Compound oplopanax elatus nakai essential oil with bacteriostatic activity and preparation method thereof
By detecting the effective ingredients of Northeast Pillaria ginseng leaves and preparing compound essential oils, the problem of inadequate utilization of the medicinal value of Northeast Pillaria ginseng was solved, the effective utilization of its leaves and the antibacterial activity of compound essential oils were achieved, and the sustainable development of medicinal resources was promoted.
Patent Information
- Application Number
- CN202411947489.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-04-04
AI Technical Summary
The development and utilization of Northeast Pillar Ginseng is limited by the problems of its low fruiting rate and depletion of wild resources. The existing research mainly focuses on its rhizomes, and there are few studies on leaves in non-traditional medicinal areas, resulting in the inadequate use of its medicinal value.
By picking Northeast Pinnacle Ginseng leaves at different times, using gas chromatography and mass spectrometry combined technology for active ingredient detection, and compound essential oils with antibacterial activity were prepared, including Northeast Pinnacle Ginseng Essential Oil, Red Pinnacle Essential Oil, patchouli Essential Oil, Lavender Essential Oil, Geranium Essential Oil, Jojoba Essential Oil and Grape Seed Oil.
The effective utilization of Northeast Pinnacle Ginseng leaves has been achieved. Compound essential oil has strong antibacterial ability to E. coli, Staphylococcus aureus, Candida albicans, and Bacillus aeruginosa, which has improved the comprehensive utilization rate of Northeast Pinnacle Ginseng and is of great significance to the sustainable development of medicinal resources.
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Abstract
Description
Technical Field
[0001] The invention belongs to the extraction and application technology of effective components of Panax notoginseng, and in particular designs a Panax notoginseng compound essential oil with antibacterial activity and a preparation method thereof. Technical Background
[0002] Northeastern spiny ginseng is a plant of the genus Panax notoginseng of the Araliaceae family, also known as spiny ginseng. It has the effects of replenishing qi and yang, relieving fever and relieving pain, and has significant results in the treatment of neurasthenia, depression, rheumatism, dermatophytes, hypotension, impotence and other diseases. It is a precious medicinal plant with great development value. As a rare medicinal material in the Changbai Mountain area, it has attracted more and more attention from researchers in recent years because of its ginseng-like effects. Related reports show that more than 400 compounds have been found in Northeastern spiny ginseng, including saponins, phenolic acids, flavonoids, volatile oils, etc. Among them, saponins and flavonoids are present in leaves, while phenolic acids, anthraquinones and fatty acids are mainly present in roots and stems, and volatile oils are more present in roots and stems. On this basis, modern pharmacological studies have confirmed that these ingredients have good therapeutic effects in antifungal, anti-inflammatory, antioxidant, anti-fatigue, anti-cancer and central nervous system regulation. However, because the Northeastern spiny ginseng has been growing in a cold environment for a long time, its fruiting rate is very low, the natural growth of its population is restricted, and wild resources are becoming increasingly depleted, which seriously hinders the development and utilization of the Northeastern spiny ginseng.
[0003] Northeastern spiny ginseng is a deciduous shrub, less than 2 meters tall. Single leaves are alternate, petioles are 4-10 cm long, densely covered with thorns, base is enlarged and phimosis, leaves are palmately 3-5 shallowly lobed, thin in texture, 10-20 cm long, about 15-25 cm wide, heart-shaped at the base, with irregular serrations and prickles on the edges, dark green on the surface, light green on the back, protruding main veins along the veins with dense yellow prickles of different sizes, and the effective components accumulated in its leaves will change with the growth period. However, most of the research focuses on roots and rhizomes, and the survival status of Northeastern spiny ginseng is difficult to provide large-scale medicinal use, and there is still a certain gap from realizing its large-scale artificial cultivation, which seriously inhibits its medicinal value as a Chinese herbal medicine; therefore, it is necessary to explore the feasibility of its non-traditional medicinal parts leaves as new medicinal parts resources, and provide a reference for exploring the potential value of its non-medicinal parts. In addition, the research on the effective components of Northeastern spiny ginseng is not comprehensive, and how to further explore the effective components of Northeastern spiny ginseng and improve its medicinal value has become one of the hot topics studied by scientific researchers in this field.
