CN115812888A - Attapulgite/antibacterial lipopeptide composite material and preparation method and application thereof - Google Patents
Attapulgite/antibacterial lipopeptide composite material and preparation method and application thereof Download PDFInfo
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Images
Abstract
The invention discloses an attapulgite/antibacterial lipopeptide composite material and a preparation method and application thereof. Under unit conditions, the modified attapulgite can load more than 367.97mg/L of bacillomycin D under the conditions of 2h and 40 ℃, and the loading rate is as high as 93.13%. Meanwhile, the composite material under unit conditions can remove 11.08ppb of aflatoxin B at 2h and 50 DEG C 1 The removal rate can reach more than 80%. The composite material prepared by the invention can resist bacteria, remove mycotoxin and has stabilityGood antibacterial property, wide application range, and solves the limitation problems of poor antibacterial property of inorganic materials and poor stability of organic materials, no acid and alkali resistance, easy oxidation and the like.
Description
Technical Field
The invention relates to the technical field of biological materials, and particularly relates to an attapulgite/antibacterial lipopeptide composite material, and a preparation method and application thereof.
Background
Along with the improvement of living standard and the increase of attention to health life, the demands of people on living environment and health care are higher and higher, and particularly, the safety and the reassurance of eating the health food become the first problems considered by most people in the aspect of food safety. Ubiquitous harmful fungi are a major cause of food safety hazards. Therefore, the research and development of antibacterial agents are receiving more and more attention.
Bacitracin D (BD) is a natural antimicrobial lipopeptide produced by the secondary metabolism of Bacillus and is a cyclic lipopeptide formed by the linkage of a hydrophilic heptapeptide and a hydrophobic beta-amino fatty acid chain (Anti-toxin enzymes and toxin-reducing effects of Bacillus D in combination with antibiotics. Toxicon,2022, 216, 107-113.). Bacillus D has good Biological activity against fungi, tumors, etc. (Biological activity of lipids from Bacillus and Biotechnology,2017, 101 (15): 5951-5960), which makes it have a wide application prospect in Food preservation, food storage, and biomedicine, etc. (effective of combined Bacillus D and yeast on growth of microorganisms storage and Botrytis circuits and microbial preservation. Journal of the Science of Food and Agriculture,2020, 101 (1): 229-239.
Aflatoxins are secondary metabolites produced by aspergillus flavus and aspergillus parasiticus and are highly toxic and carcinogenic (arachi hypothoaea l.). World Mycotoxin Journal,2018, 11. These fungi can infect crops, including peanuts and corn, during growth, harvesting, drying, storage and other processes (world aflatoxin regulation of agricultural products and foods: from Ocurrence to control. Comprehensive Reviews in Food Science and Food Safety,2021, 20 2332-2381.). In recent years, much research has focused on preventing and controlling the growth of fungi and mycotoxins.
Attapulgite (ATP, jiangsu Jichu nano materials Science and technology Co., ltd.) is a crystalline hydrated magnesium aluminum silicate Clay mineral with a lamellar chain fibrous structure, widely available around the world, and low in price (crystalline new applications for Kaolin, small, and palygorskite: a general overview. Applied Clay Science,2000, 17 (5): 207-221). It consists of two continuous tetrahedral layers and a 2: 1 strip-shaped discontinuous octahedral layer, the interior of the crystal is porous, the external surface is concave-convex, and the edge has multiple Si-OH bonds (Effect of pH, ionic strength, temperature and humidity subsistence on the basis of the reflection of Ni (II) to Na-absorption. Chemical engineering Journal,2008, 150 (1): 188-195). The basic structure of attapulgite clay makes it a natural nanomaterial, exhibiting various excellent physicochemical properties such as adsorption, rheology, etc. (Preparation of well-defined stator polymer from highly branched macroporous adsorbent based adsorption anode by surface-inorganic transport polymerization technique&Engineering Chemistry Research,2007, 46 (1): 97-102) with adsorption performance determined by its large specific surface area, surface physical-chemical structure and its ion state, and its adsorption including physical adsorption, chemical adsorption and ion exchange adsorption (Magnetic gamma-Fe) 2 O 3 -loaded attapulgite sorbent for Hg-0removal in coal-fired flue gas.Energy&Fuel,2019, 33 (8): 7522-7533). Therefore, the attapulgite is widely applied to the fields of chemical industry, light industry, agriculture, textile, building materials, geological exploration, casting, silicate industry, atomic energy industry, environmental protection, pharmacy and the like, is acid-base resistant and good in stability, is an excellent material carrier, is listed as a food processing aid allowed to be used in food by GB 29225-2012, and is gradually added and applied to food besides the adsorption and removal of heavy metal ions in the environment. But it isPoor antibacterial properties (characteristics of a new antibacterial of tissue group: bacillus D.J. Antibiot (Tokyo) 1980, 33 (10): 1146-9.) are also important problems.
