Safflower extract, safflower formula granules and preparation method

Abstract

The invention belongs to the technical field of traditional Chinese medicine preparation processing, and particularly relates to a safflower extract, safflower formula granules and a method for preparing the safflower extract and the safflower formula granules based on a pure electric drive evaporation low-temperature concentration technology. According to the preparation method of the safflower extract and the safflower formula granules, the safflower is extracted by adding water, and a pure electroconcentration technology is adopted, so that the content and the transfer rate of hydroxysafflor yellow A and kaempferol + 6-methoxy kaempferol in the safflower formula granules can be remarkably increased, the concentration temperature is low, the time is short, and the energy consumption is low.

Description

Technical Field

[0001] The present invention belongs to the technical field of traditional Chinese medicine preparation processing, and particularly relates to a safflower extract, safflower formula granules, and a method for preparing the safflower extract and safflower formula granules based on a pure-electric drive evaporation low-temperature concentration technology. Background Art

[0002] Traditional Chinese medicine formula granules are made from single herbs. After being processed into traditional Chinese medicine decoction pieces, they are prepared by water extraction, concentration, drying, and granulation, and are used for patients to take after being formulated in traditional Chinese medicine clinical prescriptions. The quality level of traditional Chinese medicine formula granules is usually evaluated by the consistency of three major indicators, namely, the extract yield, fingerprint or characteristic spectrum, and the transfer rate (or content) of main active ingredients, with the standard decoction (prepared by the preparation method of traditional Chinese medicine decoction).

[0003] Safflower is the dried flower of the plant Carthamus tinctorius L. of the genus Carthamus in the Compositae family. It has a pungent taste and a warm nature, and belongs to the heart and liver meridians. It has the effects of promoting blood circulation to remove blood stasis, dispersing stasis and relieving pain, etc. As a commonly used medicinal material, safflower not only has rich resources, but also has high medicinal value and low toxicity. Its main effects include antioxidant, anti-tumor, anti-inflammatory, anti-thrombotic and analgesic effects, and is widely used in clinical practice. It is reported that the chemical components of safflower mainly include flavonoids, polyynes, lignins, alkaloids, and water-soluble components safflower yellow pigments. In the current edition of the pharmacopoeia, safflower is used for quality control with hydroxysafflor yellow A and kaempferol as the index components.

[0004] In the existing production technology, the preparation process of safflower formula granules mainly adopts static decoction, vacuum concentration, and dry granulation. However, the heat stability of the index components hydroxysafflor yellow A and kaempferol in safflower is relatively poor. During the production of safflower formula granules, due to heat and long time in the concentration stage, the content loss of the index components is large, the transfer rate is low, deviating from the technical requirement range of the standard decoction, and the batch-to-batch difference is large, seriously affecting the product quality of safflower formula granules and the safety and effectiveness of clinical medication. Therefore, the industry has tried to control the content loss during the concentration process of safflower formula granule preparation to improve the product quality. However, in the current research on the preparation process of safflower formula granules, only simple preparation processes are often concerned, and there are no reports on the research of key processes affecting quality such as production stability. Therefore, the industry expects to develop a preparation process for safflower granules with higher active ingredients and better product quality. Summary of the Invention

[0005] Therefore, the technical problem to be solved by the present invention is to provide a safflower extract and a preparation method thereof, effectively solving the problem of large loss of safflower active ingredients;

[0006] The second technical problem to be solved by the present invention is to provide a safflower formula granule and its preparation method, which solves the problems of high energy consumption, unstable quality and low transfer rate of safflower formula granules, enables the content of active ingredients in safflower formula granules to continuously and stably reach a relatively high level, and improves the product quality of safflower formula granules.

[0007] To solve the above technical problems, a preparation method of a safflower extract described in the present invention includes the following steps:

[0008] (1) Take safflower and mix it with water at 98 - 100 °C, perform the first extraction on the safflower under a pressing state, and collect the first filtrate and the first filter residue;

[0009] (2) Transfer the first filtrate to a pure - electric concentration device for concentration to an extract, and that's it.

