CN103054128A - Application of nanometer magnesium oxide as antimicrobial - Google Patents
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- CN103054128A CN103054128A CN2012105931405A CN201210593140A CN103054128A CN 103054128 A CN103054128 A CN 103054128A CN 2012105931405 A CN2012105931405 A CN 2012105931405A CN 201210593140 A CN201210593140 A CN 201210593140A CN 103054128 A CN103054128 A CN 103054128A
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Abstract
The invention discloses application of nanometer magnesium oxide as antimicrobial. According to the invention, the application is that nanometer magnesium oxide granules are used as the antimicrobial of Candida tropicalis; and the nanometer magnesium oxide granules provided by the invention have the characteristics of non-toxicity, good inhibition effect to common beverage microbes, good potential to be used as preservative for acid beverage, and particularly remarkable inhibition effect to the Candida tropicalis in acid beverage. The nanometer magnesium oxide is simple and convenient to prepare, and magnesium oxide powder of different grain diameters can be prepared through controlling the calcination conditions of precursor, so that the nanometer magnesium oxide is suitable for industrial production.
Description
(1) technical field
The present invention relates to a kind of nano oxidized magnesium granules as the application of bacteriostatic agent, be specifically related to nano oxidized magnesium granules candida tropicalis (Candida tropicalis) is had the inhibition growth.
(2) background technology
Beverage is the necessity in our daily life.Beverage is because its nutritional labeling is abundant, is very easy to be subject to the pollution of microorganism in processing and sales process, all needs to add a certain amount of anticorrisive agent in the commercialization beverage for this reason.Anticorrisive agent mainly is divided into chemical preservative and natural antiseptic agent two large classes.Chemical preservative is divided into again organic anti-corrosive agent and inorganic corrosion inhibitor.The former mainly comprises benzoic acid, sorbic acid etc., and the latter mainly comprises sulphite and nitrite etc.Natural antiseptic agent normally extracts from the metabolite of animal, plant and microorganism.Although antiseptics for natural food is nontoxic, the price of antiseptics for natural food is high at present, does not also form scale and uses.In food beverage industry, chemical preservative is benzoic acid, sorbic acid etc. or main flow particularly at present.But along with the raising of people to health requirements, people are to anticorrisive agent research and use more and more concern.
Nano oxidized magnesium granules is a kind of novel high function fine inorganic material, is widely used in fields such as electronics, catalysis, pottery, food.Nanometer magnesia powder because the particularity of its structure has larger specific area, has certain antibacterial and sterilizing ability.Document Peter K. Stoimnov, Rosalyn L. Klinger, George L. Marchin, and Kenneth J. Klabunde, Langmuir points out among 2002, the 18:6679-6686, and particle diameter is about 4 nm, and specific surface reaches 1000 m
2The nanometer magnesia powder absorption halogen of/g is adsorbed on bacterium and spore surface with electrostatic force, so that cell membrane is destroyed, cell interior liquid flows out, thereby reaches bactericidal effect.At present, existing a lot of about the preparation of Mgo Nanopowder and the report of bacteriostasis property.All concentrate on neutral environment about its bacteriostasis property research, zinc oxide nano-powder shows good fungistatic effect.There is not relevant report about its application in sour environment.In addition, magnesium is highly profitable to health as the trace element of the necessary daily iron supplement of human body.For this reason, in the acidic beverages field, Mgo Nanopowder has the potentiality that become anticorrisive agent very much.
(3) summary of the invention
The object of the invention provides a kind of nano oxidized magnesium granules anti-microbial property in acidic beverages, the bitter earth nano particle is used in beverage industry as inorganic antiseptic, is specially meter magnesium oxide particle as the bacteriostatic agent of candida tropicalis (Candida tropicalis).
The technical solution used in the present invention is:
The invention provides a kind of nano magnesia as the application of antiseptic, describedly be applied as nano oxidized magnesium granules as the bacteriostatic agent of candida tropicalis (Candida tropicalis).
Further, the particle diameter of described nano oxidized magnesium granules is 4 ~ 150nm.
