Preparation of HP-beta-CD-based nano-silver antibacterial material and application of HP-beta-CD-based nano-silver antibacterial material in tobacco flavor

Abstract

The invention discloses preparation of an HP-beta-CD-based nano-silver antibacterial material and application of the HP-beta-CD-based nano-silver antibacterial material in tobacco flavor. A preparation method comprises the following steps: preparing a silver nitrate solution; adding PDDA into the silver nitrate solution, and stirring; a hydrazine hydrate solution is slowly dropped into a silver ion solution dissolved with PDDA, stirring is carried out while adding is carried out, a nano-silver suspension is obtained through a reaction at the room temperature, an AgNPS solution is obtained after cleaning, the AgNPS solution is centrifuged and then dried, and nano-silver particles are obtained; adding the hydroxypropyl-beta-cyclodextrin into the deionized water, and dissolving the hydroxypropyl-beta-cyclodextrin; nano-silver particles are slowly added into the hydroxypropyl-beta-cyclodextrin solution, an HP-beta-CD nano-silver solution is obtained, and continuous stirring is conducted in the adding process; and the HP-beta-CD nano-silver solution is subjected to freeze drying treatment, and the antibacterial material based on the HP-beta-CD nano-silver is obtained. The flavors and fragrances treated by the antibacterial material have good performance in sensory evaluation, and have almost no obvious difference compared with untreated samples, and the antibacterial material meets the strict requirements of the tobacco industry on the product quality.

Description

Technical Field

[0001] The invention relates to the technical field of tobacco, and in particular to the preparation of an HP-β-CD nano-silver antibacterial material and its application in tobacco flavorings. Background Art

[0002] Tobacco flavors and fragrances can directly change the quality style of cigarette products and are one of the decisive factors affecting the stability of cigarette product quality. During the production and processing of flavors and fragrances, they will inevitably come into contact with microorganisms (such as yeast, mold, etc.). If they are stored in a high temperature environment for a long time, because flavors and fragrances contain a large amount of carbon and nitrogen sources, they become natural culture media for microorganisms such as yeast. The large-scale reproduction of microorganisms will cause the quality of flavors and fragrances to fluctuate, which can easily affect the quality of cigarette products. Therefore, how to reduce the quality changes of flavors and fragrances caused by microbial fermentation and deterioration is one of the hot topics in industry research.

[0003] Antibacterial film is a functional film with antibacterial and fresh-keeping effects made by adding antibacterial agents to edible or biodegradable film matrices, which can effectively extend the shelf life of food. Nanosilver, as a highly effective bactericidal material, has been widely studied and applied in the field of sterilization because of its safety, high efficiency, practicality, and recyclability. The HP-β-CD nanosilver antibacterial material prepared by the present invention can effectively kill microorganisms such as yeast and mold without affecting the effects of flavors and fragrances, and extend the shelf life of flavors and fragrances, and has good application potential. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a preparation method of an antibacterial material based on HP-β-CD nanosilver and its application in tobacco flavors, so as to solve the problem that tobacco flavors and fragrances are easily contaminated by microorganisms during the production and processing. The antibacterial material of the present application can effectively kill microorganisms such as yeast and mold while maintaining its quality and sensory characteristics, thus meeting the tobacco industry's demand for the stability of the quality of flavors and fragrances.

[0005] The technical problem to be solved by the present invention is achieved through the following technical solutions:

[0006] A method for preparing an antibacterial material based on HP-β-CD nanosilver comprises the following steps:

[0007] (1) dissolving silver nitrate in deionized water to prepare a silver nitrate solution;

[0008] (2) adding polydiallyldimethylammonium chloride (PDDA) dropwise to the silver nitrate solution of step (1) under stirring, and continuing stirring for 30 minutes;

[0009] (3) slowly dripping the hydrazine hydrate solution into the silver ion solution containing PDDA in step (2), stirring while dripping, reacting at room temperature for 4 hours, to obtain a nanosilver suspension, washing with deionized water to obtain an AgNPS solution, centrifuging the AgNPS solution to remove the supernatant, and vacuum drying to obtain nanosilver particles;

[0010] (4) Weigh hydroxypropyl-β-cyclodextrin and add it to deionized water to dissolve it for later use;

[0011] (5) slowly adding the nanosilver particles into the hydroxypropyl-β-cyclodextrin solution to obtain a HP-β-CD nanosilver solution, with continuous stirring during the addition process;

[0012] (6) The HP-β-CD nanosilver solution is freeze-dried to obtain an antibacterial material based on HP-β-CD nanosilver.

