Method for directional enrichment of chlorogenic acid components in honeysuckle flower
By performing directional dry heat treatment on honeysuckle powder, the problem of obtaining highly active chlorogenic acid components was solved, and the chlorogenic acid content was significantly improved, making it suitable for deep processing and high-value utilization of honeysuckle.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- EAST CHINA UNIV OF SCI & TECH
- Filing Date
- 2026-04-20
- Publication Date
- 2026-06-02
AI Technical Summary
In existing technologies, it is difficult to obtain highly active chlorogenic acid components, the component transformation in traditional thermal processing is uncontrollable, and the effective components are easily degraded, resulting in high costs, low yields, and unstable product quality.
By subjecting honeysuckle powder to dry heat treatment under constant temperature heating conditions, and setting different heating temperatures and times, the targeted enrichment of different chlorogenic acid components, including the enhancement of neochlorogenic acid, chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C, can be achieved.
Significant improvements in chlorogenic acid components have been achieved, particularly in the content of neochlorogenic acid (increased by more than 4%) and isochlorogenic acid B and isochlorogenic acid C (increased by more than 10%). The process is simple, low-cost, and easy to industrialize, yielding high-quality honeysuckle slices and functional food ingredients.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of traditional Chinese medicine processing and natural product chemistry technology, specifically relating to a method for targeted enrichment of chlorogenic acid components in honeysuckle. Background Technology
[0002] honeysuckle( Lonicerae japonicae Flos This is a traditional Chinese medicine that is also used in food. Its main active ingredients are chlorogenic acid compounds, including neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid (collectively known as monocaffeoylquinic acid), and isochlorogenic acids A, B, and C (collectively known as dicaffeoylquinic acid). Among them, isochlorogenic acid B and isochlorogenic acid C exhibit stronger antioxidant and antibacterial activities, and have higher application and development value.
[0003] Currently, the following technical bottlenecks exist in this field: (1) High acquisition cost: Highly active isochlorogenic acids B and C mainly rely on direct extraction from natural plants. Separation and purification are difficult, costly, and yield is low, which limits their pharmacological research and industrial application. (2) Lack of scientific basis for thermal processing: Dry heat is the core process link for processing, drying, and storing honeysuckle slices. However, the existing thermal processing parameters for drying and processing honeysuckle are crude, and there is a lack of systematic understanding of the overall transformation law of chlorogenic acid compounds under dry heat conditions. In particular, the mutual transformation relationship and degradation pathway between monocaffeoylquinic acid and dicaffeoylquinic acid are still unclear. (3) Easy loss of effective components: Due to the unclear transformation mechanism, the traditional heating process often leads to the degradation of effective components, especially chlorogenic acid and dicaffeoylquinic acid, resulting in unstable product quality and inability to achieve targeted enrichment of highly active components.
[0004] Therefore, developing a controllable thermal conversion process that can target and increase the content of specific chlorogenic acid components in honeysuckle is of great significance for the deep processing and high-value utilization of honeysuckle. Summary of the Invention
[0005] The present invention aims to provide a method for targeted enrichment of chlorogenic acid components in honeysuckle, in order to solve the technical problems of difficulty in obtaining highly active chlorogenic acid components, uncontrollable component transformation in traditional thermal processing, and easy degradation of effective components in the prior art.
[0006] To achieve the above objectives, the technical solution of the present invention is as follows: A method for targeted enrichment of chlorogenic acid components in honeysuckle includes the following steps: placing honeysuckle powder under constant temperature heating conditions for dry heat treatment, and setting different heating conditions according to different target enrichments; including the following condition settings: When the target enrichment is neochlorogenic acid, the heating conditions are: temperature 50~70℃, time 10~25min; When the target enrichment is neochlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 5~45min; When the target enrichment is neochlorogenic acid, chlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 50~75min; When the target enrichment is neochlorogenic acid, chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 80~120min; or, temperature 90~110℃, time 10~25min. When the target enrichment is chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C, the heating conditions are: temperature 90~110℃, time 25~120min; or, temperature 110~130℃, time 10~100min; or, temperature 130~170℃, time 10~30min. When the target enrichment is isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 110~130℃, time 110~130min; or, temperature 170~210℃, time 10~30min.