Further, the quality consumption of described nano oxidized magnesium granules is counted 0.02 ~ 0.05 mg/ 10 with Candida tropicalis strain cell number
4CFU.
Further, described nano oxidized magnesium granules prepares as follows: under the room temperature, 1.0 ~ 2.0 mol/L magnesium nitrate aqueous solutions are added drop-wise in 1.0 ~ 2.0mol/L soluble carbon acid sodium aqueous solution, under 150 ~ 250W ultrasound condition, mix 10 ~ 30 minutes, obtain emulsion, with at room temperature ageing of emulsion 3 ~ 5 hours, filtration, washing, freeze drying, pulverizing, obtain the basic magnesium carbonate presoma, presoma is warming up to 450 ~ 800 ℃ with the speed of 3 ~ 10 ℃/min, calcined 2 ~ 5 hours, and obtained nano oxidized magnesium granules; In the described magnesium nitrate solution in magnesium nitrate and the soluble carbon acid sodium solution the feed intake ratio of amount of substance of solubility carbonic acid sodium be 1:1 ~ 1.3.
Further, described application is with the bacteriostatic agent of nano oxidized magnesium granules as candida tropicalis in the acidic beverages.
Further, described acidic beverages is that the pH value is 2.5 ~ 5.5.
Nano oxidized magnesium granules of the present invention is as raw material take solubility magnesium salts and soluble carbonate salt, make first the basic magnesium carbonate precursor, prepare by the control calcination condition, concrete recommendation is carried out as follows: 2.0 mol/L magnesium nitrate aqueous solution 50ml are joined the ultrasonic response container, dripping concentration under the room temperature is that 2.0 mol/L soluble carbon acid sodium aqueous solution 55ml obtain white emulsion, under the 250W ultrasound condition, mix 20 minutes again, with ageing under the emulsion room temperature that obtains 5 hours, filter, washing, freeze drying, pulverize, obtain the basic magnesium carbonate presoma, presoma is warming up to 450 ~ 800 ℃ with 3 ~ 10 ℃/min speed, calcined 2 ~ 5 hours, can obtain particle diameter is the white nano oxidized magnesium granules of 4 ~ 150 nm sizes.
Compared with prior art, beneficial effect of the present invention is mainly reflected in:
That nano oxidized magnesium granules provided by the invention has is nontoxic, common beverage microorganism is had the preferably characteristics such as antibacterial efficient, have as the good potential quality of acidic beverages anticorrisive agent, especially candida tropicalis in the acidic beverages had obvious fungistatic effect, its preparation method is easy, can prepare by control presoma calcination condition the magnesium oxide particle of different-grain diameter, be fit to suitability for industrialized production.
(4) description of drawings
The nano magnesia transmission electron microscope photo of Fig. 1 embodiment 1 preparation;
The nano magnesia X-ray diffractogram of Fig. 2 embodiment 1 preparation;
The particle diameter of nano oxidized magnesium granules is to the fungistatic effect of candida tropicalis in the cider among Fig. 3 embodiment 6;
The particle diameter of nano oxidized magnesium granules is to the fungistatic effect of candida tropicalis in the orange juice among Fig. 4 embodiment 6;
The concentration of nano oxidized magnesium granules is to the fungistatic effect of candida tropicalis in the cider among Fig. 5 embodiment 6;
The concentration of nano oxidized magnesium granules is to the fungistatic effect of candida tropicalis in the orange juice among Fig. 6 embodiment 6.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The preparation of nano magnesia: 1.0 mol/L magnesium nitrate aqueous solution 25ml are joined (Sonicafier 450 in the ultrasonic response container, Branson Ultrasonics corporation, the U.S.), the lower 1.0 mol/L soluble carbon acid sodium aqueous solution 25ml that drip of room temperature (25 ℃) obtain white emulsion, under the 250W ultrasound condition, mix 20 minutes, with the at room temperature ageing of emulsion that obtains 5 hours, then filter, at-50 ℃ of freeze drying 3h, pulverize after the filter cake washing, obtain the basic magnesium carbonate presoma, presoma is warmed up to 450 ℃ with 5 ℃/min speed, calcined 1.5 hours, and got white nano oxidized magnesium granules, particle diameter 25 nm.Scanning electron microscope (SEM) photograph is seen Fig. 1, and X-ray diffractogram as shown in Figure 2.