[0013] Preferably, in the above technical solution, in step (1), the mass ratio of the silver nitrate to the deionized water is 1:1 to 1:3, and the amount of the PDDA added in step (2) does not exceed 2% of the mass of the silver nitrate solution.

[0014] Preferably, in the above technical solution, the concentration of the hydrazine hydrate solution in step (3) is 10%, and the volume ratio of the hydrazine hydrate solution to the silver nitrate solution is 1:(2-4); the centrifugation conditions are: 15000rpm, 30min; and the drying conditions are: drying in a vacuum drying oven at 45°C for 2h.

[0015] Preferably, in the above technical solution, in step (4), the mass ratio of the hydroxypropyl-β-cyclodextrin to the deionized water is 1:9.

[0016] Preferably, in the above technical solution, in step (5), the mass ratio of the nanosilver particles to the hydroxypropyl-β-cyclodextrin solution is 1:1; and the speed of continuous stirring is 200 rpm.

[0017] Preferably, in the above technical solution, in step (6), the freeze-drying conditions are: freeze-drying at -50°C for 24 hours.

[0018] A sterilization device for tobacco flavors and fragrances comprises an outer shell which is a hollow three-dimensional cylindrical structure, a filter screen is arranged in the inner ring of the outer shell, HP-β-CD nano silver antibacterial material is filled between the anti-shell and the filter screen, and a filtering device is arranged at the bottom end of the filter screen.

[0019] The invention discloses an application of HP-β-CD nano-silver antibacterial material in sterilization in tobacco flavors.

[0020] Preferably, in the above technical solution, the application is to sterilize tobacco flavors using HP-β-CD nanosilver antibacterial materials, comprising the following steps:

[0021] (1) The flavors and fragrances flow into the sterilization device from the top, and flow out from the bottom of the device after being sterilized by the HP-β-CD nano-silver antibacterial material inside;

[0022] (2) Repeat the above step (1) three times, with the sterilization time not less than 10 min;

[0023] (3) After sterilization, rinse the sterilization equipment with pure water, dry at 45℃ and seal for storage.

[0024] The above technical solution of the present invention has the following beneficial effects:

[0025] The antibacterial material based on HP-β-CD nanosilver of the present application can be effectively used in the sterilization treatment of tobacco flavors and fragrances, significantly improving the quality stability and shelf life of the products. By combining nanosilver particles with hydroxypropyl-β-cyclodextrin, the prepared antibacterial material has the characteristics of high efficiency, safety and environmental protection. The flavors and fragrances treated with the antibacterial material performed well in the sensory evaluation, and there was almost no significant difference compared with the untreated samples. The antibacterial material meets the strict requirements of the tobacco industry for product quality. In addition, the sterilization device is cleverly designed, simple in structure, easy to operate, and reusable, which greatly reduces the production cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

[0027] Figure 1 Schematic diagram of the HP-β-CD nanosilver flavor and fragrance sterilization device.

[0028] Figure 2 This is the microbial status of samples A and B on the 7th day. DETAILED DESCRIPTION

[0029] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention unless otherwise specifically stated.

[0030] Unless otherwise specified, the reagents used in this application are all commercially available or obtained through commercial channels, or can be prepared by referring to existing chemical methods.

