CN103054128B - Application of nanometer magnesium oxide as antimicrobial - Google Patents

Application of nanometer magnesium oxide as antimicrobial Download PDF

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Publication number
CN103054128B
CN103054128B CN201210593140.5A CN201210593140A CN103054128B CN 103054128 B CN103054128 B CN 103054128B CN 201210593140 A CN201210593140 A CN 201210593140A CN 103054128 B CN103054128 B CN 103054128B
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nano oxidized
nano
candida tropicalis
granules
magnesium oxide
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CN103054128A (en
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石陆娥
唐振兴
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Hangzhou Normal University
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Hangzhou Normal University
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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

Nano magnesia is as the application of antiseptic
(1) technical field
The present invention relates to the application of a kind of nano oxidized magnesium granules as bacteriostatic agent, be specifically related to nano oxidized magnesium granules candida tropicalis (Candida tropicalis) is had to 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 commercialization beverage for this reason.Anticorrisive agent is mainly divided into chemical preservative and the large class of natural antiseptic agent two.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 application.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 more and more pay close attention to anticorrisive agent research and application.
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, due to 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 in 2002,18:6679-6686, and particle diameter is in 4nm left and right, and specific surface reaches 1000m 2the nanometer magnesia powder absorption halogen of/g, is adsorbed on bacterium and spore surface with electrostatic force, and cell membrane is destroyed, and 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.Application about it in sour environment does not have relevant report.In addition, magnesium, as the trace element of the necessary daily iron supplement of human body, is highly profitable to health.For this reason, in acidic beverages field, Mgo Nanopowder has the potentiality that become anticorrisive agent very much.
(3) summary of the invention
The object of the invention is to provide a kind of nano oxidized magnesium granules anti-microbial property in acidic beverages, bitter earth nano particle is applied in beverage industry as inorganic antiseptic, is specially the bacteriostatic agent of meter magnesium oxide particle as candida tropicalis (Candida tropicalis).
The technical solution used in the present invention is:
The invention provides the application of a kind of nano magnesia as antiseptic, the described bacteriostatic agent of nano oxidized magnesium granules as candida tropicalis (Candida tropicalis) that be applied as.
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 0.02~0.05mg/10 with Candida tropicalis strain cell number 4cFU.
Further, described nano oxidized magnesium granules is prepared as follows: under room temperature, 1.0~2.0mol/L magnesium nitrate aqueous solution is added drop-wise in 1.0~2.0mol/L soluble carbon acid sodium aqueous solution, under 150~250W ultrasound condition, be uniformly mixed 10~30 minutes, obtain emulsion, by at room temperature ageing of emulsion 3~5 hours, filtration, washing, freeze drying, pulverizing, obtain basic magnesium carbonate presoma, presoma is warming up to 450~800 DEG C with the speed of 3~10 DEG C/min, calcine 2~5 hours, obtain nano oxidized magnesium granules; In described magnesium nitrate solution, in magnesium nitrate and soluble carbon acid sodium solution, the feed intake ratio of amount of substance of solubility carbonic acid sodium is 1:1~1.3.
Further, described application is using the bacteriostatic agent of nano oxidized magnesium granules candida tropicalis in acidic beverages.
Further, described acidic beverages is that pH value is 2.5~5.5.
Nano oxidized magnesium granules of the present invention is taking solubility magnesium salts and soluble carbonate salt as raw material, first make basic magnesium carbonate precursor, prepare by controlling calcination condition, concrete recommendation is carried out as follows: 2.0mol/L magnesium nitrate aqueous solution 50ml is joined to ultrasonic response container, under room temperature, dripping concentration is that 2.0mol/L soluble carbon acid sodium aqueous solution 55ml obtains white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes again, by ageing under the emulsion room temperature obtaining 5 hours, filter, washing, freeze drying, pulverize, obtain basic magnesium carbonate presoma, presoma is warming up to 450~800 DEG C with 3~10 DEG C/min speed, calcine 2~5 hours, can obtain particle diameter is the nano oxidized magnesium granules of white of 4~150nm size.