[0004] Up to now, most of the research on the northeastern spiny ginseng has focused on the analysis of rhizomes and the cultivation technology of adventitious roots, but there are few reports on the leaves of the northeastern spiny ginseng. Therefore, this study used the picking time as an influencing factor to qualitatively and quantitatively analyze the various effective components such as saponins, phenolic acids, flavonoids, and volatile oils in the leaves of non-traditional medicinal parts. At the same time, considering the practicality, the northeastern spiny ginseng compound essential oil with antibacterial effect was developed with volatile oil as the main raw material, which fully improved the comprehensive utilization rate of the northeastern spiny ginseng and has important significance for the sustainable development of endangered medicinal resources and the development and utilization of medicinal resources. Summary of the invention
[0004] In order to solve the above problems, the present invention provides a compound essential oil of Panax notoginseng with antibacterial activity and a preparation method thereof.
[0005] In order to achieve the above-mentioned object, the present invention provides a compound essential oil of Panax notoginseng with antibacterial activity, wherein the Panax notoginseng essential oil is extracted from Panax notoginseng leaves and mixed with other essential oils, and the other essential oils include red pine essential oil, patchouli essential oil, lavender essential oil, geranium essential oil and base oil (jojoba oil and grape seed oil).
[0006] Furthermore, the leaves of the Panax ginseng are picked at different times, and their effective components are detected and analyzed by gas chromatography-mass spectrometry.
[0006] Furthermore, the method for preparing the compound essential oil of Panax notoginseng having antibacterial activity comprises the following steps: (1) The samples were collected from the Northeastern ginseng cultivation base in Changbai County, Jilin Province on June 20, July 10, August 4, September 1, and September 22, 2020; (2) The sample was prepared into coarse powder of Panax ginseng leaves by a grinder; (3) taking an appropriate amount of the coarse powder in step (2) and placing it in a round-bottom flask, adding an appropriate amount of distilled water and zeolite; (4) installing a volatile oil extraction device according to the requirements of steam distillation extraction in the pharmacopoeia, and extracting by steam distillation until the amount of volatile oil no longer increases, and obtaining a light yellow oily liquid with a special aroma; (5) Add appropriate amount of anhydrous sodium sulfate to dry, let stand and stratify, collect the essential oil and store in a dark place.
[0008] Preferably, the samples described in step (1) are all collected from mature, fresh, insect-free, and hole-free leaves. After removing impurities such as branches, bark, and weeds from the leaves, the leaves are placed in a ventilated and cool place for use.
[0009] Preferably, in step (2), the rotation speed of the pulverizer is 500-1000 r / min, the stirring time is 1-3 min, and the temperature is 25°C.
[0010] Preferably, in step (3), the mass ratio of the coarse powder of Panax ginseng leaves to water is 1:5 to 1:10.
[0011] Preferably, in step (4), the heating distillation time is 6 to 12 hours.
[0012] Preferably, in step (5), the static stratification time is 0.5 h to 3 h.
[0013] Further, the compound essential oil contains one or more of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, geranium essential oil, jojoba oil, and grape seed oil, that is, the Panax notoginseng compound essential oil is composed of Panax notoginseng essential oil, other essential oils and base oil, for example, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, geranium essential oil, jojoba essential oil and grape seed oil; or, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, jojoba oil, and grape seed oil; or, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, jojoba oil, and grape seed oil, but is not limited to the above examples.
[0014] Furthermore, the compound essential oil comprises, by volume percentage, 9% to 15% of Panax notoginseng essential oil, 12% to 15% of Korean pine essential oil, 3% to 6% of patchouli essential oil, 0% to 3% of lavender oil, 0% to 3% of geranium essential oil, 50% of jojoba oil and 20% of grape seed oil.
[0015] Furthermore, the preparation method of the compound essential oil is: taking each essential oil raw material by volume, mixing them evenly, and then ultrasonicating them at a power of 100-200w for 1-3min.
