CN115180654A - Preparation method and application of high-purity iron sulfide nano enzyme - Google Patents

Preparation method and application of high-purity iron sulfide nano enzyme Download PDF

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CN115180654A
CN115180654A CN202210076014.6A CN202210076014A CN115180654A CN 115180654 A CN115180654 A CN 115180654A CN 202210076014 A CN202210076014 A CN 202210076014A CN 115180654 A CN115180654 A CN 115180654A
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iron sulfide
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左兴华
孙国明
张延峰
刘金西
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Beijing Namomei Technology Co ltd
Hebei Jinyihe Biotechnology Co ltd
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Hebei Jinyihe Biotechnology Co ltd
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Abstract

The invention provides a preparation method of high-purity ferric sulfide nano enzyme and application of the high-purity ferric sulfide nano enzyme in preparation of medicines for resisting bacterial, viral or fungal infection. The preparation method of the high-purity ferric sulfide nano enzyme of the invention is to prepare nano ferroferric oxide particles by a solvothermal methodA sulfur source (DADS) was added during (1). High purity Fe prepared by the invention 3 S 4 The method has the advantages of high product purity, simple preparation process, low cost and the like, and has extremely high industrial application value.

Description

Preparation method and application of high-purity iron sulfide nano enzyme
Technical Field
The invention relates to the field of pharmacy, in particular to a preparation method and application of high-purity ferric sulfide nanoenzyme, and also relates to a medicament containing high-efficiency antibacterial ferric sulfide nanoenzyme.
Background
Iron sulfide exhibits enzyme-like activity by mimicking the native enzyme, which relies on the iron-sulfur cluster as a cofactor, thereby expanding its potential for use in biomedicine. The iron sulfide nano material has not been comprehensively researched and applied in the biomedical field. Since S and O are elements of the same group, iron sulfide exhibits similar physicochemical properties to iron oxide and furthermore, phases of iron sulfide in nature include tetrapyrite (FeS), pyrrhotite (Fe) 1−X S), pyrite (FeS) 2 ) Magnetite and pyrite (Fe) 7 S 8 ) And gray iron ore (Fe) 3 S 4 ) Etc. which contain Fe only 2 O 3 And Fe 3 O 4 The iron oxides of (a) show greater variability. Iron sulfide has more proper electron transfer and conductivity, and the iron-based nano material has multiple functions and excellent biocompatibility, so the iron-based nano material is widely applied to the field of biomedicine.
The most reported methods for synthesizing different phases of iron sulfide at present include high-temperature chemical synthesis, ultrasonic method, hydrothermal synthesis method, coprecipitation, biological mineralization, low-temperature synthesis method, microwave method and the like. The hydrothermal synthesis method is most commonly used for synthesizing the iron sulfide, and generally, the hydrothermal method has better dispersity and controllability of products, but iron oxide impurities also appear in the process of synthesizing the iron sulfide. Meanwhile, x-ray diffraction (XRD) analysis of the hydrothermally synthesized samples showed that heterogeneous iron sulfide easily occurred. The chemical coprecipitation does not introduce impurities, the process has mild conditions, and the process is generally synthesized by adopting a method of dissolving iron sulfate heptahydrate and sodium sulfide in ultrapure deionized water, wherein the reaction is N 2 The synthesis conditions required by the coprecipitation method are more severe than those of other methods, and the uniformity of the obtained product is poorer. The main advantages of the microwave-assisted method are short reaction time and small particle size distributionHigh purity, although this emerging technology may be preferable, it should be noted that the aggregation phenomenon does not appear to be improved. Methods for chemically synthesizing iron sulfide using high temperature have been reported, and such synthesis methods are very sensitive to experimental conditions. The biosynthesis of iron sulfide by microorganisms has advantages in biomedical applications, for example, the growth of magnetotactic bacteria sulfate reducing bacteria on an iron-containing substrate produces iron sulfide materials, besides the advantage of green synthesis, the biosynthesis method improves the biocompatibility of iron sulfide, and the produced particles have high catalytic activity and large surface area. In addition, some unusual synthetic chemistry methods such as low temperature synthesis have been reported.
Disadvantages of current iron sulfide production processes include: the preparation process has harsh conditions, the product is aggregated, and the solubility in water is poor. Even though the product has better dispersibility and controllability, the product is often a mixture containing different forms of iron sulfide, and iron oxide impurities can occur in the process of synthesizing the iron sulfide. Preparation of high purity Fe 3 S 4 The method has the difficulties of easy agglomeration, doping and degradation, difficult control and complex operation of shape and grain diameter, poor environmental friendliness, high production cost and the like.