[0010] Specifically, in the preparation method of the safflower extract, in step (1), the amount of water added is 10 - 14 times the amount of safflower fed;

[0011] Preferably, the temperature of the first extraction step is 98 - 100 °C;

[0012] Preferably, the extraction time of the first extraction step is 25 - 35 min;

[0013] Preferably, the first extraction step includes the step of placing the safflower in a static extraction tank with a static pressing device.

[0014] Preferably, in the first extraction step, add 12 times the amount of water and extract at 100 °C for 30 minutes, then filter to obtain the first filtrate and the first filter residue.

[0015] In the first extraction step, since the texture of safflower slices is relatively light and it is easy to float after adding water, it is pressed after being put into a static extraction tank with a static pressing device, which can effectively guarantee the active ingredients of the safflower extract.

[0016] Specifically, in the preparation method of the safflower extract, in step (2), the pure - electric concentration device includes a double - effect concentration device with a pure - electric evaporation module.

[0017] Specifically, in the preparation method of the safflower extract, in step (2), the temperature of the concentration step is 50 - 65 °C;

[0018] Preferably, the relative density of the extract is controlled to be 1.02 - 1.12 g / ml in the concentration step.

[0019] Specifically, in the preparation method of the safflower extract, in step (1), it further includes the step of collecting the first filter residue, mixing it with water at 98 - 100 °C, and performing a second extraction;

[0020] Preferably, the addition amount of water is 8 - 12 times the amount of safflower charged;

[0021] Preferably, the temperature in the second extraction step is 98 - 100 °C;

[0022] Preferably, the extraction time in the second extraction step is 15 - 25 min.

[0023] Preferably, the time in the second extraction step is 20 minutes, the temperature is 100 °C, and the water addition amount for the second decoction is 10 times.

[0024] Specifically, in the method for preparing the safflower extract, in step (1), it further includes the step of collecting the second filter residue, mixing it with water at 98 - 100 °C, and performing a third extraction;

[0025] Preferably, the addition amount of water is 8 - 12 times the amount of safflower charged;

[0026] Preferably, the temperature in the third extraction step is 98 - 100 °C;

[0027] Preferably, the extraction time in the third extraction step is 15 - 25 min.

[0028] Preferably, the time for the third extraction is 20 minutes, the temperature is 100 °C, and the water addition amount for the third decoction is 10 times.

[0029] Specifically, in the method for preparing the safflower extract, in step (2), it further includes the step of combining the first filtrate with the second filtrate and / or the third filtrate.

[0030] The present invention also discloses a safflower extract prepared by the above method.

[0031] The present invention also discloses a safflower formula granule, comprising the safflower extract;

[0032] Preferably, the safflower formula granule further comprises a pharmaceutically acceptable excipient;

[0033] Preferably, the excipient includes a filler;

[0034] Preferably, the dosage of the filler accounts for 5 - 26 wt% of the total amount of the safflower formula granule;

[0035] Preferably, the filler includes maltodextrin and / or dextrin;

[0036] Preferably, based on 100 wt% of the safflower formula granule, it comprises 5 - 15 wt% of maltodextrin and 0 - 11 wt% of dextrin, and the balance is the safflower extract.

[0037] Preferably, for the safflower formula granules, the liquid extract is spray-dried with 10% (by the amount of medicinal materials) of maltodextrin. After the drying process and pulverization, the excipient added is dextrin, and the addition amount of dextrin is 0%-11% of the amount of the prepared granules.

[0038] The present invention also discloses a method for preparing the safflower formula granules, which includes the step of spray-drying the safflower extract to prepare a dry powder, and the step of adding the excipient for granulation.

[0039] Preferably, the method for preparing the safflower formula granules includes: taking a selected amount of the safflower extract and mixing it with the maltodextrin, then performing spray-drying to obtain a dry powder, pulverizing it, adding the dextrin and mixing for granulation, thus obtaining the safflower formula granules.