[0007] It should be noted that the content of different chlorogenic acid components in honeysuckle powder changes during dry heat treatment. Targeted enrichment refers to a significant improvement in the target component compared to the untreated sample. Based on the different chlorogenic acid components in the original honeysuckle powder, significant improvement is defined as an increase of ≥4% in chlorogenic acid content, ≥5% in neochlorogenic acid content, ≥10% in isochlorogenic acid B content, and ≥10% in isochlorogenic acid C content after dry heat treatment.
[0008] The present invention is further configured such that, when the target enrichment is neochlorogenic acid, the heating conditions are: temperature 55~65℃, time 10~20min.
[0009] The present invention is further configured such that when the target enrichment is neochlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 75~85℃, time 10~40min; preferably, temperature 75~85℃, time 15~35min.
[0010] The present invention is further configured such that when the target enrichment is neochlorogenic acid, chlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature of 75~85℃ and time of 55~70min; preferably, the temperature is 75~85℃ and the time is 55~65min.
[0011] The present invention is further configured such that when the target enriched substances are neochlorogenic acid, chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 75~85℃, time 80~120min, preferably temperature 75~85℃, time 90~120min; or temperature 95~105℃, time 10~20min.
[0012] The present invention is further configured such that, when the target enriched substances are chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C, the heating conditions are: a temperature of 90~110℃ and a time of 30~120 min; or, a temperature of 110~130℃ and a time of 15~100 min; or, a temperature of 130~160℃ and a time of 10~25 min, preferably a temperature of 135~160℃ and a time of 10~20 min.
[0013] The present invention is further configured such that when the target enriched substances are isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature of 115~125℃ and time of 110~130min; or, temperature of 175~205℃ and time of 10~25min, preferably temperature of 180~200℃ and time of 10~20min.
[0014] The present invention is further configured such that the honeysuckle powder is obtained by pulverizing honeysuckle slices and sieving them.
[0015] The present invention is further configured such that the honeysuckle powder is obtained by pulverizing honeysuckle slices and passing them through a 20-60 mesh sieve.
[0016] The present invention is further configured such that, after the honeysuckle powder undergoes dry heat treatment, it is rapidly cooled to room temperature to terminate the thermal reaction and lock in the product composition of the honeysuckle powder.
[0017] Compared with the prior art, the present invention has the following beneficial effects: The present invention innovatively proposes a method for the directional and efficient enrichment of effective components in honeysuckle tablets based on temperature control; and the process is simple, low-cost, does not require organic solvents to participate in the conversion process, is easy to operate, and is easy to scale up for industrial production; the directional enrichment product obtained by this method can be directly used as high-quality honeysuckle slices, functional food raw materials, or used to prepare high-purity chlorogenic acid reference standards and drug raw materials. Detailed Implementation
[0018] The present invention will be further illustrated below through embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the invention.
[0019] Example 1 The targeted enrichment of neochlorogenic acid components in honeysuckle powder includes the following process: Honeysuckle slices were pulverized using a traditional Chinese medicine pulverizer and passed through a 40-mesh sieve to obtain honeysuckle powder. 5g of honeysuckle powder was weighed and spread evenly in a glass petri dish (approximately 2mm thick), then placed in a vacuum drying oven preheated to 60℃. The dish was heated at 60℃ for 15 min. After heating, the petri dish was quickly transferred to a desiccator and cooled to room temperature. 0.1g of the cooled sample was taken and 10 mL of 80% (V / V) methanol aqueous solution was added. The sample was ultrasonically extracted (300 W, 40 kHz) for 60 min and then filtered. The filtrate was analyzed by HPLC and compared with the untreated control sample to detect changes in the content of various chlorogenic acid components in the honeysuckle powder. The results are shown in Table 1. Compared with the untreated control sample, the content of neochlorogenic acid increased by 11.40%, chlorogenic acid increased by 0.46%, isochlorogenic acid B increased by 1.63%, and isochlorogenic acid C increased by 6.6%. The "-" before the values in Table 1 indicates a decrease in content.
[0020] control group Compared to Example 1, the difference is that the honeysuckle powder was not subjected to dry heat treatment. Specifically, 0.1 g of honeysuckle powder sample was taken, 10 mL of 80% (V / V) methanol aqueous solution was added, and ultrasonic extraction was performed (300 W, 40 kHz) for 60 min, followed by filtration. The filtrate was analyzed by HPLC.