Biocidal property: with above-mentioned nano oxidized magnesium granules and bacteria suspension (10
6CFU/mL) join in the cider, in cider, cell concentration 10
4CFU/mL, nano magnesia granule density are 300ppm.Sample stores 21 days at ambient temperature, and sampling in per 3 days utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.The result shows that room temperature storage did not detect any bacterium colony after 21 days.
Embodiment 2
The preparation of nano magnesia: 1.5 mol/L magnesium nitrate aqueous solution 50ml are joined the ultrasonic response container, drip 1.0 mol/L soluble carbon acid sodium aqueous solution 80ml under the room temperature and obtain white emulsion, under the 250W ultrasound condition, mix 20 minutes, with ageing under the emulsion room temperature that obtains 5 hours, filter, washing ,-50 ℃ of freeze drying 3h, pulverizing, to obtain the basic magnesium carbonate presoma and be warmed up to 600 ℃ of lower calcinings 1.5 hours with 5 ℃/min speed, get white nano oxidized magnesium granules, particle diameter 50 nm.
Biocidal property: with above-mentioned nano oxidized magnesium granules and bacteria suspension (10
6CFU/mL) join in the cider, in cider, cell concentration 10
4CFU/mL, nano magnesia granule density are 300ppm.Sample stores 21 days at ambient temperature, and sampling in per 3 days utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.The result shows that room temperature storage 18 days does not detect any bacterium colony, and after 21 days, can detect bacterium colony is 10
1.2CFU/mL.
Embodiment 3
The preparation of nano magnesia: 1.0 mol/L magnesium nitrate aqueous solution 50ml are joined the ultrasonic response container, dripping concentration under the room temperature is that 1.5mol/L soluble carbon acid sodium aqueous solution 40ml obtains white emulsion, under the 250W ultrasound condition, mix 20 minutes, with ageing under the emulsion room temperature that obtains 5 hours, filter, washing ,-50 ℃ of freeze drying 3h, pulverizing, to obtain the basic magnesium carbonate presoma and be warmed up to 800 ℃ with 5 ℃/min speed, calcined 1.5 hours, get white nano oxidized magnesium granules, particle diameter 80 nm.
Biocidal property: with above-mentioned nano oxidized magnesium granules and bacteria suspension (10
6CFU/mL) join in the orange juice, in orange juice, cell concentration 10
4CFU/mL, nano magnesia granule density are 300 ppm.Sample stores 21 days at ambient temperature, and sampling in per 3 days utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.The result shows that room temperature storage 12 days does not detect any bacterium colony.
Embodiment 4
The preparation of nano magnesia: 2.0 mol/L magnesium nitrate aqueous solution 20ml are joined the ultrasonic response container, dripping concentration under the room temperature is that 1.5 mol/L soluble carbon acid sodium aqueous solution 30ml obtain white emulsion, under the 250W ultrasound condition, mix 20 minutes, with ageing under the emulsion room temperature that obtains 5 hours, filter, washing ,-50 ℃ of freeze drying 3h, pulverizing, to obtain the basic magnesium carbonate presoma and be warmed up to 500 ℃ with 5 ℃/min speed, calcined 3 hours, get white nano oxidized magnesium granules, particle diameter 120 nm.
Biocidal property: with above-mentioned nano oxidized magnesium granules and bacteria suspension (10
6CFU/mL) join in the orange juice, in orange juice, cell concentration 10
4CFU/mL, nano magnesia granule density are 400ppm.Sample stores 21 days at ambient temperature, and sampling in per 3 days utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.The result shows that room temperature storage did not detect any bacterium colony after 21 days.