[0040] Preferably, the granulation is carried out by dry granulation, wet granulation or one-step granulation.

[0041] For the method for preparing the safflower extract of the present invention, safflower is extracted with water without using other organic solvents for extraction, which ensures the quality and safety of the safflower formula granules. Moreover, by extracting safflower three times, the contents and transfer rates of hydroxysafflor yellow A and kaempferol + 6-methoxykaempferol in the safflower formula granules can be significantly increased. For the extraction liquid of the method, a pure electric concentration technology is adopted, which can significantly increase the contents and transfer rates of hydroxysafflor yellow A and kaempferol + 6-methoxykaempferol in the safflower formula granules, with a low concentration temperature, short time and low energy consumption. The method for preparing the safflower extract of the present invention solves the problems of low production efficiency and poor product quality in the production process of traditional Chinese medicines with unstable index components, and the preparation process is simple and energy-consuming less. The contents and content transfer rates of hydroxysafflor yellow A and kaempferol + 6-methoxykaempferol in the obtained safflower extract are high, meeting the national standards for safflower formula granules. At the same time, the preparation process of the present invention is reasonably designed, simple, reliable and suitable for large-scale industrial production.

[0042] For the method for preparing the safflower extract of the present invention, in the exploration of a large amount of creative work, it is found that the number of decocting times, the multiple of water addition, the decocting time, the concentration method and temperature in the extraction process all affect the quality of the safflower formula granules. The present invention studies the number of decocting times, the multiple of water addition, the decocting time, the concentration method and temperature, solves the problems of low production efficiency and poor quality in the extraction process of the safflower extract, enables the contents of the safflower formula granules prepared thereby to continuously and stably reach a relatively high level, and improves the product quality of the safflower formula granules.

[0043] The preparation method of the safflower extract described in the present invention adopts pure electric concentration technology, which has remarkable energy-saving effects. It not only has mature technology and low operation and maintenance costs, but also has the advantages of safety and reliability, low noise, simple operation, low concentration temperature, and short time. The preparation method of the safflower extract described in the present invention adopts pure electric concentration technology, and uses pure electric concentration at a lower temperature, which has better protection for heat-sensitive materials, can reduce the loss of the content of active ingredients, and the content of the index components for preparing safflower formula granules is significantly increased compared with double-effect concentration, solving the problem of unstable quality of safflower formula granules.

[0044] The preparation method of the safflower formula granules described in the present invention optimizes the safflower extraction process and concentration process. In production, in addition to improving efficiency and reducing energy consumption, the key is to reduce the chemical degradation of hydroxysafflor yellow A and kaempferol + 6-methoxykaempferol. Combining the parameters of the extraction, concentration, drying, and granulation processes can continuously and stably produce safflower formula granules with a higher content of hydroxysafflor yellow A and kaempferol + 6-methoxykaempferol, improve the quality of safflower formula granules, and achieve the overall quality control of safflower formula granules. Specific embodiments

[0045] The present invention will be further described below through specific embodiments. The following examples are specific embodiments of the present invention, but the embodiments of the present invention are not limited by the following examples.

[0046] In the following examples of the present invention, the method for concentrating the safflower extract is on a pure electric concentration device. At present, the adaptable devices for pure electric drive evaporation low-temperature concentration technology include components such as heaters, evaporation chambers, condensers, separators, and compressors. It uses the compressor to work, discharges high-temperature and high-pressure freon gas, conducts heat exchange with the material in the heating chamber, the material evaporates, and the high-temperature and high-pressure freon gas releases heat and becomes a relatively high-temperature liquid. The relatively high-temperature freon liquid becomes a relatively low-temperature and low-pressure liquid through an electronic expansion valve. The low-temperature and low-pressure freon liquid conducts heat exchange with the secondary steam generated by evaporation in the condenser, absorbs heat, and becomes a relatively low-temperature and low-pressure gas (at the same time, the secondary steam is condensed), and then does work through the compressor and becomes high-temperature and high-pressure freon gas again.