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 to the features such as good antibacterial efficiency, have as the good potential quality of acidic beverages anticorrisive agent, especially candida tropicalis in acidic beverages is had to obvious fungistatic effect, its preparation method is easy, the magnesium oxide particle that can prepare by controlling presoma calcination condition different-grain diameter, is applicable to suitability for industrialized production.
(4) brief description of the drawings
Nano magnesia transmission electron microscope photo prepared by Fig. 1 embodiment 1;
Nano magnesia X-ray diffractogram prepared by Fig. 2 embodiment 1;
The fungistatic effect of the particle diameter of nano oxidized magnesium granules to candida tropicalis in cider in Fig. 3 embodiment 6;
The fungistatic effect of the particle diameter of nano oxidized magnesium granules to candida tropicalis in orange juice in Fig. 4 embodiment 6;
The fungistatic effect of the concentration of nano oxidized magnesium granules to candida tropicalis in cider in Fig. 5 embodiment 6;
The fungistatic effect of the concentration of nano oxidized magnesium granules to candida tropicalis in orange juice in Fig. 6 embodiment 6.
(5) detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1
The preparation of nano magnesia: 1.0mol/L magnesium nitrate aqueous solution 25ml is joined to (Sonicafier450 in ultrasonic response container, Branson Ultrasonics corporation, the U.S.), the lower 1.0mol/L soluble carbon acid sodium aqueous solution 25ml that drips of room temperature (25 DEG C) obtains white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes, by at room temperature ageing of the emulsion obtaining 5 hours, then filter, after filter cake washing at-50 DEG C of freeze drying 3h, pulverize, obtain basic magnesium carbonate presoma, presoma is warmed up to 450 DEG C with 5 DEG C/min speed, calcine 1.5 hours, obtain white nano oxidized magnesium granules, particle diameter 25nm.Scanning electron microscope (SEM) photograph is shown in Fig. 1, and X-ray diffractogram as shown in Figure 2.
Biocidal property: by above-mentioned nano oxidized magnesium granules and bacteria suspension (10 6cFU/mL) join in cider, in cider, cell concentration 10 4cFU/mL, nano magnesia granule density is 300ppm.Sample stores 21 days at ambient temperature, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.Result shows, room temperature storage, after 21 days, does not detect any bacterium colony.
Embodiment 2
The preparation of nano magnesia: 1.5mol/L magnesium nitrate aqueous solution 50ml is joined to ultrasonic response container, under room temperature, drip 1.0mol/L soluble carbon acid sodium aqueous solution 80ml and obtain white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes, by ageing under the emulsion room temperature obtaining 5 hours, filter, washing ,-50 DEG C of freeze drying 3h, pulverizing, to obtain basic magnesium carbonate presoma is warmed up at 600 DEG C and calcines 1.5 hours with 5 DEG C/min speed, obtain white nano oxidized magnesium granules, particle diameter 50nm.
Biocidal property: by above-mentioned nano oxidized magnesium granules and bacteria suspension (10 6cFU/mL) join in cider, in cider, cell concentration 10 4cFU/mL, nano magnesia granule density is 300ppm.Sample stores 21 days at ambient temperature, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.Result shows, room temperature storage 18 days, does not detect any bacterium colony, after 21 days, can detect that bacterium colony is 10 1.2cFU/mL.
Embodiment 3
The preparation of nano magnesia: 1.0mol/L magnesium nitrate aqueous solution 50ml is joined to ultrasonic response container, under room temperature, dripping concentration is that 1.5mol/L soluble carbon acid sodium aqueous solution 40ml obtains white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes, by ageing under the emulsion room temperature obtaining 5 hours, filter, washing ,-50 DEG C of freeze drying 3h, pulverizing, to obtain basic magnesium carbonate presoma and be warmed up to 800 DEG C with 5 DEG C/min speed, calcine 1.5 hours, obtain white nano oxidized magnesium granules, particle diameter 80nm.
Biocidal property: by above-mentioned nano oxidized magnesium granules and bacteria suspension (10 6cFU/mL) join in orange juice, in orange juice, cell concentration 10 4cFU/mL, nano magnesia granule density is 300ppm.Sample stores 21 days at ambient temperature, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.Result shows, room temperature storage 12 days, does not detect any bacterium colony.