[0016] Compared with the prior art, the present invention has the following advantages and technical effects:
[0017] (1) The present invention uses the leaves of the northeastern thorny ginseng for the first time to extract volatile oil, and performs component detection, and then prepares a compound essential oil. The northeastern thorny ginseng compound essential oil has a strong antibacterial ability against Escherichia coli, Staphylococcus aureus, Candida albicans, and Bacillus aeruginosa. Therefore, the present invention realizes the effective utilization of the leaves of the northeastern thorny ginseng, and the northeastern thorny ginseng compound essential oil has great potential in antibacterial.
[0018] (2) The raw material compound essential oil of the present invention is all from natural plants, has good broad-spectrum antibacterial activity, and most of the essential oils have pleasant aroma, and are green, safe, and have few side effects. The compound essential oil can exert a good antibacterial effect through the synergistic effect of the active ingredients, and has broad market prospects and application potential in the preparation of the Northeastern spiny ginseng compound essential oil.
[0019] (3) The compound essential oil of the present invention is prepared from essential oils of natural plant sources, and has a rich and sweet overall aroma, and has the characteristics of coolness, floral fragrance, grass fragrance and other rhymes. The aroma is harmonious and pleasant, and it can achieve common antibacterial effect with significant antibacterial effect. No toxic chemicals such as ethanol, chlorophenol, and xylenol are contained in the entire preparation process, and it is a more sustainable, healthy and environmentally friendly compound essential oil. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] The drawings constituting a part of the present application are used to provide a further understanding of the present application. The illustrative embodiments and descriptions of the present application are used to explain the present application and do not constitute an improper limitation on the present application. In the drawings:
[0021] Figure 1 GC-MS spectra of the leaves of Panax ginseng at different stages in Example 1 of the present invention. DETAILED DESCRIPTION
[0022] Since the compound essential oil prepared by the present invention differs only in the ingredients and the percentage of each ingredient, the preparation process of the compound essential oil is explained by taking the formula of 9% Panax notoginseng essential oil + 15% Korean pine essential oil + 3% patchouli essential oil + 3% lavender oil + 50% jojoba oil + 20% grape seed oil as an example. (1) The samples were collected from the Northeastern ginseng cultivation base in Changbai County, Jilin Province on June 20, July 10, August 4, September 1, and September 22, 2020; (2) The sample was prepared into coarse powder of Panax ginseng leaves by a grinder; (3) taking an appropriate amount of the coarse powder in step (2) and placing it in a round-bottom flask, adding an appropriate amount of distilled water and zeolite; (4) installing a volatile oil extraction device according to the requirements of steam distillation extraction in the pharmacopoeia, and extracting by steam distillation until the amount of volatile oil no longer increases, and obtaining a light yellow oily liquid with a special aroma; (5) Add appropriate amount of anhydrous sodium sulfate to dry, let stand and stratify, collect the essential oil and store in a dark place. (6) adding red pine essential oil, patchouli essential oil, lavender oil, jojoba oil and grape seed oil to the volatile oil of Panax notoginseng and mixing them by ultrasound to obtain Panax notoginseng compound essential oil.
[0023] Preferably, the samples described in step (1) are all collected from mature, fresh, insect-free, and hole-free leaves. After removing impurities such as branches, bark, and weeds from the leaves, the leaves are placed in a ventilated and cool place for use.
[0024] Preferably, in step (2), the rotation speed of the pulverizer is 500-1000 r / min, the pulverizing time is 1-3 min, and the temperature is 25°C.
[0025] Preferably, in step (3), the mass ratio of the coarse powder of Panax ginseng leaves to water is 1:5 to 1:10.
[0026] Preferably, in step (4), the heating distillation time is 6 to 12 hours.
[0027] Preferably, in step (5), the static stratification time is 0.5 h to 3 h.