The Bacillomycin D has good biological activities such as antifungal and antitumor (Bacillomycin D: the present invention relates to a Food preservative and Food preservation composition, which has a broad application prospect in Food preservation, and biomedicine (Effect of combined Bacillus D and yeast on growth of Rhizopus stolonifer and Botrytis cinerea and cell preservation. Journal of the Science of Food and cultivation, 2020, 101 (1) 229-239 microbial peptide self-assembly a method-tissue of Food-grade tissue and Food preservation, 21018 (2024): 2023).
The attapulgite was approved by the U.S. department of agriculture, AAFCO approved, and passed the review by the U.S. department of agriculture. The united states food and drug administration recognizes that it can be used in animal feed. The basic structure of the attapulgite enables the attapulgite to form a natural nano material, thereby showing various excellent physical and chemical properties such as adsorbability, rheological property and the like, and being widely applied to the fields of chemical industry, light industry, agriculture, textile, building materials, geological exploration, casting, silicate industry, atomic energy industry, environmental protection, pharmacy and the like.
In the prior art, mycotoxins such as bacillomycin D and the like are mainly directly applied or a strain producing the bacillomycin D is directly fermented to achieve the bacteriostatic effect, and the bacteriostatic effect of the bacillomycin D may be lost due to the defects of easy oxidation, poor stability and the like of the bacillomycin D. Currently, few researchers have studied on materials capable of carrying bacitracin D to improve the disadvantages of poor stability and the like.
Disclosure of Invention
Aiming at the problems mentioned in the background technology, the invention provides an attapulgite/antibacterial lipopeptide composite material and a preparation method thereof, wherein natural attapulgite is modified by sulfuric acid, then the modified attapulgite is used for loading mycotoxin such as bacillomycin D, and the mycotoxin is firmly combined on the surface in a covalent bond mode to prepare a novel composite material which is marked as H-ATP-BD. The attapulgite/antibacterial lipopeptide composite material prepared by the invention has good antibacterial performance and stability, solves the problems of poor water solubility, no alkali resistance, easy oxidation, poor stability and the like of the bacillomycin D, and can be better applied to the fields of food preservation, grain storage and the like.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of an attapulgite/antibacterial lipopeptide composite material is characterized by comprising the following steps: the method comprises the following steps:
step (1): preparation of bacillomycin D: extracting the bacillomycin D, diluting the bacillomycin D with deionized water, and freeze-drying;
step (2), preparing modified attapulgite by using an acid solution;
and (3) loading the modified attapulgite on the bacillomycin D: and (3) adding the attapulgite modified in the step (2) into a bacillomycin D aqueous solution, carrying for a period of time, and carrying out ultrasonic treatment to obtain the attapulgite/antibacterial lipopeptide composite material, wherein the attapulgite/antibacterial lipopeptide composite material is recorded as H-ATP-BD.
Preferably, in step (1), the dilution ratio of bacitracin D to deionized water is 1: 30 to 1: 50 (v: v). The dilution ratio of bacitracin D and deionized water is any value in the range of 1: 30 to 1: 50, such as 1: 30, 1: 35, 1: 40, 1: 45, 1: 50.
In any of the above embodiments, preferably, in the step (2), the acidic solution is sulfuric acid, and the concentration of the sulfuric acid is 0.5 to 4mol/L. The concentration of sulfuric acid is any value within the range of 0.5 to 4mol/L, such as 0.5mol/L,1mol/L,2mol/L,3mol/L,4mol/L.