Up to now, various applications of iron sulfide in the biomedical field (catalysts, antibacterial agents, cancer therapy, drug delivery systems, thrombolytic agents, biosensors, antifungal agents, plant seed improving agents, etc.) and their action mechanisms have been reported. The chemical forms of iron in tumors are reported to be ferrous sulfide-like iron and ferritin, and the potential of iron sulfide for treating cancers is highlighted. Fe 3 S 4 The nanosheet is proved to have high efficiency in MRI-guided photothermal and chemokinetic synergistic treatment, and a new direction is opened for designing inorganic iron sulfide for future clinical application. In addition, iron sulfide can be used as a drug carrier, and in previous researches, beta-cyclodextrin (beta-CD) and polyethylene glycol Fe are modified 3 S 4 (GMNCs) were used as drug-loaded NPs. Both beta-CD and PEG were used to control the shape and size of the surfactant GMNCs. Further, fe 3 S 4 Has improved biocompatibility, and can be used for treating chemotherapy drugThe encapsulation efficiency for modified delivery of the mycin was 58.7%. Meanwhile, intensive chemotherapy treatment of mouse tumors was obtained by intravenous injection of doxorubicin (Dox) -loaded GMNCs. The iron sulfide in vitro antifungal shows obvious antifungal activity, and has better effect than the standard bactericide carbendazim. Iron sulfide is effective in bacterial infections and the rapid absorption of iron ions can affect bacterial metabolism. Fe 2+ Is oxidized into Fe 3+ Resulting in the production of Reactive Oxygen Species (ROS) and damage to biomolecules.
Thus, high purity Fe is prepared 3 S 4 Has important significance for later scientific research, especially for developing high-activity antibacterial and antiviral medicaments and the like.
Disclosure of Invention
Through years of research, the inventor finds that the preparation method of the high-purity iron sulfide nanoenzyme comprises the step of synthesizing the iron sulfide nanoenzyme by utilizing an iron source and a sulfur source through a hydrothermal method or a solvothermal method. Wherein the iron source is selected from one or more of ferric chloride, ferric chloride pentahydrate, ferrous sulfate, ferric nitrate and ferric bromide; the sulfur source is selected from one or more of diallyl sulfide, diallyl disulfide (DADS) and diallyl trisulfide compounds in the allicin; the sulfur source is preferably DADS; the iron sulfide is preferably Fe 3 S 4 (ii) a The final concentration of the added iron source is 1-100mg/mL, the final concentration of the added sulfur source is 1-100mg/mL, and the mass ratio of the iron source to the sulfur source is 1.
Specifically, the invention provides high-purity Fe 3 S 4 The preparation method comprises the following steps:
(1) FeCl is added 3 Dissolving in ethylene glycol to obtain a uniform solution;
(2) Adding NaAc.3H 2 O, stirring uniformly, adding DADS, and stirring uniformly;
(3) Transferring the mixture into a high-pressure kettle for reaction at 200 ℃;
(4) Cooling the autoclave, washing and drying the black precipitate to obtain the high-purity Fe 3 S 4 。
Preferably, in step (1), the FeCl 3 In BThe concentration of the diol is 0.01-0.05mg/mL.
Preferably, in step (2), the NaAc.3H 2 The concentration of O in ethylene glycol is 0.5-1.5mg/mL.
Preferably, in step (2), the NaAc.3H 2 The concentration of O in ethylene glycol is 0.5-1.5mg/mL.
Preferably, in step (2), the added DADS is at a concentration of 0.01-0.05mg/mL.
Preferably, in the step (3), the reaction time at 200 ℃ is 10 to 24 hours.
Preferably, wherein said Fe 3 S 4 The thickness of the nano enzyme is 47.92 +/-10.72 nm, and the transverse dimension is 491.10 +/-264.50 nm.
In addition, the invention provides an application of the high-purity iron sulfide nano enzyme in preparation of medicines for resisting bacterial, viral or fungal infection, wherein the medicines are preferably medicines for treating wound healing or vaginitis.
Based on the technical scheme, the invention has the following beneficial effects:
1. high-purity Fe synthesized by the invention 3 S 4 The nano enzyme has the advantages of good dispersibility in water, simple preparation, easy magnetic separation, stable property, good biocompatibility and long antibacterial effect period.
2. High-purity Fe synthesized by the invention 3 S 4 The nano enzyme is harmless to human body in the application range, is environment-friendly, ecological and easy to control, has low price, and is an efficient and low-toxicity antibacterial material.
3. High purity Fe synthesized by the present invention, as compared with the comparative example 3 S 4 The nano enzyme can kill drug-resistant bacteria and intracellular bacteria more efficiently, destroy bacterial cell membranes, promote the generation of bacteria ROS, and improve the content of bacterial lipid oxide to achieve the effects of inhibiting and killing bacteria. The drug resistance experiment shows that the bacteria have no drug resistance to the bacteria after 20 generations of induction, which is superior to other biochemical antibacterial drugs.
Drawings
FIG. 1: high purity Fe prepared in example 1 3 S 4 Sweeping of nanoenzymesScanning electron microscope images;
FIG. 2: high purity Fe prepared in example 1 3 S 4 Transmission electron microscope images of the nanoenzymes;
FIG. 3: high purity Fe prepared in example 1 3 S 4 XRD pattern of nanoenzyme;
FIGS. 4 to 6: fe prepared in comparative examples 1 to 3 3 S 4 Transmission electron microscopy images of MNPS;
FIG. 7: high purity Fe prepared in example 1 3 S 4 Nanoenzyme and Fe prepared in comparative example 1 3 O 4 MNPS, DADS, metronidazole and nano-silver antibacterial activity control experiment results;
FIG. 8: high purity Fe prepared in example 1 and comparative example 1 3 S 4 Nanoenzyme, fe 3 O 4 MNPS results against gardnerella biofilms.
Detailed Description
The specific embodiments of the present invention are provided only to illustrate possible embodiments of the present invention and should not be construed as limiting the present invention in any way. The raw and auxiliary materials, reagents, instruments and equipment and the like related to the embodiment of the invention are all purchased from the market.
Example 1 high purity Fe of the invention 3 S 4 Preparation method of nano enzyme
(1) 0.82g of FeCl 3 Dissolving in 40 mL ethylene glycol, stirring at room temperature for 20 min, and ultrasonic treating for 10 min to ensure FeCl 3 And completely dissolving.
