Preparation method of cinnamon volatile oil clathrate compound

Abstract

The invention relates to a preparation method of a cinnamon volatile oil clathrate compound. The preparation method comprises the following steps: extracting cinnamon volatile oil; the mass ratio of the beta-cyclodextrin to the distilled water is 12: 24; starting a colloid mill, adding the mixed beta-cyclodextrin aqueous solution into the colloid mill, and continuously grinding for 2 minutes; slowly adding 1 part of cinnamon volatile oil into the beta-cyclodextrin aqueous solution, continuously grinding for 60 minutes, collecting clathrate liquid, carrying out vacuum suction filtration on the clathrate liquid after standing, and drying in a hot air drying oven to obtain the first volatile oil clathrate compound. The cortex cinnamomi volatile oil clathrate compound prepared by the preparation method of the cortex cinnamomi volatile oil clathrate compound has the effects of remarkably shortening the production period and improving the encapsulation efficiency and high-temperature stability of the clathrate compound, does not use an organic solvent, and has better thermal stability and long-term storage stability.

Description

Technical Field

[0001] The present invention relates to the technical field of medicine, and particularly to a preparation method of cinnamomum cassia volatile oil inclusion compound. Background Art

[0002] Volatile oils are contained in many traditional Chinese medicinal materials, but these volatile oils are unstable by themselves. If the untreated volatile oils are directly sprayed into the products made by the granulation method, their active ingredients are likely to volatilize and oxidize, resulting in a large loss of volatile oils, directly affecting the efficacy of drugs and reducing the therapeutic effect. In addition, due to differences in storage conditions, the quality of products in different batches may also be uneven, further affecting the effectiveness of clinical applications. To improve the stability of volatile oils and mask their pungent odor, β-cyclodextrin (β-CD) is often used for inclusion to powderize liquid drugs and facilitate the preparation of various dosage forms.

[0003] Cinnamomum cassia volatile oil is usually a volatile substance extracted from cinnamomum cassia pieces, and has various pharmacological effects such as regulating blood circulation, protecting the myocardium, reducing swelling and inflammation, relieving asthma, analgesia, antibacterial, improving glucose metabolism, anti-tumor, antioxidant, and anti-aging. However, cinnamomum cassia volatile oil has strong irritation and poor stability. When directly added to solid preparations such as granules and capsules, the volatile oil is extremely volatile, has strong irritation, and poor compliance, which limits the wide application of cinnamomum cassia. In actual production, cinnamomum cassia oil is often used as medicine in the form of inclusion compound to form a more stable complex, effectively reducing the irritation of cinnamomum cassia oil, reducing its volatilization loss, improving its applicability in different preparations, ensuring the effectiveness of the drug during storage and use, and thus achieving long-term stability.

[0004] The inclusion methods of volatile oils mainly include saturated aqueous solution method, grinding method, ultrasonic method, etc. Among them, the saturated aqueous solution method is favored because of its simple process, convenient operation, and ability to achieve a high drug loading and encapsulation rate of volatile oils, and is more commonly used in actual production. The saturated aqueous solution method can improve the interaction between volatile oils and inclusion agents (such as β-cyclodextrin), thereby forming inclusion compounds to improve the quality and stability of volatile oils and broaden their application in traditional Chinese medicine preparations. However, the production cycle of preparing inclusion compounds by the saturated aqueous solution method is long and the efficiency is low.

[0005] Spray drying has become a commonly used drying method in the production process of traditional Chinese medicine preparations due to its high efficiency, rapid drying, and good product uniformity, ensuring the stability and effectiveness of traditional Chinese medicine components. During the spray drying process, by quickly removing the moisture in the liquid, the volatile oil is rapidly converted into solid powder, thereby reducing the oxidation and degradation of volatile components. When the aqueous solution of β-cyclodextrin inclusion complex is spray-dried, β-cyclodextrin forms spherical microcapsules, which can not only significantly improve the stability of the volatile oil inclusion complex but also effectively prevent it from being affected by the external environment during storage and use, thereby improving the product quality.