Embodiment 4
The preparation of nano magnesia: 2.0mol/L magnesium nitrate aqueous solution 20ml is joined to ultrasonic response container, under room temperature, dripping concentration is that 1.5mol/L soluble carbon acid sodium aqueous solution 30ml obtains white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes, by ageing under the emulsion room temperature obtaining 5 hours, filter, washing ,-50 DEG C of freeze drying 3h, pulverizing, to obtain basic magnesium carbonate presoma and be warmed up to 500 DEG C with 5 DEG C/min speed, calcine 3 hours, obtain white nano oxidized magnesium granules, particle diameter 120nm.
Biocidal property: by above-mentioned nano oxidized magnesium granules and bacteria suspension (10 6cFU/mL) join in orange juice, in orange juice, cell concentration 10 4cFU/mL, nano magnesia granule density is 400ppm.Sample stores 21 days at ambient temperature, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.Result shows, room temperature storage, after 21 days, does not detect any bacterium colony.
Embodiment 5
The preparation of nano magnesia: 2.0mol/L magnesium nitrate solution 20ml is joined to ultrasonic response container, under room temperature, dripping concentration is that 2.0mol/L soluble carbon acid sodium aqueous solution 24ml obtains white emulsion, under 250W ultrasound condition, be uniformly mixed 20 minutes, by ageing under the emulsion room temperature obtaining 5 hours, filter, washing ,-50 DEG C of freeze drying 3h, pulverizing, to obtain basic magnesium carbonate presoma and be warmed up to 600 DEG C with 5 DEG C/min speed, calcine 5 hours, obtain white nano oxidized magnesium granules, particle diameter 150nm.
Biocidal property: by above-mentioned nano oxidized magnesium granules and bacteria suspension (10 6cFU/mL) join in orange juice, in orange juice, cell concentration 10 4cFU/mL, nano magnesia granule density is 300ppm.Sample stores 21 days at ambient temperature, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, and experimental implementation and solution preparation are with embodiment 6.Result shows, room temperature storage, after 6 days, does not detect any bacterium colony.
Embodiment 6
Nano oxidized magnesium granules prepared by embodiment 1-5 detects the common microorganism candida tropicalis of beverage (Candida tropicalis) rejection, and concrete steps are as follows:
1) detect bacterial classification
Choose common microorganism in beverage: candida tropicalis (Candida tropicalis), purchased from microbial collection center, Sichuan, numbering SCTCC300199.
2) preparation of samples
Bacteria suspension: prepare the bacteria suspension of above microbial strains with sodium chloride-peptone buffer agent that pH is 7.0, the thalline final concentration of bacteria suspension is 10 6cFU/mL.
Nano magnesia: nano magnesia prepared by embodiment 1 (25nm), embodiment 2 (50nm), embodiment 3 (80nm), embodiment 4 (120nm), embodiment 5 (150nm) carries out sterilizing activation processing 60 minutes at 180 DEG C respectively, for subsequent use.
3) assay method
(1) nano magnesia particle diameter affects fungistatic effect:
A, cider
Respectively different-grain diameter nano magnesia (5nm, 15nm, 25nm, 50nm, 80nm and 160nm) is joined in cider (1L dress Huiyuan cider) as experimental group, add respectively again the bacteria suspension of the candida tropicalis of above-mentioned preparation, nano magnesia final concentration is 300ppm, and the bacteria suspension thalline final concentration of candida tropicalis is 10 4cFU/mL.
In addition preservative benzoic acid/potassium sorbate (mass ratio 1:1) is added in cider as a control group, add the bacteria suspension of the candida tropicalis of above-mentioned preparation, bacteria suspension thalline final concentration is 10 4cFU/mL, preservative benzoic acid/potassium sorbate (1:1) final concentration is 520ppm.
Experimental group and control sample are naturally stored to 21 days under room temperature (25 DEG C) condition, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, the results are shown in Figure shown in 3.
B, orange juice
Cider in method a is replaced by orange juice (1L dress Huiyuan orange juice), and other operation and grouping, with method a, the results are shown in Figure shown in 4.