[0047] In the following examples of the present invention, the method for concentrating the safflower extract is on a pure electric concentration device. The pure electric concentration device is a 3000L double-effect evaporator (3000-type double-effect pure electric evaporation module concentrator, vertical) of Lanwang Energy Saving Technology (Zhejiang) Co., Ltd., and the flow paste is concentrated under the condition of a concentration temperature of 50 - 65 °C.

[0048] Example 1

[0049] Take safflower medicinal materials, remove impurities, and prepare safflower decoction pieces. Take the safflower decoction pieces and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the third filtrate and the third filter residue.

[0050] Merge the above-mentioned first filtrate, second filtrate, and third filtrate, and transfer them to a pure electric concentration device for concentration. Control the concentration temperature at 55°C and the concentration time at 150 min until a thick extract with a relative density of 1.07 g / ml is obtained.

[0051] Take the above thick extract, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and carry out spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of the granules prepared, then it is obtained.

[0052] Example 2

[0053] Take safflower medicinal materials, remove impurities, and prepare safflower decoction pieces. Take the safflower decoction pieces and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the third filtrate and the third filter residue.

[0054] Merge the above-mentioned first filtrate, second filtrate, and third filtrate, transfer them to a pure electric concentration device for concentration. Control the concentration temperature at 60°C and the concentration time at 140 min until a thick extract with a relative density of 1.07 g / ml is obtained.

[0055] Take the above thick extract, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and carry out spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of the granules prepared, then it is obtained.

[0056] Example 3

[0057] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the third filtrate and the third filter residue.

[0058] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, transfer them to a pure electric concentration device for concentration, with a concentration temperature of 65°C and a concentration time of 120 min, until a thick extract with a relative density of 1.07 g / ml is obtained.

[0059] Take the above thick extract, add 10% (medicinal material amount) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin adjuvant, and the addition amount of dextrin is 5% of the amount of granules prepared, then it is obtained.

[0060] Example 4

[0061] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue.

[0062] Combine the above-mentioned first filtrate and second filtrate, transfer them to a pure electric concentration device for concentration, with a concentration temperature of 60°C and a concentration time of 125 min, until a thick extract with a relative density of 1.07 g / ml is obtained.

[0063] Take the above thick extract, add 10% (medicinal material amount) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin adjuvant, and the addition amount of dextrin is 5% of the amount of granules prepared, then it is obtained.

[0064] Example 5

[0065] Take the safflower medicinal material, remove impurities, and prepare safflower decoction pieces. Take the safflower decoction pieces and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 14 times the amount of water at 98°C, control the extraction temperature at 98°C and extract for 35 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 8 times the amount of water at 98°C, control the extraction temperature at 98°C and extract for 25 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 8 times the amount of water at 98°C, control the extraction temperature at 98°C and extract for 25 minutes, then filter to obtain the third filtrate and the third filter residue.

[0066] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, transfer them to a pure electric concentration device for concentration, with a concentration temperature of 60°C, until a thick extract with a relative density of 1.02 g / ml is obtained.

[0067] Take the above thick extract, add 5% (by the amount of the medicinal material) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin adjuvant, and the addition amount of dextrin is 11% of the amount of the granules prepared, and then it is obtained.

[0068] Example 6

[0069] Take the safflower medicinal material, remove impurities, and prepare safflower decoction pieces. Take the safflower decoction pieces and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 10 times the amount of water at 99°C, control the extraction temperature at 99°C and extract for 25 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 12 times the amount of water at 99°C, control the extraction temperature at 99°C and extract for 15 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 12 times the amount of water at 99°C, control the extraction temperature at 99°C and extract for 15 minutes, then filter to obtain the third filtrate and the third filter residue.

[0070] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, transfer them to a pure electric concentration device for concentration, with a concentration temperature of 60°C, until a thick extract with a relative density of 1.12 g / ml is obtained.