[0006] Currently, in the production process of common products containing cinnamon volatile oil, the β-cyclodextrin saturated aqueous solution inclusion method is used to include the volatile oil. After inclusion, it needs to be left standing at low temperature to completely precipitate the crystals, then filtered by suction, and finally dried. On the one hand, these processes have a long production cycle. It takes at least 2 to 3 days in production to carry out subsequent mixing with concentrated liquid dry extract powder and granulation, with a long production cycle. On the other hand, there are significant losses under heating and long-term storage, affecting the quality stability of the pharmaceutical preparation. Summary of the Invention

[0007] In view of the above deficiencies in the prior art, the present invention provides a method for preparing a cinnamon volatile oil inclusion complex with a high inclusion rate, and the obtained cinnamon volatile oil inclusion complex has better thermal stability and long-term storage stability.

[0008] The technical solution adopted by the present invention is as follows: A method for preparing a cinnamon volatile oil inclusion complex, comprising the following steps: S11. The extraction method of cinnamon volatile oil is as follows: Take cinnamon cut pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S12. Stir and mix the β-cyclodextrin and distilled water in a ratio of 12 parts: 24 parts evenly; S13. Start the colloid mill, immediately add the mixed β-cyclodextrin aqueous solution in step S12 into the colloid mill, and continue to grind for 2 min; S14. Slowly add 1 part of cinnamon volatile oil to the β-cyclodextrin aqueous solution in step S13, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed; S15. Vacuum filter the inclusion liquid standing well in step S14, and place it in a hot air drying oven to dry, thereby obtaining the first cinnamon volatile oil inclusion complex.

[0009] A method for preparing a cinnamon volatile oil inclusion complex, comprising the following steps: S21. The extraction method of cinnamon volatile oil is as follows: Take cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S22. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water evenly by stirring, and set aside; S23. Start the colloid mill, immediately add the mixed β-cyclodextrin aqueous solution in step S22 into the colloid mill, and continue to grind for 2 min; S24. Slowly add 1 part of cinnamon volatile oil to the β-cyclodextrin aqueous solution in step S23, continue to grind for 60 min, collect the inclusion liquid, and let it stand still in the dark and sealed; S25. Spray-dry the inclusion liquid standing still in step S24 to obtain the second cinnamon volatile oil inclusion compound.

[0010] A preparation method of cinnamon volatile oil inclusion compound includes the following steps: S31. The extraction method of cinnamon volatile oil is as follows: Take cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S32. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water evenly by stirring; S33. Take 1 part of cinnamon volatile oil, add one of palmitic acid ascorbate, propyl gallate, octyl gallate, eugenol, thymol, 2,6-di-tert-butyl-p-cresol, hold and rotate for 60 seconds, and ultrasonicate for 30 seconds to mix evenly; S34. Start the colloid mill, immediately add the mixed β-cyclodextrin aqueous solution in step S32 into the colloid mill, and continue to grind for 2 min; S35. Slowly add the well-mixed substance in step S33 to the β-cyclodextrin aqueous solution in step S34, continue to grind for 60 min, collect the inclusion liquid, and let it stand still in the dark and sealed; S36. Spray-dry the inclusion liquid standing still in step S35 to obtain the third cinnamon volatile oil inclusion compound.

[0011] Preferably, in step S33, the amount of one of palmitic acid ascorbate, propyl gallate, octyl gallate, eugenol, thymol, 2,6-di-tert-butyl-p-cresol added is 0.0004 parts.

[0012] Preferably, in step S33, the amount of one of octyl gallate and propyl gallate added is 0.0008 parts.