In any of the above schemes, preferably, in the step (3), in the process of loading bacitracin D on the modified attapulgite, the addition amount of the modified attapulgite is 0.1-0.5 wt%, the loading temperature is 30-70 ℃, the stirring speed is 300-700r/min, and the loading time is 0-300min. Specifically, the addition amount of the modified attapulgite can be any value within the range of 0.1-0.5 wt%, such as 0.1%,0.2%,0.3%,0.4%,0.5%; the loading temperature is any value within the range of 30-70 ℃, such as 30 ℃,35 ℃,40 ℃,45 ℃,50 ℃,60 ℃ and 70 ℃; the stirring rate is any value within the range of 300-700r/min, such as 300r/min,400r/min,450r/min,500r/min,550r/min,600r/min,700r/min; the loading time is 0-300min, such as 1min,5min,50min,100min,150min,200min,300min.
In any of the above schemes, preferably, in the step (3), in the process of loading the modified attapulgite with the bacillomycin D, the addition amount of the modified attapulgite is 0.2-0.4wt%, the loading temperature is 35-45 ℃, the stirring rate is 450-550r/min, and the loading time is 100-150min.
In any of the above schemes, preferably, in the step (3), the ultrasonic treatment condition is 40kHz for 30min.
The invention also discloses an attapulgite/antibacterial lipopeptide composite material prepared by the preparation method.
The invention also discloses application of the attapulgite/antibacterial lipopeptide composite material in removing mycotoxin.
Preferably, the mycotoxin at least comprises one or more of aflatoxin and/or aspergillus niger and/or bacillomycin.
Preferably in any of the above schemes, the aflatoxin is specifically aflatoxin B 1 The bacillomycin is bacillomycin D.
Preferably, the application method of the attapulgite/antibacterial lipopeptide composite material in removing aflatoxin and/or fumagillin is as follows: preparing mother liquor without aflatoxin and/or aspergillus niger in advance, and respectively adding a solution without aflatoxin and/or aspergillus niger and the attapulgite/antibacterial lipopeptide composite material prepared by the preparation method into a beaker.
The aflatoxin is specifically aflatoxin B 1 The application separately derives from aflatoxin B at different initial concentrations 1 The addition amount of different composite materials, different removal time and different removal temperature of the composite material to aflatoxin B 1 The removal effect of (2) was investigated.
The invention discloses a preparation method and application of an attapulgite/antibacterial lipopeptide composite material.
Advantageous effects
1. According to the invention, sulfuric acid is adopted to modify natural attapulgite, so that some carbonate impurities contained in the natural attapulgite are removed, the surface adsorption sites of the natural attapulgite are increased, the loading effect is efficiently improved, then the modified attapulgite is used to load bacillomycin D, and the modified attapulgite is firmly combined on the surface in a covalent bond mode, so that a novel composite material (marked as H-ATP-BD) is prepared. Under the unit condition, the modified attapulgite can load bacillomycin D of more than 367.97mg/L under the conditions of 2h and 40 ℃, the load rate is as high as 93.13%, and the prepared composite material and the bacillomycin D have no significant difference in mould inhibition effect. And secondly, the bacillomycin D is fixed on the surface of the modified attapulgite in a covalent bond combination mode, and has strong desorption resistance. Meanwhile, the composite material under unit conditions can remove 11.08ppb of aflatoxin B at 2h and 50 DEG C 1 The composite material prepared by the invention has good antibacterial performance and good stability, overcomes the defects of poor water solubility, no alkali resistance, easy oxidation, poor stability and the like of the bacillomycin D, and can be better applied to the fields of food preservation, grain storage and the like.
2. According to the invention, natural attapulgite is used as an excellent carrier, and bacillus mycin D is efficiently loaded after modification by sulfuric acid, so that the composite material which has good antifungal activity and can remove mycotoxin is prepared. Provides a feasible technology for solving the problem of food infected by mycotoxin.
3. The modified attapulgite prepared by the method has a good loading effect on the bacitracin D, the maximum loading capacity of the unit modified attapulgite on the bacitracin D can reach 367.97mg/L, and the loading rate can reach 93.13%. And the modified attapulgite is loaded on the bacillomycin D in a chemical adsorption manner combined by covalent bonds, so that compared with physical adsorption, the load effect is firm and stable, and the risk of falling off after loading is reduced.
4. The composite material prepared by the method of the invention can be used for treating aflatoxin B 1 Also has good removal effect, and the unit composite material has good effect on aflatoxin B 1 The removal amount of the composite material can reach 11.08ppb, the removal rate reaches more than 80 percent, and the composite material is green and easy to remove.
5. The preparation method is an organic (bacillomycin D)/inorganic (modified attapulgite) compounding mode. The advantages of the organic material and the inorganic material can be complemented, and the prepared composite material has the advantages of the attapulgite and the bacillomycin D.