[0071] Take the above thick extract, add 15% (by the amount of the medicinal material) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin adjuvant, and the addition amount of dextrin is 1% of the amount of the granules prepared, and then it is obtained.

[0072] Comparative Example 1

[0073] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 20 minutes, then filter to obtain the third filtrate and the third filter residue.

[0074] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, and transfer them to a single-effect steam evaporation and concentration device for concentration. Control the concentration temperature at 70 °C and the concentration time at 180 min until a paste with a relative density of 1.07 g / ml is obtained.

[0075] Take the above-mentioned paste, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of granules prepared, then it is obtained.

[0076] Comparative Example 2

[0077] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 30 minutes, then filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 20 minutes, then filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100 °C, control the extraction temperature at 100 °C and extract for 20 minutes, then filter to obtain the third filtrate and the third filter residue.

[0078] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, and transfer them to a single-effect steam evaporation and concentration device for concentration. Control the concentration temperature at 80 °C and the concentration time at 148 min until a paste with a relative density of 1.07 g / ml is obtained.

[0079] Take the above-mentioned paste, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and perform spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of granules prepared, then it is obtained.

[0080] Comparative Example 3

[0081] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device. Under static pressing, mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 30 minutes, filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 20 minutes, filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 20 minutes, filter to obtain the third filtrate and the third filter residue.

[0082] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, and transfer them to a double-effect steam evaporation and concentration equipment for concentration. Control the concentration temperature at 85°C and the concentration time at 100 min until a flowable paste with a relative density of 1.07 g / ml is obtained.

[0083] Take the above-mentioned flowable paste, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and carry out spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of the prepared granules, then it is obtained.

[0084] Comparative Example 4

[0085] Take safflower medicinal materials, remove impurities, and prepare safflower slices. Take the safflower slices and put them into a static extraction tank with a static pressing device, but do not perform static pressing. Mix with 12 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 30 minutes, filter to obtain the first filtrate and the first filter residue respectively; take the first filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 20 minutes, filter to obtain the second filtrate and the second filter residue; take the second filter residue, mix with 10 times the amount of water at 100°C, control the extraction temperature at 100°C for extraction for 20 minutes, filter to obtain the third filtrate and the third filter residue.

[0086] Combine the above-mentioned first filtrate, second filtrate, and third filtrate, and transfer them to a pure electric concentration equipment for concentration. Control the concentration temperature at 55°C and the concentration time at 150 min until a flowable paste with a relative density of 1.07 g / ml is obtained.

[0087] Take the above-mentioned flowable paste, add 10% (by the amount of medicinal materials) of maltodextrin, mix well and carry out spray drying. After the drying process is pulverized, add dextrin auxiliary materials, and the addition amount of dextrin is 5% of the amount of the prepared granules, then it is obtained.

[0088] Experimental Example

[0089] 1. Detection of the content of active ingredients

[0090] Respectively take the safflower formula granules prepared in Examples 1-4 and Comparative Examples 1-3 above, determine the contents of hydroxysafflor yellow A, kaempferol + 6-methoxykaempferol, and calculate their paste yield and transfer rate.

[0091] In this experimental example, the content of hydroxysafflor yellow A in safflower medicinal materials in each example and comparative example was determined with reference to the standards of the 2020 edition of the Chinese Pharmacopoeia. For the determination of the total content of kaempferol + 6-methoxykaempferol in safflower medicinal materials, the reference is: Wei Jiabao, Tang Shuangyan, Zhao Weizhi, et al. Discussion on the Determination of Kaempferol Content in Safflower in the 2020 Edition of the Chinese Pharmacopoeia [J]. Chinese Pharmaceutical Standards, 2023, 24(03): 281-288.