[0013] The beneficial effects of the present invention compared with the prior art: The cinnamomum volatile oil inclusion compound prepared by the preparation method of the present invention has the effects of significantly shortening the production cycle, improving the encapsulation efficiency of the inclusion compound and the high-temperature stability, and avoiding the use of organic solvents, and has better thermal stability and long-term storage stability. Brief Description of the Drawings

[0014] Figure 1 Take a small amount of β-cyclodextrin powder and fix it on the conductive adhesive. Blow off the excess powder with an ear bulb, place it in an ion sputtering device to gold-plate the powder surface, and observe the appearance characteristics of each sample powder under a scanning electron microscope; Figure 2 Take a small amount of the inclusion compound powder in Example 1 and fix it on the conductive adhesive. Blow off the excess powder with an ear bulb, place it in an ion sputtering device to gold-plate the powder surface, and observe the appearance characteristics of each sample powder under a scanning electron microscope; Figure 3 Take a small amount of the inclusion compound powder in Example 2 and fix it on the conductive adhesive. Blow off the excess powder with an ear bulb, place it in an ion sputtering device to gold-plate the powder surface, and observe the appearance characteristics of each sample powder. Detailed Description of the Invention

[0015] The present invention will be described in detail below with reference to the accompanying drawings and embodiments: The preparation method of the cinnamomum volatile oil inclusion compound of the present invention is to uniformly mix the volatile oil with octyl gallate or propyl gallate with an appropriate concentration, and then jointly prepare a cinnamomum volatile oil inclusion compound with strong stability by using a colloid mill inclusion and spray drying method, including the following steps: weigh according to the mass ratio of oil: β-cyclodextrin: distilled water = 1:12:24. After mixing and stirring β-cyclodextrin and distilled water evenly, pour them into a colloid mill. First, grind for 2 minutes, and then slowly drop octyl gallate or propyl gallate with a mass fraction of 0.08% into the liquid vortex in the middle of the colloid mill to obtain a uniformly mixed cinnamomum volatile oil. Start timing and grind for 1 hour to complete the inclusion. Take out the inclusion liquid and place it in a closed container, and let it stand at normal temperature in the dark and sealed. Then carry out spray drying (spray drying feed rate 15Hz, atomization 35Hz, inlet air temperature 165-170°C, exhaust air speed 72-75Hz, outlet air temperature 99-103°C) to obtain the product.

[0016] The preparation steps of a preparation method of a cinnamomum volatile oil inclusion compound are as follows: 1. The extraction method of cinnamomum volatile oil is as follows: Take cinnamomum officinale cuttings, crush them through a 5-mesh sieve, moisten them with water, spread them evenly in a multi-functional extraction tank, the power of the extraction tank is 6KW, extract for 6 hours, collect the cinnamomum volatile oil, and dehydrate the obtained cinnamomum volatile oil with anhydrous sodium sulfate to obtain the product.

[0017] 2. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water evenly by stirring, and set aside.

[0018] β - cyclodextrin is a commonly used auxiliary material for encapsulating (solidifying) volatile oils. The ratio is obtained based on the results of preliminary pre - experiments. The ratio of cyclodextrin to distilled water has no significant effect on the encapsulation rate of volatile oils (as shown in the following table). Therefore, a ratio suitable for production is selected. (The liquid volume needs to be larger to adapt to the specifications of existing instruments); The purpose of adding distilled water: β - cyclodextrin encapsulates volatile oils by adsorbing through its own molecular pores. Adding distilled water makes it more swollen, with larger pores, increasing the probability of capturing oil molecules.

[0019] Table 1 is a comparison table of the effect of the ratio of cyclodextrin to distilled water on the encapsulation rate of cinnamon volatile oil.

[0020]

[0021] 3. Take 1 part of cinnamon volatile oil, add 0.0008 part of octyl gallate or propyl gallate, vortex for 60 seconds, sonicate for 30 seconds, and mix evenly for standby.

[0022] 4. Start the colloid mill, and immediately add the well - mixed β - cyclodextrin aqueous solution in step 2 into the colloid mill, and continue to grind for 2 min.

[0023] 5. Slowly add the well - mixed substance in step 3 into the β - cyclodextrin aqueous solution in step 4, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed.