[0031] Example 1 Preparation of Sterilization Device

[0032] A sterilization device for tobacco flavors and fragrances comprises a shell 201 which is a hollow three-dimensional cylindrical structure. A filter screen 202 is arranged inside the shell 201. HP-β-CD nano silver antibacterial material 203 is filled between the shell 201 and the filter screen 202. A filtering device 204 is arranged at the bottom of the filter screen 202.

[0033] The following embodiments of the present application will use this device, but are certainly not limited to this device, as long as similar functions are met, such as a reactor, etc.

[0034] Example 2 Preparation of HP-β-CD Nanosilver Antibacterial Material

[0035] (1) Weigh 50 g of silver nitrate and dissolve it in 50 g of deionized water to prepare a silver nitrate solution;

[0036] (2) adding polydiallyldimethylammonium chloride (PDDA) dropwise to the silver nitrate solution under stirring, the amount added not exceeding 2% of the mass of the silver nitrate solution, and stirring continuously for 30 minutes for later use;

[0037] (3) Weigh 5 g of hydrazine hydrate, dissolve it in 45 mL of deionized water, and slowly drip it into the silver ion solution containing PDDA, stirring while adding, react at room temperature for 4 h to obtain a nanosilver suspension, and wash it with deionized water three times to obtain an AgNPS solution;

[0038] The AgNPS solution was centrifuged using a high-speed centrifuge (rotation speed of 15000 rpm, time of 30 min), the supernatant was removed and then dried in a vacuum drying oven at 45° C. for 2 h to obtain silver nanoparticles.

[0039] (4) Weigh 10 g of hydroxypropyl-β-cyclodextrin and add it to 90 g of deionized water to dissolve it and set aside for use;

[0040] (5) slowly adding the nanosilver particles of step (3) into the hydroxypropyl-β-cyclodextrin solution to obtain an HP-β-CD nanosilver solution, wherein the mass ratio of the nanosilver particles to the hydroxypropyl-β-cyclodextrin solution is 1:1, and stirring is continued during the addition process at a rotation speed of 200 rpm;

[0041] (6) The HP-β-CD nanosilver solution was freeze-dried at -50°C for 24 h (FD-1C-50, Shanghai Bilang Instrument Manufacturing Co., Ltd.) to obtain the HP-β-CD nanosilver antibacterial material.

[0042] Example 3 Sterilization treatment

[0043] A certain amount of HP-β-CD nanosilver antibacterial material is weighed and loaded into a homemade filter box to prepare a flavor and fragrance sterilization device (the device can be the sterilization device of Example 1, of course, the present application is not limited thereto, and any sterilization device with the same or similar function can be used).

[0044] The tobacco flavor and fragrance flows into the front of the sterilization device and fills the entire cavity, and then flows out from the back of the device after being sterilized by the internal HP-β-CD nano-silver antibacterial material; the above operation is repeated three times, and the sterilization time each time is not less than 10 minutes; after the sterilization is completed, the sterilization equipment is rinsed with pure water, dried at 45°C, and sealed for storage.

[0045] Application Example 1

[0046] 1. Preparation of apricot extract:

[0047] Weigh 200 g of fresh pitted apricot flesh, cut it into pieces, mix it in a mass ratio of apricot flesh: water = 1:10, perform ultrasonic extraction, and obtain apricot extract after filtration, which is recorded as sample A.

[0048] 100 g of the prepared apricot extract was weighed and treated with a homemade flavor and fragrance sterilization device for 30 min, which was recorded as sample B.

[0049] 2. Determination of total colony count:

[0050] Weigh 100 g of the prepared apricot extract and treat it with a homemade flavor and fragrance sterilization device for 30 min, which is recorded as sample B. Store sample B at room temperature of 25°C in a sealed container, and take a sample on the 7th day to determine the total number of colonies according to GB 4789.2-2016 "Determination of the total number of colonies in food microbiology examination".

[0051] 3. Sample evaluation:

[0052] Sample A was injected into blank cigarettes at a ratio of 0.05% and kept at a constant temperature for 48 hours. Sensory evaluation was performed compared with the blank control sample. The evaluation results are shown in Table 1.