From Fig. 3 and 4, in the time that the particle diameter of nano oxidized magnesium granules is less than 50nm, nano oxidized magnesium granules has similar antibacterial effect with commercial anticorrisive agent, and microorganism does not all grow in cider or orange juice.In the time that the particle diameter of nano oxidized magnesium granules is greater than 50nm, the bacteriostasis property of nano oxidized magnesium granules reduces along with the increase of particle diameter.Therefore, in actual application, should choose the nano oxidized magnesium granules that particle diameter is less than 50nm.
(2) impact of nano oxidized magnesium density on fungistatic effect:
Bacteria suspension: prepare the bacteria suspension of above microbial strains with sodium chloride-peptone buffer agent that pH is 7.0, the thalline final concentration of bacteria suspension is 10 4cFU/mL.
Nano magnesia: nano magnesia prepared by embodiment 1 (25nm) was 180 DEG C of sterilizing activation processing 60 minutes, for subsequent use.
A, cider: respectively above-mentioned nano magnesia is joined in cider (1L dress Huiyuan cider) as experimental group, add respectively again the bacteria suspension of the candida tropicalis of above-mentioned preparation, nano magnesia final concentration is respectively 50ppm, 100ppm, 200ppm, 300ppm, 400ppm and 500ppm, and the bacteria suspension thalline final concentration of candida tropicalis is 10 4cFU/mL.
In addition preservative benzoic acid/potassium sorbate (mass ratio 1:1) is added in cider as a control group, add the bacteria suspension of the bacteria suspension of the candida tropicalis of above-mentioned preparation, bacteria suspension thalline final concentration is 10 4cFU/mL, preservative benzoic acid/potassium sorbate (1:1) final concentration is 520ppm.
Experimental group and control sample are naturally stored to 21 days under room temperature (25 DEG C) condition, and sampling in every 3 days, utilizes plate count, measures fungistatic effect, the results are shown in Figure shown in 5.
B, orange juice
Cider in method a is replaced by orange juice (1L dress Huiyuan orange juice), and other operation and grouping, with method a, the results are shown in Figure shown in 6.
Fig. 5 and 6 results show, when nano magnesia granule density in fruit juice is lower than 200ppm, along with the reduction of nano magnesia granule density in fruit juice, fungistatic effect becomes worse and worse; When nano magnesia granule density in fruit juice is greater than 200ppm, nano oxidized magnesium granules has good fungistatic effect.
That nano oxidized magnesium granules has is nontoxic, common beverage microorganism is had to the features such as good antibacterial efficiency, has as the good potential quality of acidic beverages anticorrisive agent.Its preparation method is easy, can prepare by controlling presoma calcination condition the magnesium oxide particle of different-grain diameter, is applicable to suitability for industrialized production.

Claims (2)

1. a nano magnesia is as the application of antiseptic, it is characterized in that the described bacteriostatic agent of nano oxidized magnesium granules as candida tropicalis in acidic beverages (Candida tropicalis) that be applied as, the quality consumption of described nano oxidized magnesium granules is counted 0.02~0.05mg/10 with Candida tropicalis strain cell number 4cFU, the particle diameter of described nano oxidized magnesium granules is 4~150nm; The pH value of described acidic beverages is 2.5~5.5.
As claimed in claim 1 nano magnesia as the application of antiseptic, it is characterized in that described nano oxidized magnesium granules prepared as follows: under room temperature, 1.0~2.0mol/L magnesium nitrate aqueous solution is added drop-wise in 1.0~2.0mol/L soluble carbon acid sodium aqueous solution, under 150~250W ultrasound condition, be uniformly mixed 10~30 minutes, obtain emulsion, by at room temperature ageing of emulsion 3~5 hours, filter, washing, freeze drying, pulverize, obtain basic magnesium carbonate presoma, presoma is warming up to 450~800 DEG C with the speed of 3~10 DEG C/min, calcine 2~5 hours, obtain nano oxidized magnesium granules, in described magnesium nitrate solution, in magnesium nitrate and soluble carbon acid sodium solution, the feed intake ratio of amount of substance of solubility carbonic acid sodium is 1:1.0~1.3.
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