6. The method for preparing the modified attapulgite capable of loading the bacillomycin D has the advantages of low cost, simple preparation method and no environmental pollution and resource waste. And the attapulgite is extremely rich in mineral resources, belongs to food-grade additives, and can be directly applied to grain storage, fruit and vegetable preservation, animal feed and biomedicine.
7. The composite material prepared by the invention can resist bacteria and remove mycotoxin, has good stability and wide application range, and solves the problems of poor antibacterial performance of inorganic materials and poor stability of organic materials, no acid and alkali resistance, easy oxidation and the like. Secondly, the composite material prepared by the preparation method has low preparation cost, does not use organic solvent, is not easy to cause secondary pollution, and does not pollute the environment.
Drawings
FIG. 1 is a flow chart of a method of preparing an attapulgite/antimicrobial lipopeptide composite material according to the present invention;
FIG. 2 is an ATR diagram of a modified attapulgite prepared according to the present invention; a is ATR picture of natural attapulgite and modified attapulgite, B is ATR picture after attapulgite loads bacillomycin D;
FIG. 3 is an SEM image of a modified attapulgite prepared according to the present invention; a is natural attapulgite, B is 0.5mol/L sulfuric acid modified attapulgite, C is 1mol/L sulfuric acid modified attapulgite, D is 2mol/L sulfuric acid modified attapulgite, and E is 4mol/L sulfuric acid modified attapulgite;
FIG. 4 is a graph showing the variation trend of different single-factor experiments on modified attapulgite loaded with bacitracin D in the present invention; FIG. A shows the effect of sulfuric acid modified attapulgite with different concentrations on the load bacillomycin D; FIG. B shows the effect of different addition amounts of modified attapulgite on the load bacillomycin D; panel C is the effect of different temperatures on the load bacitracin D; panel D is the effect of different loading times on the loading of bacitracin D; panel E shows the effect of the starting concentration of different bacillomycin D on loading.
FIG. 5 is an XRD pattern of a composite material prepared by single factor optimization of the present invention;
FIG. 6 is a test of Aspergillus flavus inhibition by the composite material prepared by single factor optimization;
FIG. 7 is a bacteriostasis test of the composite material prepared by single factor optimization of the present invention to Aspergillus niger;
FIG. 8 shows the aflatoxin B pair of composite material prepared by single-factor optimization 1 The removal experiment of (1); graph a shows the effect of different aflatoxin concentrations on removal; FIG. B is the effect of different addition amounts of the composite material on aflatoxin removal; FIG. C is the effect of different temperatures on aflatoxin removal; panel D is the effect of different removal times on aflatoxin removal.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only other embodiments that can be obtained by a person skilled in the art without any creative efforts, and all of them belong to the protection scope of the present invention. The relevant materials appearing in the subsequent examples are prepared in the preceding examples without specific mention.
Example 1
A preparation method of an attapulgite/antibacterial lipopeptide composite material is shown in a preparation flow chart of figure 1, and specifically comprises the following steps:
modification of attapulgite: taking 10g of natural attapulgite (Jiangsu Jiuzhuachuan nano-material science and technology Limited, 200 meshes), adding 50mL of sulfuric acid with the concentration of 0.5-4.0mol/L, carrying out vortex mixing for 30s, stirring for 3H in a water bath at 90 ℃, carrying out suction filtration while the mixture is hot, washing the mixture for multiple times by using ultrapure water to be neutral, putting the mixture into an electric heating forced air drying oven for drying for 24H at 45 ℃, grinding the mixture, and sieving the ground mixture by using a 100-mesh sieve to obtain attapulgite modified by different acids, wherein the attapulgite is respectively marked as 0.5M-H-ATP,1M-H-ATP,2M-H-ATP and 4M-H-ATP;
FIG. 3 is an SEM image of a modified attapulgite prepared according to the present invention; a is natural attapulgite, B is 0.5mol/L sulfuric acid modified attapulgite, C is 1mol/L sulfuric acid modified attapulgite, D is 2mol/L sulfuric acid modified attapulgite, and E is 4mol/L sulfuric acid modified attapulgite;
preparation of bacillomycin D: bacillus subtilis fmbJ and its inhibition effects obtained by Gongwei et al (Identification of Bacillus sp. Fumonis 2014 (1): 8-14) was used to extract bacomycin D. Diluting bacitracin D with ultrapure water at a ratio of 1: 30 (v/v), and freeze-drying; and re-dissolving the freeze-dried sample with ultrapure water to obtain the bacillomycin D solution required by the experiment.