[0053] Table 1 Sensory evaluation results

[0054]

[0055] Evaluation results: After sterilization, the sensory effect of apricot extract in cigarettes remained almost unchanged, indicating that sterilization had little effect on the flavor components and met the requirements of consistency evaluation.

[0056] Although the present invention has been disclosed as above by the embodiments, it is not intended to limit the present invention. Any person skilled in the art may make various choices and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention is limited by the claims and their equivalents.

Claims

1. A method for preparing an antibacterial material based on HP-β-CD nanosilver, characterized in that: The following steps are involved: (1) dissolving silver nitrate in deionized water to prepare a silver nitrate solution; (2) adding polydiallyldimethylammonium chloride (PDDA) dropwise to the silver nitrate solution of step (1) under stirring, and continuing stirring for 30 minutes; (3) slowly dripping the hydrazine hydrate solution into the silver ion solution containing PDDA in step (2), stirring while dripping, reacting at room temperature for 4 hours, to obtain a nanosilver suspension, washing with deionized water to obtain an AgNPS solution, centrifuging the AgNPS solution to remove the supernatant, and vacuum drying to obtain nanosilver particles; (4) Weigh hydroxypropyl-β-cyclodextrin and add it to deionized water to dissolve it for later use; (5) slowly adding the nanosilver particles into the hydroxypropyl-β-cyclodextrin solution to obtain a HP-β-CD nanosilver solution, with continuous stirring during the addition process; (6) The HP-β-CD nanosilver solution is freeze-dried to obtain an antibacterial material based on HP-β-CD nanosilver.

2. The method for preparing the HP-β-CD nanosilver antibacterial material according to claim 1, characterized in that: In step (1), the mass ratio of the silver nitrate to the deionized water is 1:1 to 1:3, and the amount of the PDDA added in step (2) does not exceed 2% of the mass of the silver nitrate solution.

3. The method for preparing the HP-β-CD nanosilver antibacterial material according to claim 1, characterized in that: The concentration of the hydrazine hydrate solution in step (3) is 10%, and the volume ratio of the hydrazine hydrate solution to the silver nitrate solution is 1:(2-4); the centrifugal conditions are: 15000rpm, 30min; and the drying conditions are: drying in a vacuum drying oven at 45°C for 2h.

4. The method for preparing the HP-β-CD nanosilver antibacterial material according to claim 1, characterized in that: In step (4), the mass ratio of the hydroxypropyl-β-cyclodextrin to the deionized water is 1:

9.

5. The method for preparing the HP-β-CD nanosilver antibacterial material according to claim 1, characterized in that: In step (5), the mass ratio of the nanosilver particles to the hydroxypropyl-β-cyclodextrin solution is 1:1; and the speed of continuous stirring is 200 rpm.

6. The method for preparing the HP-β-CD nanosilver antibacterial material according to claim 1, characterized in that: In step (6), the freeze-drying conditions are: freeze-drying at -50°C for 24 hours.

7. A sterilization device for tobacco flavors and fragrances, characterized in that: The invention comprises an outer shell (201) which is a hollow three-dimensional cylindrical structure. A filter screen (202) is arranged inside the inner ring of the outer shell (201). HP-β-CD nano silver antibacterial material (203) is filled between the outer shell (201) and the filter screen (202). A filtering device (204) is arranged at the bottom end of the filter screen (202).

8. Use of the HP-β-CD nanosilver antibacterial material according to any one of claims 1 to 6 in sterilization in tobacco flavors.

9. The use according to claim 8, characterized in that: The application is to sterilize tobacco flavors using HP-β-CD nano-silver antibacterial materials, including the following steps: (1) The flavors and fragrances flow into the sterilization device from the top, and flow out from the bottom of the device after being sterilized by the HP-β-CD nano-silver antibacterial material inside; (2) Repeat the above step (1) three times, with the sterilization time being no less than 10 min; (3) After sterilization, rinse the sterilization equipment with pure water, dry at 45℃ and seal for storage.

Images