[0028] Further, the compound essential oil contains one or more of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, geranium essential oil, jojoba oil, and grape seed oil, that is, the Panax notoginseng compound essential oil is composed of Panax notoginseng essential oil, other essential oils and base oil, for example, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, geranium essential oil, jojoba essential oil and grape seed oil; or, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, lavender oil, jojoba oil, and grape seed oil; or, the compound essential oil is composed of Panax notoginseng essential oil, Korean pine essential oil, patchouli essential oil, jojoba oil, and grape seed oil, but is not limited to the above examples.
[0029] Furthermore, the compound essential oil comprises, by volume percentage, 9% to 15% of Panax notoginseng essential oil, 12% to 15% of Korean pine essential oil, 3% to 6% of patchouli essential oil, 0% to 3% of lavender oil, 0% to 3% of geranium essential oil, 50% of jojoba oil and 20% of grape seed oil.
[0030] Furthermore, the preparation method of the compound essential oil is: taking each essential oil raw material by volume, mixing them evenly, and then ultrasonicating them at a power of 100-200w for 1-3min. Ingredient Identification Test
[0031] Detection of effective ingredients in the leaves of Panax ginseng at different periods. The samples were taken from the Panax ginseng cultivation base in Changbai County, Jilin Province. The collection times were June 20, July 10, August 4, September 1, and September 22, 2020, and were marked as samples A, B, C, D, and E, respectively.
[0032] The components of samples A, B, C, D and E were analyzed by gas chromatography-mass spectrometry, and the detected chromatographic peaks were retrieved by referring to the identification methods of predecessors and previous studies in combination with the mass spectrometry library, and analyzed in combination with relevant literature. The total ion current chromatograms of volatile oils from leaves at different stages are shown in Figure 1. Figure 1 As shown; the relative percentage of its chemical components was determined by peak area normalization method. Table 1 Chemical composition information of volatile oil from leaves of Panax ginseng
[0033] The results showed that 84 components were isolated from the volatile oil of leaves at different harvesting times, of which 68 components were identified. The chemical components and relative percentages of the volatile oil of leaves at different harvesting times are shown in Table 1. 29, 48, 34, 21, and 35 components were identified in the volatile oil of leaves at different harvesting times, of which there were 3 components in total, namely α-pinene (1.34%-6.20%), β-farnesene (5.40%-19.12%), and β-bisabolene (37.22%-44.43%). The relative percentage of β-bisabolene in the leaves of Panax ginseng collected at different harvesting times was the highest, all greater than 30%, and it was the main component in the volatile oil of Panax ginseng. The relative percentage of β-farnesene (5.40%-19.12%) was also high, all greater than 5%. The analysis showed that the volatile oil of the leaves of the northeastern spiny ginseng is composed of terpenes (40 species), alkanes (17 species), fatty acids (8 species), aldehydes (2 species) and phenols (1 species). As shown in the figure, the chemical composition of sample B is similar to that of sample D, with the relative percentage of terpenes being higher (88.98% and 68.22%), followed by alkanes (8.98% and 28.18%). The chemical composition of sample C is similar to that of sample E, with the relative percentage of terpenes being higher, 88.76% and 95.81% respectively, followed by fatty acids, 7.31% and 3.40% respectively. Terpenes were present in high levels in all volatile oils. Sample A contained 12 sesquiterpenes (65.72%), 3 diterpenes (6.00%), including phyton (0.85%), phytol (2.84%), geranyl linalool (2.27%), and 4 monoterpenes. Sample B contained 24 sesquiterpenes (78.13%), including citronellal, α-serone, γ-galactone, γ-galactone, and γ-linalool. Cedrene is its unique component, 2 diterpenoid components (4.71%), phyton (1.43%), and phytol (3.28%); C leaf volatile oil contains 20 sesquiterpenoid components (79.00%), cadinene is its unique component, 2 diterpenoid components (3.82%), phyton (0.90%) and phytol (2.92%); D contains 7 sesquiterpenoid components (62.67%). E contains 19 sesquiterpenoid components (81.43%), β-serene and cubebol are its unique components, 2 diterpenoid components (3.72%), phyton (0.85%) and phytol (2.84%). In previous reports on the chemical composition of the roots and rhizomes of Panax ginseng, A-bergamotene, β-serene, isocaryophyllene, γ-guruene, α-serone, and risone have not been reported. The same chemical components as those in the roots and rhizomes were found in the leaves, including α-pinene, β-myrcene, β-pinene, α-cubene, octanal, eucalyptol, thujacene, etc.