(2) 3.6g NaAc.3H was added 2 And O, stirring for 20 minutes at room temperature, and carrying out ultrasonic treatment for 10 minutes.
(3) 2g of DADS was added and vigorous stirring was continued for 30 minutes.
(4) The mixture was transferred to a 50ml stainless steel autoclave and reacted at 200 ℃ for 12 h, with natural cooling to room temperature.
(5) Washing the black precipitate with water and ethanol alternately for 6 times, and vacuum drying at 60 deg.C for 5 hr to obtain high purity Fe 3 S 4 Scanning electron microscope, transmission electron microscope and XRD are shown in figures 1, 2 and 3 respectively.
Comparative example 1 Fe 3 S 4 Preparation method of nano enzyme
(1) 0.82g of FeCl 3 Dissolving in 40 mL ethylene glycol, stirring at room temperature for 20 min, and ultrasonic treating for 10 min to ensure FeCl 3 And completely dissolving.
(2) 3.6g NaAc.3H was added 2 And O, stirring for 20 minutes at room temperature, and carrying out ultrasonic treatment for 10 minutes.
(3) 0.25g of DADS was added and vigorous stirring was continued for 30 minutes.
(4) The mixture was transferred to a 50ml stainless steel autoclave and reacted at 200 ℃ for 12 h, with natural cooling to room temperature.
(5) Washing black precipitate with water and ethanol for 6 times, and vacuum drying at 60 deg.C for 5 hr to obtain Fe 3 S 4 MNPS, the transmission electron microscope of which is shown in figure 4.
Comparative example 2 Fe 3 S 4 Preparation method of nano enzyme
(1) 0.82g of FeCl 3 Dissolving in 40 mL ethylene glycol, stirring at room temperature for 20 min, and ultrasonic treating for 10 min to ensure FeCl 3 And completely dissolving.
(2) 3.6g NaAc.3H was added 2 And O, stirring for 20 minutes at room temperature, and carrying out ultrasonic treatment for 10 minutes.
(3) 0.5g of DADS was added and vigorous stirring was continued for 30 minutes.
(4) The mixture was transferred to a 50ml stainless steel autoclave and reacted at 200 ℃ for 12 h, with natural cooling to room temperature.
(5) Washing black precipitate with water and ethanol for 6 times, and vacuum drying at 60 deg.C for 5 hr to obtain Fe 3 S 4 MNPS, the transmission electron microscope thereof is shown in figure 5.
Comparative example 3 Fe 3 S 4 Preparation method of nano enzyme
(1) 0.82g of FeCl 3 Dissolving in 40 mL ethylene glycol, stirring at room temperature for 20 min, and ultrasonic treating for 10 min to ensure FeCl 3 And completely dissolving.
(2) 3.6g NaAc.3H was added 2 And O, stirring for 20 minutes at room temperature, and carrying out ultrasonic treatment for 10 minutes.
(3) 1.5g of DADS was added and vigorous stirring was continued for 30 minutes.
(4) The mixture was transferred to a 50ml stainless steel autoclave and reacted at 200 ℃ for 12 h, with natural cooling to room temperature.
(5) Washing black precipitate with water and ethanol for 6 times, and vacuum drying at 60 deg.C for 5 hr to obtain Fe 3 S 4 MNPS, the transmission electron microscope thereof is shown in figure 6.
Experimental example 1 high purity Fe 3 S 4 Control experiment of nano enzyme antibacterial activity
(1) Packet situation
Experimental groups: high purity Fe prepared in example 1 3 S 4 And (3) nano enzyme.
Control group: fe prepared in comparative example 1 3 O 4 MNPS, DADS, metronidazole and nano-silver.
(2) Experimental methods
Taking the sample in logarithmic growth phase (OD) 600 = 0.5) Gardner's bacterium solution containing about 1-2x10 8 CFU/ml. Gardnerella vaginalis was diluted 100-fold in BHIs solutions at approximately 1-2X10 6 CFU/ml, adding drugs with different concentrations into the prepared bacterial suspension, culturing at 37 deg.C and 5% CO2 constant temperature incubator for 24 hr, and measuring OD with microplate reader 600 End-of-point readings to assess bacterial growth. The Minimum Inhibitory Concentration (MIC) is defined as the lowest antibiotic concentration at which growth is significantly reduced or not grown at all.
(3) Results of the experiment
Fe prepared by the invention 3 S 4 The MIC of the nano-enzyme to Gardner's bacteria is as follows: 75.65 μ M; the MIC of nano-silver to Gardnerella is as follows: 86.91 μ M; the MIC of metronidazole to gardnerella is: 109.55 μ M; fe prepared in comparative example 1 3 O 4 And DADS has no inhibitory effect on Gardner bacteria, as shown in FIG. 7.
According to a similar experiment, fe prepared in comparative examples 2 and 3 3 O 4 It also has no inhibiting effect on Gardner bacteria.
Experimental example 2 evaluation of high-purity Fe3S4 anti-Gardnerella biofilm Performance
Gardnerella were cultured in BHIs liquid medium for 12 hours. Then taking the bacterial liquid and diluting the bacterial liquid with BHIs 100 times, further culturing for 8 hours until OD is reached 600 When the nm reached 0.6, the bacteria were diluted 100-fold with 1% glucose in BHIs broth and transferred to 24-well plates. Then placing the circular cell slide into a pore plate of a bacteria culture solution, and keeping the temperature of CO at 37 DEG C 2 When 48H and 24H are cultured in the incubator, the bacterial culture solution is replaced once. The glass plate on which the biofilm had grown was taken out and added to the solution containing Fe of purity prepared in example (1) 3 S 4 The culture solution of BHIs was applied for 3 hours, and then the membrane was washed and fixed with PBS buffer containing 2.5% glutaraldehyde for 12 hours. Then dehydrating with ethanol/water gradient mixed solution, drying at critical point, spraying gold, and observing the growth condition of the biological membrane with a scanning electron microscope. As shown in FIG. 8, fe prepared in comparative example 1 3 S 4 In contrast, the high purity Fe prepared in example 1 3 S 4 The nano enzyme can obviously inhibit the growth of a Gardner bacterium biological membrane.
According to similar experimental results, fe prepared in comparative examples 2 and 3 3 S 4 In contrast, the high purity Fe prepared in example 1 3 S 4 The nano enzyme can also obviously inhibit the growth of the biological membrane of the gardnerella.