[0024] 6. Spray - dry the inclusion liquid that has been allowed to stand in step 5 to obtain the cinnamon volatile oil inclusion compound. The spray - drying parameters are: feed rate 225 mL / h, inlet air temperature 170 °C, outlet temperature 100 °C, air flow rate 40 m 3 / h.

[0025] In the following examples, the content of cinnamaldehyde in cinnamon volatile oil is determined by the method in the determination item of cinnamon oil in the Chinese Pharmacopoeia (2025 Edition).

[0026] 1) Chromatographic conditions and system suitability test: A capillary column with cross - linked 5% phenyl methyl polysiloxane as the stationary phase (column length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm). The column temperature is programmed: the initial temperature is 100 °C, rising at a rate of 5 °C per minute to 150 °C, holding for 5 minutes, then rising at a rate of 5 °C per minute to 200 °C and holding for 5 minutes; the inlet temperature is 200 °C; the detector temperature is 220 °C; split injection, split ratio 20:1. The number of theoretical plates calculated based on the cinnamaldehyde peak should be not less than 20000.

[0027] 2) Preparation of the reference substance solution: Take an appropriate amount of cinnamaldehyde reference substance, accurately weigh it, and make a solution containing 3 mg per 1 ml with ethyl acetate, that is, obtain it.

[0028] 3) Preparation of the test solution: Accurately weigh 100 mg of this product, place it in a 25-ml volumetric flask, add ethyl acetate to the scale, shake well to obtain the solution.

[0029] 4) Assay method: Accurately pipette 1 μl each of the reference solution and the test solution, inject them into the gas chromatograph for determination to obtain the result.

[0030] In the following examples, the content of cinnamaldehyde in the inclusion compound was determined by ultra-high performance liquid chromatography.

[0031] 1) Chromatographic conditions and system suitability test: Use octadecylsilane-bonded silica gel as the filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.6 µm), use acetonitrile as mobile phase A, use 0.1% phosphoric acid solution as mobile phase B, and perform gradient elution according to the regulations in the following table; the flow rate is 0.4 mL per minute; the column temperature is 30 °C; the detection wavelength is 290 nm; the number of theoretical plates calculated based on the cinnamaldehyde peak should be not less than 3000.

[0032] Table 2 is the table of chromatographic conditions and system suitability test.

[0033] ; 2) Preparation of the reference solution: Take an appropriate amount of cinnamaldehyde reference substance, accurately weigh it, and dissolve it in methanol to make a solution containing 10 µg per 1 mL to obtain the solution.

[0034] 3) Preparation of the test solution: Take 0.10 g of the inclusion compound, accurately weigh it, place it in a stoppered conical flask, accurately add 200 mL of 50% methanol, stopper it, weigh it, ultrasonically treat it for 30 minutes, let it cool, weigh it again, make up the lost weight with 50% methanol, shake well, filter, and take the filtrate to obtain the solution.

[0035] 4) Assay method: Accurately pipette 1 μL each of the reference solution and the test solution, inject them into the ultra-high performance liquid chromatograph for determination to obtain the result.

[0036] Calculate the yield of the inclusion compound and the encapsulation efficiency of the volatile oil according to the following formula.

[0037] ;

[0038] Example 1, a preparation method of a cinnamon volatile oil inclusion compound, includes the following steps: S11. The extraction method of cinnamon volatile oil is as follows: Take the cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, spread them evenly in a multi-functional extraction tank, select an extraction power of 6 KW, extract for 6 h, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S12. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water evenly and stir for later use; S13. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S12 into the colloid mill, and continue grinding for 2 min; S14. Slowly add 1 part of cinnamon volatile oil into the β-cyclodextrin aqueous solution in step S13, continue grinding for 60 min, collect the inclusion liquid, and let it stand still in the dark and sealed; S15. Vacuum filter the inclusion liquid that has stood still in step S14, and place it in a hot air drying oven to dry, then the first cinnamon volatile oil inclusion complex is obtained.