[0021] Example 2 The targeted enrichment of neochlorogenic acid and isochlorogenic acid C in honeysuckle powder includes the following process: Honeysuckle slices were pulverized using a traditional Chinese medicine pulverizer and passed through a 40-mesh sieve to obtain honeysuckle powder. 5g of honeysuckle powder was weighed and spread evenly in a glass petri dish (approximately 2mm thick), then placed in a vacuum drying oven preheated to 80℃. The dish was heated at 80℃ for 15 minutes. After heating, the petri dish was quickly transferred to a desiccator and cooled to room temperature. 0.1g of the cooled sample was taken and 10 mL of 80% (V / V) methanol aqueous solution was added. The sample was ultrasonically extracted (300 W, 40 kHz) for 60 minutes and then filtered. The filtrate was analyzed by HPLC and compared with the untreated control sample to detect changes in the content of various chlorogenic acid components in the honeysuckle powder. The results are shown in Table 1. Compared with the untreated control sample, the content of neochlorogenic acid increased by 10.1%, chlorogenic acid by 1.92%, isochlorogenic acid B by 2.20%, and isochlorogenic acid C by 17.03%.
[0022] Example 3 The targeted enrichment of neochlorogenic acid and isochlorogenic acid C components in honeysuckle powder included the following steps: Honeysuckle slices were pulverized using a traditional Chinese medicine pulverizer and passed through a 40-mesh sieve to obtain honeysuckle powder. 5g of honeysuckle powder was weighed and spread evenly in a glass petri dish (approximately 2mm thick), then placed in a vacuum drying oven preheated to 80℃. The dish was heated at 80℃ for 30min. After heating, the petri dish was quickly transferred to a desiccator and cooled to room temperature. 0.1g of the cooled sample was taken and 10 mL of 80% (V / V) methanol aqueous solution was added. The sample was ultrasonically extracted (300 W, 40 kHz) for 60min and then filtered. The filtrate was analyzed by HPLC and compared with the untreated control sample to detect changes in the content of each chlorogenic acid component in the honeysuckle powder. The results are shown in Table 1.
[0023] Example 4 The targeted enrichment of chlorogenic acid, neochlorogenic acid, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 3, except for the dry heat treatment time. In this example, the powder was heated at 80°C for 60 min, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0024] Example 5 The targeted enrichment of chlorogenic acid, neochlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 3, except for the dry heat treatment time. In this example, the powder was heated at 80°C for 90 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0025] Example 6 The targeted enrichment of chlorogenic acid, neochlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 3, except for the dry heat treatment time. In this example, the powder was heated at 80°C for 120 min, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0026] Example 7 The targeted enrichment of chlorogenic acid, neochlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder followed the same process as in Example 3, except for the dry heat treatment temperature and time. In this example, the powder was heated at 100°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0027] Example 8 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 7, except for the dry heat treatment time. In this example, the powder was heated at 100°C for 30 minutes, while the remaining operations were the same as in Example 7. The detection results are shown in Table 1.
[0028] Example 9 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 7, except for the dry heat treatment time. In this example, the powder was heated at 100°C for 60 min, while the remaining operations were the same as in Example 7. The detection results are shown in Table 1.
[0029] Example 10 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 7, except for the dry heat treatment time. In this example, the powder was heated at 100°C for 90 min, while the remaining operations were the same as in Example 7. The detection results are shown in Table 1.
[0030] Example 11 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 7, except for the dry heat treatment time. In this example, the powder was heated at 100°C for 120 min, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0031] Example 12 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 7, except for the dry heat treatment temperature and time. In this example, the powder was heated at a constant temperature of 120°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0032] Example 13 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 12, except for the dry heat treatment time. In this example, the dry heat treatment was carried out at a constant temperature of 120°C for 30 minutes, while the other operations were the same as in Example 12. The detection results are shown in Table 1.
[0033] Example 14 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 12, except for the dry heat treatment time. In this example, the dry heat treatment was carried out at a constant temperature of 120°C for 60 minutes, while the other operations were the same as in Example 12. The detection results are shown in Table 1.