Example 2
20mg of attapulgite which is not modified in the embodiment 1 and before modification are respectively added into 5mL of bacitracin D solution (prepared in the embodiment 1), vortex mixing is carried out for 30s, stirring is carried out for 2h at 500r/min at room temperature, and ultrasonic treatment is carried out for 30min, so that the attapulgite/antibacterial lipopeptide composite material loaded with the bacitracin D is obtained.
Example 3
1mL of modified attapulgite loaded with bacitracin D (prepared in example 2) was centrifuged at 8000r/min at 4 ℃ for 4min; taking the supernatant to pass through an inorganic filter membrane with the thickness of 0.45 μm, adopting Gong Qingwei and the like (Identification of Bacillus subtilis mbJ and its inhibition effects against Bacillus flavus. Food Control 2014) to measure the concentration of the bacillomycin D by using a high performance liquid chromatograph, and calculating the loading rate of the bacillomycin D. The load factor calculation formula is as follows:
in the formula: c. C 0 Initial concentration of bacitracin D (mg/L); c. C e The concentration of bacitracin D (mg/L) at which the load reached equilibrium.
Example 4
20mg of attapulgite modified with different acid concentrations were added to 5mL of bacitracin D solution (prepared in example 1), vortex mixed for 30s, stirred at 500r/min for 2h at room temperature, and sonicated for 30min. Centrifuging the attapulgite solution loaded with the bacillomycin D for 4min at 4 ℃ at 8000 r/min; the supernatant was filtered through an inorganic filter of 0.45 μm, and the concentration of the bacillomycin D was measured by Gong Qingwei et al using a high performance liquid chromatograph and the loading rate was calculated. As shown in FIG. 4A, the concentration of sulfuric acid of 1mol/L is preferably selected to modify the attapulgite, and the load factor can reach 90.30%.
Example 5
Adding 10-50mg of attapulgite modified by 1mol/L sulfuric acid into 5mL of bacitracin D solution, vortex mixing for 30s, stirring at room temperature at 500r/min for 2h, and performing ultrasonic treatment for 30min. Centrifuging the attapulgite solution loaded with the bacillomycin D for 4min at 4 ℃ at 8000 r/min; the supernatant was filtered through an inorganic filter of 0.45 μm, and the concentration of bacitracin D was measured by HPLC using the method known as Gong-Gegh et al, and the loading rate was calculated. As shown in FIG. 4B, the addition amount of 30mg of acid-modified attapulgite is preferably selected to load the bacitracin D, and the loading rate can reach 92.51%.
Example 6
Adding 30mg of attapulgite modified by 1mol/L sulfuric acid into 5mL of bacitracin D solution, vortex mixing for 30s, stirring at 30-70 deg.C for 2h at 500r/min, and performing ultrasonic treatment for 30min. Centrifuging the attapulgite solution loaded with the bacillomycin D for 4min at 4 ℃ at 8000 r/min; the supernatant was filtered through an inorganic filter of 0.45 μm, and the concentration of the bacillomycin D was measured by Gong Qingwei et al using a high performance liquid chromatograph and the loading rate was calculated. As shown in FIG. 4C, the acid-modified attapulgite is preferably selected to load the bacitracin D at 40 ℃, and the loading rate can reach 92.46%.
Example 7
Adding 30mg of attapulgite modified by 1mol/L sulfuric acid into 5mL of bacitracin D solution, vortex mixing for 30s, stirring at 40 deg.C at 500r/min for 0-360min, and performing ultrasonic treatment for 30min. Centrifuging the attapulgite solution loaded with the bacillomycin D for 4min at 4 ℃ at 8000 r/min; the supernatant was filtered through an inorganic filter of 0.45 μm, and the concentration of the bacillomycin D was measured by Gong Qingwei et al using a high performance liquid chromatograph and the loading rate was calculated. As shown in FIG. 4D, the acid-modified attapulgite is preferably selected to load the bacillomycin D under the condition of stirring at 400r/min for 240min, and the loading rate can reach 93.13%.
Example 8
The experiments of Fourier transform infrared spectroscopy, a scanning electron microscope, an X-ray diffractometer and the like verify that the clarithromycin D is loaded on the surface of the attapulgite through chemical action, so that the biological activity of the bacillomycin D is well protected, and the antibacterial performance of the bacillomycin D is not reduced.