[0039] Example 2. A preparation method of a cinnamon volatile oil inclusion complex includes the following steps: S21. The extraction method of cinnamon volatile oil is as follows: Take cinnamon cut pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, select an extraction power of 6 KW, extract for 6 h, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S22. Stir and mix 12 parts of β-cyclodextrin and 24 parts of distilled water evenly, and set aside; S23. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S22 into the colloid mill, and continue grinding for 2 min; S24. Slowly add 1 part of cinnamon volatile oil into the β-cyclodextrin aqueous solution in step S23, continue grinding for 60 min, collect the inclusion liquid, and let it stand still in the dark and sealed; S25. Spray-dry the inclusion liquid that has stood still in step S24, then the second cinnamon volatile oil inclusion complex is obtained.

[0040] The spray-drying parameters are: feed rate 225 mL / h, inlet air temperature 170 °C, outlet temperature 100 °C, air flow rate 40 m 3 / h.

[0041] Example 3. A preparation method of a cinnamon volatile oil inclusion complex includes the following steps: S31. The extraction method of cinnamon volatile oil is as follows: Take cinnamon cut pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, select an extraction power of 6 KW, extract for 6 h, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S32. Stir and mix 12 parts of β-cyclodextrin and 24 parts of distilled water evenly; S33. Take 1 part of cinnamon volatile oil, add 0.0004 part of palmitic acid ascorbate, vortex for 60 seconds, ultrasonic for 30 seconds, and mix evenly; S34. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S32 into the colloid mill, and continue grinding for 2 min; S35. Slowly add the well-mixed substance in step S33 into the β-cyclodextrin aqueous solution in step S34, continue to grind for 60 min, collect the inclusion liquid, and let it stand still in the dark with sealed packaging. S36. Spray-dry the inclusion liquid that has been allowed to stand still in step S35 to obtain the third cinnamon volatile oil inclusion complex 3-1.

[0042] The parameters for spray drying are as follows: feeding rate 225 mL / h, inlet air temperature 170 °C, outlet temperature 100 °C, and air flow rate 40 m 3 / h.

[0043] Replace the ascorbyl palmitate in step S33 with 0.0004 parts of propyl gallate, repeat the above steps to obtain the third cinnamon volatile oil inclusion complex 3-2.

[0044] Replace the ascorbyl palmitate in step S33 with 0.0004 parts of octyl gallate, repeat the above steps to obtain the third cinnamon volatile oil inclusion complex 3-3.

[0045] Replace the ascorbyl palmitate in step S33 with 0.0004 parts of eugenol, repeat the above steps to obtain the third cinnamon volatile oil inclusion complex 3-4.

[0046] Replace the ascorbyl palmitate in step S33 with 0.0004 parts of thymol, repeat the above steps to obtain the third cinnamon volatile oil inclusion complex 3-5.

[0047] Replace the ascorbyl palmitate in step S33 with 0.0004 parts of 2,6-di-tert-butyl-p-cresol, repeat the above steps to obtain the third cinnamon volatile oil inclusion complex 3-6.

[0048] Determine the encapsulation efficiency of all the prepared cinnamon volatile oil inclusion complexes in Examples 1, 2, and 3, and the encapsulation efficiency of all the inclusion complexes after 15 days of experiment in a constant temperature and humidity stability chamber (the inclusion complexes are exposed to a temperature of 60 °C and a humidity of 40%) to screen for excellent spray-drying protectants. The results are shown in the following table: Table 3 shows the encapsulation efficiency of the inclusion complexes before and after the 15-day high-temperature stability experiment.

[0049] ; In Example 1 and Example 2, no spray-drying protectant was added to the cinnamon volatile oil. Example 1 used a hot air drying process, while Example 2 used a spray drying process. As can be seen from the results in Table 3, although the initial encapsulation efficiency in Example 2 was lower than that in Example 1, its high temperature stability was better. Therefore, the spray drying process in Example 2 was selected for the preparation of the inclusion compound. Both Example 2 and Example 3 used the spray drying process, but different types of spray-drying protectants were added to the cinnamon volatile oil in Example 3. The results showed that the inclusion compounds with added spray-drying protectants all had good effects, but their high temperature stability effects varied. Therefore, propyl gallate and octyl gallate, which had better high temperature stability, were selected as the types of spray-drying protectants.