[0034] The volatile oil of Panax ginseng has a unique aroma, which is related to the presence of a large number of terpenoids. Among the 40 terpenoid components identified, β-bisabolene has the highest relative content (44.43%), followed by β-farnesene (17.23%). β-bisabolene is a substance with good physiological activity and practical value, with a good fragrance, and is a natural fragrance with anti-itch, anti-inflammatory and anti-tumor effects. In addition, bisabolene can also be used as a chemical precursor for the synthesis of various medicines. In addition, the sesquiterpenoids such as guarene and caryophyllene contained in the volatile oil of Panax ginseng are indispensable raw materials in the pharmaceutical and food industries due to their high aroma and biological activity. Diterpenes and their oxygen-containing derivatives also have good biological activity. Phytol has anti-inflammatory activity and has antibacterial activity against Mycobacterium tuberculosis and Staphylococcus aureus, which is consistent with the reported antibacterial and anti-inflammatory effects of the volatile oil of Panax ginseng. In summary, by analyzing the chemical components of volatile oils in the leaves of non-medicinal parts of Panax ginseng, the differences in the composition of volatile oils in different periods were explored, which provided a reference for the extraction, separation and preparation of chemical components in the volatile oils of Panax ginseng, and also laid a foundation for further development of the comprehensive utilization of Panax ginseng. Screening of compound essential oils
[0035] Based on the previous work, jojoba oil and grape seed oil were determined as the base oils. The formula of the compound essential oil was selected as shown in Table 2. The amount of Panax ginseng essential oil added was screened, and the formula was determined by sensory evaluation, heat and cold resistance experiments, and physical and chemical properties. Table 2 Northeastern spiny ginseng compound essential oil formula Sensory evaluation
[0036] This study used the comprehensive sensory score of compound essential oils as the evaluation index, and organized an evaluation team of 20 people to conduct sensory evaluation of the products from three aspects: color, aroma, and application effect. The comprehensive score is the average score of all valid scores. According to the "General Guidelines for Establishing Sensory Analysis Laboratories for Sensory Analysis (GB / T 13868-2009)" and "General Theory of Sensory Analysis (GB / T 10220-2012)", the evaluation standards were formulated. The total score of the three factors of color, aroma, and application effect is 10 points. The specific standards are shown in Table 3. Table 3 Sensory evaluation standards Cold and heat resistance
[0037] The compound essential oil samples were placed in -5℃ and 40℃ constant temperature boxes respectively, taken out after 24 hours, and observed for crystal precipitation, stratification, and turbidity. Antibacterial activity assay
[0038] The suspension quantitative sterilization method was used to determine the antibacterial activity of the compound essential oil. The bacteria selected were Staphylococcus aureus, Escherichia coli, Candida albicans, and Bacillus aeruginosa, which are common microorganisms that can cause skin inflammation. Each treatment was repeated three times, and the number of surviving colonies after treatment was determined. The concentration of viable bacteria (CFU / ml) was calculated and converted into a logarithmic value (N). The calculation formula for the killing logarithmic value is as follows: Killing log value = No / Nx Where No is the logarithmic value of the average viable bacteria concentration in the control group; Nx is the logarithmic value of the viable bacteria concentration in the sample.