Fourier transform infrared spectrum results show that the attapulgite material disclosed by the invention is subjected to acid modification, and then some carbonate impurities carried by the attapulgite material are removed, so that the attapulgite material is beneficial to later-stage loading of the bacitracin D, as shown in figure 2A. The infrared spectrogram of the modified attapulgite loaded with the bacillomycin D is larger at 1535cm -1 A stretching vibration absorption peak of an aromatic hydrocarbon carbon skeleton appears nearby, which shows that the bacillomycin D is firmly bonded to the surface of the modified attapulgite by means of a covalent bond, as shown in fig. 2B.
Scanning electron microscopy showed that the attapulgite material used in the present invention was in the micron range. And with the modification of sulfuric acid, the surface pore structure of the copper-nickel alloy tends to increase and then decrease, which indicates that the crystal structure of the copper-nickel alloy is damaged and the surface adsorption active sites of the copper-nickel alloy are reduced due to the overhigh acid concentration. The result shows that the good sulfuric acid concentration is selected, so that the modified attapulgite is more favorable for loading the bacillomycin D, as shown in figure 5.
The characterization result of an X-ray diffraction instrument shows that the crystal characteristic peaks of the modified attapulgite loaded with the bacillomycin D are obviously higher than the crystal characteristic peaks of the bacillomycin D at 2 theta =31.50 degrees and 45.27 degrees. Indicating that the bacillomycin D is successfully loaded on the surface of the attapulgite, as shown in figure 5.
Example 9
The results of bacteriostatic experiments show that the prepared composite material has obvious inhibition effect on aspergillus niger (A.niger, MK 779059.1) and aspergillus flavus (A.oryzae, MTO 93257.1) which are common in grains. The modified attapulgite has no bacteriostatic effect on aspergillus flavus and aspergillus niger, the size of a bacteriostatic zone of the bacillomycin D on the aspergillus flavus is (20.95 +/-0.56) mm, the size of the bacteriostatic zone of the bacillomycin D on the aspergillus flavus is (20.30 +/-0.21) mm, as shown in figure 6, the size of the bacteriostatic zone of the bacillomycin D on the aspergillus niger is (20.22 +/-0.02) mm, the size of the bacteriostatic zone of the composite material on the aspergillus niger is 19.70 +/-0.36) mm, as shown in figure 7, no significant difference exists, and the composite material prepared is proved to have good antifungal activity.
Example 10
20mg of the composite material prepared by the optimal conditions of the above example was added to 5mL of aflatoxin B of different concentrations 1 To the solution, vortex for 30s and stir at 500r/min for 2h at room temperature. Centrifuging the mixed solution at 4 deg.C and 6000r/min for 10min; collecting supernatant, filtering with 0.22 μm organic filter membrane, and detecting aflatoxin B in peanut and its products by adopting Rongshaoyao cary (isotope internal standard-ultra high performance liquid chromatography-tandem mass spectrometry) 1 Food safety quality testing bulletin, 2021, 12 (22): 8643-8650.) et al, by using ultra high performance liquid chromatography-tandem mass spectrometry 1 And calculating the removal efficiency thereof. The removal rate calculation formula is as follows:
in the formula: c 0 Is aflatoxinB 1 Initial concentration (ppb); c e To remove aflatoxin B when equilibrium is reached 1 Concentration (ppb)
Wherein, as shown in FIG. 8A, aflatoxin B is followed 1 The initial concentration is increased, and the composite material prepared by the invention is used for treating aflatoxin B 1 The removal efficiency of (a) is a trend of increasing and then decreasing, because the composite material surface has more removal sites at the initial removal, so the removal efficiency is very high, and along with the aflatoxin B 1 The removal sites of the composite material are gradually filled by the increase in concentration, resulting in a decrease in removal efficiency. Preferred aflatoxins B for subsequent experiments 1 Has a concentration of about 30 ppb.
Example 11
10-50mg of the composite material is taken and added into 5mL of 36.40ppb aflatoxin B 1 To the solution, vortex for 30s and stir at 500r/min for 2h at room temperature. Centrifuging the mixed solution at 4 deg.C and 6000r/min for 10min; taking the supernatant, filtering the supernatant with an organic filter membrane of 0.22 mu m, and determining aflatoxin B by using the method of Wangshao Yingyang et al and by using ultra-high performance liquid chromatography-tandem mass spectrometry 1 And calculating the removal efficiency thereof. As shown in FIG. 8B, the amount of the composite material added is preferably 30mg to remove aflatoxin B 1 The removal rate can reach 52.66%.