[0050] From the scanning electron microscope images attached Figure 1 and attached Figure 2 It can be seen that the morphology of the first cinnamon volatile oil inclusion compound prepared in Example 1 and the β-cyclodextrin auxiliary material was not very different, but the structure was relatively loose, and there were large pores and cracks in the powder particles. Therefore, the encapsulation efficiency of its high temperature stability was poor, which corresponded to Table 3. The morphology of the second cinnamon volatile oil inclusion compound prepared in Example 2 and the β-cyclodextrin auxiliary material was significantly different. It can be seen that a large number of spherical microcapsule inclusion compounds would be formed after spray drying. This was the reason why the encapsulation efficiency was still better after the high temperature stability experiment in Example 2.

[0051] Example 4, a method for preparing a cinnamon volatile oil inclusion compound, includes the following steps: S41. The extraction method of the cinnamon volatile oil is as follows: Take the cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, spread them evenly in a multi-functional extraction tank, select an extraction power of 6 KW, extract for 6 h, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S42. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water evenly by stirring; S43. Take 1 part of the cinnamon volatile oil, add 0.0008 parts of octyl gallate, vortex for 60 seconds, and ultrasonicate for 30 seconds to mix evenly; S44. Start the colloid mill, and immediately add the well-mixed β-cyclodextrin aqueous solution in step S42 into the colloid mill and continue to grind for 2 min; S45. Slowly add the well-mixed substance in step S43 into the β-cyclodextrin aqueous solution in step S44, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed; S46. Spray dry the inclusion liquid that has stood well in step S45 to obtain the fourth cinnamon volatile oil inclusion compound 4-1.

[0052] The spray drying parameters are: the feeding speed is 225 mL / h, the inlet air temperature is 170 °C, the outlet temperature is 100 °C, and the air flow rate is 40 m 3 / h.

[0053] Replace the octyl gallate in step S43 with 0.0008 parts of propyl gallate, repeat the above steps, and obtain the fourth cinnamon volatile oil inclusion complex 4-2.

[0054] The differences between Examples 1 to 4 are as follows: In Example 1, drying is carried out without a spray-drying protective agent; in Example 2, spray drying is carried out without a spray-drying protective agent; in Example 3, 0.0004 parts of a spray-drying protective agent is added for spray drying; in Example 4, 0.0008 parts of a spray-drying protective agent is added for spray drying.

[0055] Measure the encapsulation efficiency of all the prepared cinnamon volatile oil inclusion complexes in Examples 1, 2, 3, and 4, and the encapsulation efficiency of the inclusion complexes after 15 days of experiment in a constant temperature and humidity stability chamber (the inclusion complexes are exposed to a temperature of 60 °C and a humidity of 40%). The results are shown in the following table: Table 4 is the table of the encapsulation efficiency of the inclusion complexes before and after the 15-day high-temperature stability experiment.