[0034] Example 15 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 12, except for the dry heat treatment time. In this example, the dry heat treatment was carried out at a constant temperature of 120°C for 90 minutes, while the other operations were the same as in Example 12. The detection results are shown in Table 1.
[0035] Comparative Example 1 Compared with Example 12, the difference lies in the dry heat treatment time. In this example, the dry heat treatment is carried out at a constant temperature of 120°C for 5 minutes, while the other operations are the same as in Example 12. The test results are shown in Table 1.
[0036] Example 16 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 1, except for the dry heat treatment temperature. In this example, the dry heat treatment was carried out at a constant temperature of 140°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0037] Example 17 The targeted enrichment of chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C in honeysuckle powder was performed using a process different from that in Example 1, except for the dry heat treatment temperature. In this example, the dry heat treatment was carried out at 160°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0038] Example 18 The targeted enrichment of isochlorogenic acid B and isochlorogenic acid C in honeysuckle powder differed from that in Example 12 in that the dry heat treatment time was different. In this example, the powder was heated at a constant temperature of 120°C for 120 minutes, while the other operations were the same as in Example 12. The detection results are shown in Table 1.
[0039] Example 19 The targeted enrichment of isochlorogenic acid B and isochlorogenic acid C in honeysuckle powder differed from that in Example 1 in that the dry heat treatment temperature was different. In this example, the temperature was kept constant at 180°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0040] Example 20 The targeted enrichment of isochlorogenic acid B and isochlorogenic acid C in honeysuckle powder differed from that in Example 1 in that the dry heat treatment temperature was different. In this example, the temperature was kept constant at 200°C for 15 minutes, while the remaining operations were the same as in Example 2. The detection results are shown in Table 1.
[0041] Table 1. Changes in the content of each chlorogenic acid component in each example and comparative example compared to the control group.
[0042] The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be construed as limiting the scope of protection of the present invention. All equivalent transformations or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.
Claims
1. A method for targeted enrichment of chlorogenic acid components in honeysuckle, characterized in that, The process includes placing honeysuckle powder under constant temperature heating conditions for dry heat treatment, and setting different heating conditions according to different target concentrates; including the following condition settings: When the target enrichment is neochlorogenic acid, the heating conditions are: temperature 50~70℃, time 10~25min; When the target enrichment is neochlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 5~45min; When the target enrichment is neochlorogenic acid, chlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 50~75min; When the target enrichment is neochlorogenic acid, chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 70~90℃, time 80~120min; or, temperature 90~110℃, time 10~25min. When the target enrichment is chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C, the heating conditions are: temperature 90~110℃, time 25~120min; or, temperature 110~130℃, time 10~100min; or, temperature 130~170℃, time 10~30min. When the target enrichment is isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 110~130℃, time 110~130min; or, temperature 170~210℃, time 10~30min.
2. The method according to claim 1, characterized in that, When the target enrichment is neochlorogenic acid, the heating conditions are: temperature 55~65℃, time 10~20min.
3. The method according to claim 1, characterized in that, When the target enrichment is neochlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 75~85℃, time 10~40min.
4. The method according to claim 1, characterized in that, When the target enrichment is neochlorogenic acid, chlorogenic acid and isochlorogenic acid C, the heating conditions are: temperature 75~85℃, time 55~70min.
5. The method according to claim 1, characterized in that, When the target enrichment is neochlorogenic acid, chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature 75~85℃, time 80~120min; or temperature 95~105℃, time 10~20min.
6. The method according to claim 1, characterized in that, When the target enriched substances are chlorogenic acid, isochlorogenic acid B, and isochlorogenic acid C, the heating conditions are: temperature 90~110℃, time 30~120min; or temperature 110~130℃, time 15~100min; or temperature 130~160℃, time 10~25min.
7. The method according to claim 1, characterized in that, When the target enriched substances are isochlorogenic acid B and isochlorogenic acid C, the heating conditions are: temperature of 115~125℃ and time of 110~130min; or, temperature of 175~205℃ and time of 10~25min.
8. The method according to claim 1, characterized in that, The honeysuckle powder is obtained by crushing honeysuckle slices and sieving them.
9. The method according to claim 1, characterized in that, After the honeysuckle powder has undergone dry heat treatment, it needs to be rapidly cooled to room temperature to terminate the thermal reaction and lock in the product composition of the honeysuckle powder.