[0092] For the obtained safflower formula granules, the content of hydroxysafflor yellow A, the total content of kaempferol + 6-methoxykaempferol (refer to the national standard YBZ-PFKL-2022022), the initial feeding amount of safflower medicinal materials was weighed, the weight of the obtained extract powder after drying, and the weight of the obtained safflower formula granules were measured. The extract yield was measured and calculated, and the granule yield, the transfer rate of hydroxysafflor yellow A in granules, and the total transfer rate of kaempferol + 6-methoxykaempferol in granules were calculated to judge the quality of the obtained safflower formula granules.

[0093] The calculation formulas for each data are as follows:

[0094] Extract yield = weight of dried extract powder / initial feeding amount of safflower medicinal materials × 100% - proportion of dried excipients;

[0095] Yield = weight of dried powder / initial feeding amount of safflower medicinal materials × 100%;

[0096] Granule yield = weight of safflower formula granules / initial feeding amount of safflower medicinal materials × 100%;

[0097] Transfer rate of hydroxysafflor yellow A in granules = content of hydroxysafflor yellow A in granules (mg / g) × granule yield / content of hydroxysafflor yellow A in medicinal materials (%) / 1000 × 100%;

[0098] Total transfer rate of kaempferol + 6-methoxykaempferol in granules = total content of kaempferol + 6-methoxykaempferol in granules (mg / g) × granule yield / total content of kaempferol + 6-methoxykaempferol in medicinal materials (%) / 1000 × 100%.

[0099] In this experimental example, the judgment criteria for the quality of safflower formula granules (refer to the national standard YBZ-PFKL-2022022) are as follows: the extract yield ranges from 28% to 35.5%, the content of hydroxysafflor yellow A ranges from 16.5 to 37.0 mg / g, and the total content of kaempferol + 6-methoxykaempferol ranges from 0.60 to 1.80 mg / g; if the extract yield or content is not within the range, it is unqualified, and if both the extract yield and content are within the range, it is qualified.

[0100] The specific results are shown in Table 1.

[0101] Comparison of Results between the Examples and Comparative Examples of Safflower Formula Granules

[0102]

[0103]

[0104]

[0105] As can be seen from the above table, in the safflower formula granule product of the present invention, the number of times of safflower extraction for preparing the safflower extract, whether extraction is pressed, the concentration method and temperature all have an impact on the quality of safflower formula granules.

[0106] From the results of Example 2 and Example 4, it can be seen that with the concentration method being pure electric concentration at 60°C, the number of decoction times has a greater impact on the content and transfer rate of the granules. The paste yield increases by 12% and the transfer rates increase by 19% and 11% respectively when decocting three times compared to twice.

[0107] From the results of Example 1, Example 2 and Example 3, it can be seen that when the concentration temperature is increased from 55°C to 65°C, the concentration duration is reduced but the content is also correspondingly reduced, indicating that the concentration temperature has an impact on the quality of safflower formula granules.

[0108] From the results of Example 2 and Example 5, it can be seen that adjusting the water addition amount and decoction temperature has a relatively small impact on the quality of safflower formula granules; from the results of Example 2 and Example 6, it can be seen that adjusting the water addition amount, decoction temperature and increasing the paste density have a greater impact on the content and transfer rate of safflower formula granules, but the safflower formula granules are qualified.

[0109] From the results of Example 1 and Comparative Example 1, it can be seen that when the concentration method is changed to single-effect concentration at 70°C, the concentration duration is prolonged and the efficiency is reduced, and the content and transfer rate are also reduced; while comparing Comparative Example 2 and Comparative Example 3, it can be seen that with single-effect and double-effect concentration methods and continuous increase in the concentration temperature, the content and transfer rate continue to decrease, and the safflower formula granules are unqualified.

[0110] From the results of Example 1 and Comparative Example 4, it can be seen that changing the extraction pressing to non-pressing has a relatively small impact on the content and transfer rate of hydroxysafflor yellow A in safflower formula granules, but has a greater impact on the total content and transfer rate of kaempferol + 6-methoxykaempferol, and the safflower formula granules are unqualified.