[0039] The evaluation results are shown in Table 4. The essential oils in each formula are relatively stable under low and high temperature environments, without crystal precipitation, stratification, turbidity and other phenomena. The color, smell and application effect of the essential oil will affect the consumer's experience of use. Group D scored the highest in the sensory evaluation. Compared with other groups, the geranium essential oil added to the formula of group D not only has a refreshing fruity aroma, but also has the effects of balancing sebum secretion, promoting blood circulation and sterilization. Therefore, group D with the best sensory experience is determined to be the best formula for the compound essential oil. Table 4 Formulation screening 6.2.2 Antibacterial activity assay
[0040] The results are shown in Tables 5, 6, 7 and 8. After three repeated tests, the killing logarithmic values of the compound essential oil for Escherichia coli, Staphylococcus aureus, Candida albicans and Bacillus aeruginosa were ≥5.00 when the compound essential oil was used for 0.5min, 1min and 1.5min, respectively, and the killing rate was above 99.999%, indicating that the compound essential oil has good antibacterial activity and meets the requirements of hygiene indicators. Table 5 Inhibition of Escherichia coli Note: Negative controls showed no growth Table 6 Inhibitory effect on Staphylococcus aureus Note: Negative controls showed no growth Table 7 Inhibitory effect on Candida albicans Note: Negative controls showed no growth Table 8 Inhibitory effect on Bacillus aeruginosa Note: Negative controls showed no growth The above are only preferred specific implementations of the present application, but the protection scope of the present application is not limited thereto. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed in the present application should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the patent claim.
Claims
1. A compound essential oil of Panax notoginseng with antibacterial activity, characterized in that: The compound essential oil mainly comprises the following ingredients: volatile oil of northeastern spiny ginseng, red pine essential oil, patchouli essential oil, lavender oil, geranium essential oil, jojoba oil and grape seed oil.
2. The compound essential oil of Panax notoginseng with antibacterial activity according to claim 1, characterized in that: The Northeastern spiny ginseng compound essential oil is prepared according to the following method: (1) Leaf samples were collected at the Northeastern ginseng cultivation base in Changbai Korean Autonomous County, Jilin Province, and the samples were collected at different times. The effective components of different samples were analyzed to select the best raw materials; (2) The selected leaf samples of Panax ginseng are prepared into coarse powder by a pulverizer, and an appropriate amount of the coarse powder of Panax ginseng is placed in a round-bottom flask, and an appropriate amount of distilled water and zeolite are added. A volatile oil extraction device is installed according to the requirements of steam distillation extraction in the pharmacopoeia, and the volatile oil is extracted by steam distillation until the amount of volatile oil no longer increases, and the extraction is stopped to obtain a light yellow oily liquid with a special aroma, and an appropriate amount of desiccant is added to obtain Panax ginseng volatile oil; (3) The volatile oil of Panax notoginseng obtained in step (2) is mixed with a base oil, and other additives are added in different volume percentages to obtain a Panax notoginseng compound essential oil with antibacterial activity.
3. The method for preparing a compound essential oil of Panax notoginseng having antibacterial activity according to claim 2, characterized in that: The picking time of the Northeastern spiny ginseng in step (1) is from summer to autumn, and the picking interval is about 1 month.
4. The method for preparing a compound essential oil of Panax notoginseng having antibacterial activity according to claim 2, characterized in that: In step (1), the ginseng sample is required to remove impurities such as branches, bark, weeds, etc. from the leaves, and then the leaves are placed in a ventilated and cool place, and after drying, they are crushed and sealed for later use.
5. The method for preparing the essential oil of Panax notoginseng according to claim 2, characterized in that: The desiccant described in step (2) is anhydrous sodium sulfate.
6. The method for preparing the essential oil of Panax notoginseng according to claim 2, characterized in that: The base oils described in step (3) are jojoba oil and grape seed oil.
7. The method for preparing the essential oil of Panax notoginseng according to claim 2, characterized in that: The total volume of the jojoba oil and grape seed oil in step (3) accounts for 80%, of which the jojoba oil accounts for 50% and the grape seed oil accounts for 30%.
8. The method for preparing Panax notoginseng essential oil according to claim 2, characterized in that: The other additives described in step (3) are red pine essential oil, patchouli essential oil, lavender oil, and geranium essential oil, wherein the red pine essential oil accounts for 12-15%, the patchouli essential oil accounts for 3-6%, the lavender oil accounts for 3%, and the geranium essential oil accounts for 3%.
9. The Panax notoginseng essential oil according to claim 1, characterized in that The compound essential oil has good antibacterial activity.