The preparation of nano magnesia: 2.0 mol/L magnesium nitrate solution 20ml are joined the ultrasonic response container, dripping concentration under the room temperature is that 2.0mol/L soluble carbon acid sodium aqueous solution 24ml obtains white emulsion, under the 250W ultrasound condition, mix 20 minutes, with ageing under the emulsion room temperature that obtains 5 hours, filter, washing ,-50 ℃ of freeze drying 3h, pulverizing, to obtain the basic magnesium carbonate presoma and be warmed up to 600 ℃ with 5 ℃/min speed, calcined 5 hours, get white nano oxidized magnesium granules, particle diameter 150 nm.
Biocidal property: with above-mentioned nano oxidized magnesium granules and bacteria suspension (10
6CFU/mL) join in the orange juice, in orange juice, cell concentration 10
4CFU/mL, nano magnesia granule density are 300ppm.Sample stores 21 days at ambient temperature, and sampling in per 3 days utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.The result shows that room temperature storage did not detect any bacterium colony after 6 days.
The nano oxidized magnesium granules of embodiment 1-5 preparation is detected the common microorganism candida tropicalis of beverage (Candida tropicalis) rejection, and concrete steps are as follows:
1) detects bacterial classification
Choose common microorganism in the beverage: candida tropicalis (Candida tropicalis), available from microbial collection center, Sichuan, numbering SCTCC300199.
2) preparation of samples
Bacteria suspension: be the bacteria suspension that sodium chloride-peptone buffer agent of 7.0 is prepared above microbial strains with pH, the thalline final concentration of bacteria suspension is 10
6CFU/mL.
Nano magnesia: with embodiment 1(25nm), embodiment 2(50nm), embodiment 3(80nm), embodiment 4(120nm), embodiment 5(150nm) nano magnesia of preparation is respectively 180 ℃ of activation process 60 minutes of sterilizing, and is for subsequent use.
3) assay method
(1) the nano magnesia particle diameter affects fungistatic effect:
A, cider
Respectively different-grain diameter nano magnesia (5 nm, 15 nm, 25 nm, 50nm, 80nm and 160nm) is joined in the cider (1L dress Huiyuan cider) as experimental group, the bacteria suspension that adds respectively again the candida tropicalis of above-mentioned preparation, the nano magnesia final concentration is 300 ppm, and the bacteria suspension thalline final concentration of candida tropicalis is 10
4CFU/mL.
In addition preservative benzoic acid/sorbierite first (mass ratio 1:1) is added in the cider and organize in contrast, add the bacteria suspension of the candida tropicalis of above-mentioned preparation, bacteria suspension thalline final concentration is 10
4CFU/mL, preservative benzoic acid/sorbierite first (1:1) final concentration is 520 ppm.
Experimental group and control sample are stored 21 days naturally under room temperature (25 ℃) condition, sampling in per 3 days utilizes plate count, measures fungistatic effect, the results are shown in shown in Figure 3.
B, orange juice
Cider among the method a is replaced by orange juice (1L dress Huiyuan orange juice), and other operation and grouping the results are shown in shown in Figure 4 with method a.
By Fig. 3 and 4 as can be known, when the particle diameter of nano oxidized magnesium granules during less than 50nm, nano oxidized magnesium granules has similar antibacterial effect with commercial anticorrisive agent, microorganism in cider or orange juice all less than growth.When the particle diameter of nano oxidized magnesium granules during greater than 50 nm, the bacteriostasis property of nano oxidized magnesium granules reduces along with the increase of particle diameter.Therefore, should choose particle diameter in the actual application less than the nano oxidized magnesium granules of 50 nm.
(2) nano oxidized magnesium density is on the impact of fungistatic effect:
Bacteria suspension: be the bacteria suspension that sodium chloride-peptone buffer agent of 7.0 is prepared above microbial strains with pH, the thalline final concentration of bacteria suspension is 10
4CFU/mL.
Nano magnesia: with embodiment 1(25nm) nano magnesia of preparation is 180 ℃ of sterilization activation process 60 minutes, and is for subsequent use.