[0111] It can be seen that for the safflower formula granule of the present invention, in the process of preparing the safflower extract, the method of preparing the safflower formula granule by the pure-electric-driven evaporation low-temperature concentration technology can, with the characteristics of lower temperature, shorter duration and lower energy consumption, improve the transfer rate of hydroxysafflor yellow A and the total transfer rate of kaempferol + 6-methoxykaempferol, reduce the degradation of its components, make the content of hydroxysafflor yellow A and the total content of kaempferol + 6-methoxykaempferol in the safflower formula granule reach a relatively high level, and can output stably, thus improving the product quality of the safflower formula granule.

[0112] Obviously, the above embodiments are merely examples given for clear illustration and are not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or modifications derived therefrom still fall within the protection scope of the present invention.

Claims

1. A method for preparing safflower extract, characterized in that, It includes the following steps: (1) Take safflower, add water at 98 - 100 °C and mix. Conduct the first extraction on the safflower under a pressing state, and collect the first filtrate and the first filter residue; (2) Transfer the first filtrate to a pure - electric concentration device for concentration to an extract, and that's it.

2. The preparation method of the safflower extract according to claim 1, characterized in that, In the step (1), the addition amount of the water is 10 - 14 times the feeding amount of the safflower; Preferably, the temperature of the first extraction step is 98 - 100 °C; Preferably, the extraction time of the first extraction step is 25 - 35 min; Preferably, the first extraction step includes the step of placing the safflower in a static extraction tank with a static pressing device.

3. The preparation method of the safflower extract according to claim 1 or 2, characterized in that In the step (2), the pure - electric concentration device includes a double - effect concentration device with a pure - electric evaporation module.

4. The preparation method of the safflower extract according to claim 3, characterized in that, In the step (2), the temperature of the concentration step is 50 - 65 °C; Preferably, the relative density of the extract is controlled to be 1.02 - 1.12 g / ml in the concentration step.

5. The preparation method of the safflower extract according to any one of claims 1-4, characterized in that, In the step (1), it also includes the step of collecting the first filter residue, adding water at 98 - 100 °C and mixing, and conducting the second extraction; Preferably, the addition amount of the water is 8 - 12 times the feeding amount of the safflower; Preferably, the temperature of the second extraction step is 98 - 100 °C; Preferably, the extraction time of the second extraction step is 15 - 25 min.

6. The preparation method of the safflower extract according to claim 5, characterized in that, In the step (1), it also includes the step of collecting the second filter residue, adding water at 98 - 100 °C and mixing, and conducting the third extraction; Preferably, the addition amount of the water is 8 - 12 times the feeding amount of the safflower; Preferably, the temperature of the third extraction step is 98 - 100 °C; Preferably, the extraction time of the third extraction step is 15 - 25 min.

7. The preparation method of safflower extract according to claim 5 or 6, characterized in that, In the step (2), it also includes the step of combining the first filtrate with the second filtrate and / or the third filtrate.

8. A safflower extract prepared by the method according to any one of claims 1 - 7.

9. A safflower formula granule, characterized in that, It includes the safflower extract according to claim 8; Preferably, the safflower formula granules further include pharmaceutically acceptable excipients; Preferably, the excipients include fillers; Preferably, the dosage of the filler accounts for 5 - 26 wt% of the total amount of the safflower formula granules; Preferably, the filler includes maltodextrin and / or dextrin; Preferably, based on the safflower formula granules being 100 wt%, it includes 5 - 15 wt% of maltodextrin and 0 - 11 wt% of dextrin, and the balance is the safflower extract.

10. A method for preparing the safflower formula granules according to claim 9, characterized in that, It includes the step of spray - drying the safflower extract to prepare a dry powder, and the step of adding the excipients for granulation; Preferably, the preparation method of the safflower formula granules includes: taking a selected amount of the safflower extract, mixing it with the maltodextrin, then conducting spray - drying to obtain a dry powder, pulverizing it, adding the dextrin, mixing and granulating, and that's it.

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