark brown surface and interior, and their safety is reduced to a certain extent.

[0113] Test Example 4

[0114] This test example adopts the preparation method of Example 1, cuts and stir-fries 15 batches of 500g of Nepeta spicata spicata charcoal, adopts the same detection method as Test Example 1, and compares the changes in the content of components before and after the Nepeta spicata charcoal processing with multiple batches of data. The specific data are shown in the following table:

[0115]

[0116]

[0117] From the above data, it can be seen that after the Nepeta spicate medicinal material is dry-cut into Nepeta spicate segments, there is no significant difference in the content of luteolin and rosmarinic acid; after charcoal frying, the luteolin content increases and the rosmarinic acid content decreases, but from the results of 15 batches of Nepeta spicate charcoal, the contents of luteolin and rosmarinic acid are relatively stable after frying, with mean ±30% of 0.036 mg / g~0.067 mg / g and 0.16 mg / g~0.30 mg / g, respectively, and mean ±3SD of 0 mg / g~0.103 mg / g and 0.05 mg / g~0.41 mg / g, respectively. The content fluctuation between batches is small, which further proves that the preparation process parameters of the present invention are relatively reasonable.

[0118] Test Example 5

[0119] This test example adopts the preparation method in Example 1, and uses production-scale equipment to cut and stir-fry three batches (K444YP01, K444YP02, K444YP03) of Schizonepeta spicata charcoal slices. Through process amplification and sample testing, the rationality of the preparation process of Schizonepeta spicata charcoal slices is further evaluated. The moisture content, luteolin content, and rosmarinic acid content are tested using the same detection method as in Test Example 1. The results are shown in the following table:

[0120]

[0121] In addition, the product properties of three batches of Schizonepeta charcoal slices were observed, such as Figure 2 As shown in the figure, the specifications of the three batches of Schizonepeta Spike Charcoal Slices are relatively consistent.

[0122] The test results show that the three batches of Schizonepeta spicate medicinal materials are dry cut into segments and then fried into charcoal, with the segmentation yield being above 99% and the charcoal fried yield being above 97%. The moisture content, luteolin content and rosmarinic acid content in the Schizonepeta spicate charcoal slices are all within the internal control standard range, and the product specifications of multiple batches of Schizonepeta spicate charcoal slices are relatively consistent, which proves that the preparation process parameters of the Schizonepeta spicate charcoal slices provided by the present invention are reasonable and suitable for mass production.

[0123] The applicant declares that the present invention illustrates the technical solution of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0124] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0125] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for preparing charcoal slices of Schizonepeta spicata, characterized in that: The preparation method comprises: cleaning, cutting and charring schizonepeta spicate to obtain schizonepeta spicate charcoal slices; The charcoal-roasting temperature is 200-320° C., and the charcoal-roasting time is 5-30 minutes.

2. The preparation method according to claim 1, characterized in that: The purification includes the removal of impurities.

3. The preparation method according to claim 1 or 2, characterized in that: The cutting comprises cutting the cleaned schizonepeta spicate into schizonepeta spicate segments with a length of 1 to 2 cm.

4. The preparation method according to any one of claims 1 to 3, characterized in that: The cutting method includes dry cutting or wet cutting, preferably dry cutting.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The charcoal-roasting temperature is 290-310° C., and the charcoal-roasting time is 8-13 minutes.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The preparation method further comprises cooling the schizonepeta spicate charcoal after charcoal frying.

7. The preparation method according to claim 6, characterized in that: The cooling temperature is 20-40°C.

8. A charcoal slice of Schizonepeta spicata prepared by the method for preparing charcoal slice of Schizonepeta spicata as claimed in any one of claims 1 to 7.

9. The charcoal slices of Schizonepeta spicata according to claim 8, characterized in that: The mass percentage of luteolin in the dry product of the schizonepeta spicate charcoal slices is above 0.0025%, and the mass percentage of rosmarinic acid is 0.010% to 0.060%.

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