[0056] ; Example 1 is a cinnamon volatile oil inclusion complex prepared by a hot air drying process, Example 2 is an inclusion complex prepared by a spray drying process, Example 3 is a cinnamon volatile oil inclusion complex prepared by a spray drying process with a spray-drying protective agent containing 0.04% (mass ratio to the volatile oil) of octyl gallate and propyl gallate added respectively, and Example 4 is a cinnamon volatile oil inclusion complex prepared by a spray drying process with a spray-drying protective agent containing 0.08% (mass ratio to the volatile oil) of octyl gallate and propyl gallate added respectively. From the results in Table 4, it can be seen that compared with the most widely used hot air drying process at present, the encapsulation efficiency of the fourth cinnamon volatile oil inclusion complex 4-1 prepared by the process in Example 4 in the high-temperature stability experiment has increased from 53.60% to 65.95%, an increase of 12.35%. Compared with the process without a spray-drying protective agent (Example 2), the initial encapsulation efficiency has increased from 75.68% to 90.38%, an increase of 14.70%. Compared with adding a 0.04% spray-drying protective agent (such as the third cinnamon volatile oil inclusion complex 3-3 prepared in Example 3, with octyl gallate added), the initial encapsulation efficiency of the fourth cinnamon volatile oil inclusion complex 4-1 prepared in Example 4 has increased from 78.64% to 90.38%. The cinnamon volatile oil inclusion complex prepared by the present process and method has the effects of significantly shortening the production cycle, improving the encapsulation efficiency and high-temperature stability of the inclusion complex, and avoiding the use of organic solvents.

[0057] The above is only a preferred embodiment of the present invention, and does not impose any form of limitation on the structure of the present invention. Any simple modification, equivalent change, and modification made to the above embodiments based on the technical essence of the present invention all fall within the scope of the technical solution of the present invention.

Claims

1. A preparation method of cinnamon volatile oil inclusion compound, characterized in that, It includes the following steps: S11. The extraction method of cinnamon volatile oil is as follows: Take cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S12. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water by mass and stir evenly; S13. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S12 into the colloid mill, and continue to grind for 2 min; S14. Slowly add 1 part of cinnamon volatile oil into the β-cyclodextrin aqueous solution in step S13, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed; S15. Vacuum filter the well-stood inclusion liquid in step S14, and place it in a hot air drying oven to dry, then the first cinnamon volatile oil inclusion complex is obtained.

2. A preparation method of cinnamomum essential oil inclusion compound, characterized in that, It includes the following steps: S21. The extraction method of cinnamon volatile oil is as follows: Take cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S22. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water by mass and stir evenly for standby; S23. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S22 into the colloid mill, and continue to grind for 2 min; S24. Slowly add 1 part of cinnamon volatile oil into the β-cyclodextrin aqueous solution in step S23, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed; S25. Spray-dry the well-stood inclusion liquid in step S24, then the second cinnamon volatile oil inclusion complex is obtained.

3. A preparation method of cinnamomum volatile oil inclusion compound, characterized in that, It includes the following steps: S31. The extraction method of cinnamon volatile oil is as follows: Take cinnamon decoction pieces, crush them through a 5-mesh sieve, moisten them with water, evenly spread them in a multi-functional extraction tank, collect the cinnamon volatile oil, and dehydrate the obtained cinnamon volatile oil with anhydrous sodium sulfate to obtain it; S32. Mix 12 parts of β-cyclodextrin with 24 parts of distilled water by mass and stir evenly; S33. Take 1 part of cinnamon volatile oil, add one of palmitic acid ascorbate, propyl gallate, octyl gallate, eugenol, thymol, 2,6-di-tert-butyl-p-cresol, hold and rotate for 60 seconds, ultrasonicate for 30 seconds, and mix evenly; S34. Start the colloid mill, immediately add the well-mixed β-cyclodextrin aqueous solution in step S32 into the colloid mill, and continue to grind for 2 min; S35. Slowly add the well-mixed substance in step S33 into the β-cyclodextrin aqueous solution in step S34, continue to grind for 60 min, collect the inclusion liquid, and let it stand in the dark and sealed; S36. Spray-dry the well-stood inclusion liquid in step S35, then the third cinnamon volatile oil inclusion complex is obtained.

4. The preparation method of a cinnamon volatile oil inclusion complex according to claim 3, characterized in that: In step S33, the amount of one of palmitic acid ascorbate, propyl gallate, octyl gallate, eugenol, thymol, 2,6-di-tert-butyl-p-cresol added is 0.0004 part.

5. The preparation method of a cinnamon volatile oil inclusion complex according to claim 3, characterized in that: In step S33, the amount of one of octyl gallate and propyl gallate added is 0.0008 parts.

Images