Example 12
Adding 30mg of the composite material into 5mL of 44.15ppb aflatoxin B solution, mixing by vortex for 30s, and stirring at 50 ℃ at 500r/min for 0-360min. Centrifuging the mixed solution at 4 deg.C and 6000r/min for 10min; taking the supernatant, filtering the supernatant with an organic filter membrane of 0.22 mu m, and determining aflatoxin B by using the method of Wangshao Yingyang et al and by using ultra-high performance liquid chromatography-tandem mass spectrometry 1 And calculating the removal efficiency thereof. Wherein, as shown in FIG. 8C, the composite material is preferably selected to remove aflatoxin B 1 The time is 120min, and the removal rate can reach 66.49%.
Example 13
30mg of the composite material was added to 5mL of 44.20ppb of aflatoxin B 1 The solution was vortexed for 30 seconds and stirred at 500r/min for 2h at 20-70 ℃. Centrifuging the mixed solution at 4 deg.C and 6000r/min for 10min; taking the supernatant, passing through an organic filter membrane of 0.22 mu m, determining the concentration of the aflatoxin B1 by using an ultra-high performance liquid chromatography-tandem mass spectrometry method by adopting a method of Wangshao Yingyang et al, and calculating the removal efficiency. As shown in FIG. 8D, the composite material is preferably selected to remove aflatoxin at 50 ℃, and the removal rate can reach 89.06%.
The attapulgite/antibacterial lipopeptide composite material and the preparation method thereof provided by the invention have the advantages that the prepared composite material can be well applied to grain storage, fruit and vegetable preservation and animal feed.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of an attapulgite/antibacterial lipopeptide composite material is characterized by comprising the following steps: the method comprises the following steps:
step (1): preparation of bacillomycin D: extracting the bacillomycin D, diluting the bacillomycin D with deionized water, and freeze-drying;
step (2) preparing modified attapulgite by using an acid solution;
and (3) loading the bacillomycin D by the modified attapulgite: and (3) adding the attapulgite modified in the step (2) into a bacitracin D aqueous solution, carrying for a period of time, and carrying out ultrasonic treatment to obtain the attapulgite/antibacterial lipopeptide composite material.
2. The method for preparing the attapulgite/antibacterial lipopeptide composite material according to claim 1, characterized in that: in the step (1), the dilution ratio of the bacillomycin D and the deionized water is 1: 30-1: 50 (v: v).
3. The method for preparing an attapulgite/antibacterial lipopeptide composite material according to claim 1, characterized in that: in the step (2), the acid solution is sulfuric acid, and the concentration of the sulfuric acid is 0.5-4mol/L.
4. The method for preparing an attapulgite/antibacterial lipopeptide composite material according to claim 1, characterized in that: in the step (3), in the process of loading the modified attapulgite with the bacitracin D, the addition amount of the modified attapulgite is 0.1-0.5 wt%, the loading temperature is 30-70 ℃, the stirring speed is 300-700r/min, and the loading time is 0-300min.
5. The method for preparing an attapulgite/antibacterial lipopeptide composite material according to claim 1, characterized in that: in the step (3), in the process of loading the modified attapulgite with the bacitracin D, the addition amount of the modified attapulgite is 0.2-0.4wt%, the loading temperature is 35-45 ℃, the stirring speed is 450-550r/min, and the loading time is 100-150min.
6. The method for preparing an attapulgite/antibacterial lipopeptide composite material according to claim 1, characterized in that: in the step (3), the ultrasonic treatment condition is 40kHz and lasts for 30min.
7. An attapulgite/antibacterial lipopeptide composite material prepared by the preparation method of any one of claims 1 to 6.
8. Use of the attapulgite/antibacterial lipopeptide composite material according to claim 7 for the removal of mycotoxins.
9. The use according to claim 8, wherein the mycotoxins comprise one or more of aflatoxins and/or fumagillin and/or bacitracin.
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| CN114774498A (en) * | 2022-05-06 | 2022-07-22 | 南京财经大学 | Method for producing bacillomycin D by fermenting bacillus immobilized by diatomite |
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