A, cider: respectively above-mentioned nano magnesia is joined in the cider (1L dress Huiyuan cider) as experimental group, the bacteria suspension that adds respectively again the candida tropicalis of above-mentioned preparation, the nano magnesia final concentration is respectively 50 ppm, 100 ppm, 200 ppm, 300 ppm, 400 ppm and 500 ppm, and the bacteria suspension thalline final concentration of candida tropicalis is 10
4CFU/mL.
In addition will preservative benzoic acid/sorbierite first (mass ratio 1:1) add in the cider in contrast group, add the bacteria suspension of bacteria suspension of the candida tropicalis of above-mentioned preparation, bacteria suspension thalline final concentration is 10
4CFU/mL, preservative benzoic acid/sorbierite first (1:1) final concentration is 520 ppm.
Experimental group and control sample are stored 21 days naturally under room temperature (25 ℃) condition, sampling in per 3 days utilizes plate count, measures fungistatic effect, the results are shown in shown in Figure 5.
B, orange juice
Cider among the method a is replaced by orange juice (1L dress Huiyuan orange juice), and other operation and grouping the results are shown in shown in Figure 6 with method a.
Fig. 5 and 6 results show that the nano magnesia granule density is lower than 200 ppm in fruit juice, and along with the reduction of nano magnesia granule density in the fruit juice, fungistatic effect becomes worse and worse; The nano magnesia granule density is greater than 200 ppm in fruit juice, and nano oxidized magnesium granules has good fungistatic effect.
That nano oxidized magnesium granules has is nontoxic, common beverage microorganism is had the preferably characteristics such as antibacterial efficient, has as the good potential quality of acidic beverages anticorrisive agent.Its preparation method is easy, can prepare by control presoma calcination condition the magnesium oxide particle of different-grain diameter, is fit to suitability for industrialized production.
Claims (6)
1. a nano magnesia is as the application of antiseptic, it is characterized in that describedly being applied as nano oxidized magnesium granules as the bacteriostatic agent of candida tropicalis (Candida tropicalis).
2. nano magnesia is as the application of antiseptic as claimed in claim 1, and the particle diameter that it is characterized in that described nano oxidized magnesium granules is 4 ~ 150nm.
3. nano magnesia is characterized in that as the application of antiseptic the quality consumption of described nano oxidized magnesium granules is counted 0.02 ~ 0.05 mg/ 10 with Candida tropicalis strain cell number as claimed in claim 1
4CFU.
As claimed in claim 1 nano magnesia as the application of antiseptic, it is characterized in that described nano oxidized magnesium granules prepares as follows: under the room temperature, 1.0 ~ 2.0 mol/L magnesium nitrate aqueous solutions are added drop-wise in 1.0 ~ 2.0mol/L soluble carbon acid sodium aqueous solution, under 150 ~ 250W ultrasound condition, mix 10 ~ 30 minutes, obtain emulsion, with at room temperature ageing of emulsion 3 ~ 5 hours, filter, washing, freeze drying, pulverize, obtain the basic magnesium carbonate presoma, presoma is warming up to 450 ~ 800 ℃ with the speed of 3 ~ 10 ℃/min, calcined 2 ~ 5 hours, and obtained nano oxidized magnesium granules; In the described magnesium nitrate solution in magnesium nitrate and the soluble carbon acid sodium solution the feed intake ratio of amount of substance of solubility carbonic acid sodium be 1:1.0 ~ 1.3.
5. nano magnesia is characterized in that as the application of antiseptic described application is with the bacteriostatic agent of nano oxidized magnesium granules as candida tropicalis in the acidic beverages as claimed in claim 1.
6. nano magnesia is characterized in that as the application of antiseptic described acidic beverages is that the pH value is 2.5 ~ 5.5 as claimed in claim 5.
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| CN113571750A (en) * | 2021-07-14 | 2021-10-29 | 湖北大学 | Wide bandgap semiconductor electrolyte and preparation method thereof, wide bandgap semiconductor electrolyte fuel cell and assembly method thereof |
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