Claims (10)

1. A preparation method of high-purity iron sulfide nanoenzyme comprises the step of synthesizing the iron sulfide nanoenzyme by using an iron source and a sulfur source through a hydrothermal method or a solvothermal method.
2. The method according to claim 1, wherein the iron source is selected from one or more of ferric chloride, ferric chloride pentahydrate, ferrous sulfate, ferric nitrate, and ferric bromide.
3. The method according to claim 1, wherein the sulfur source is selected from one or more of diallyl sulfide, diallyl disulfide and diallyl trisulfide in allicin.
4. The preparation method according to claim 1, wherein the final concentration of the iron source is 1-100mg/mL, the final concentration of the sulfur source is 1-100mg/mL, and the mass ratio of the iron source to the sulfur source is 1.
5. The method of claim 1, wherein the iron sulfide nanoenzyme is Fe 3 S 4 And (3) nano enzyme.
6. The method of claim 1 wherein the sulfur source is DADS.
7. The method of claim 1, comprising the steps of:
1) 0.82g of FeCl 3 Dissolving in 40 mL ethylene glycol, stirring at room temperature for 20 min, and subjecting to ultrasonic treatment for 10 min to ensure FeCl 3 Completely dissolving;
2) 3.6g NaAc.3H was added 2 O, stirring for 20 minutes at room temperature, and performing ultrasonic treatment for 10 min;
3) 2g of DADS are added and stirred continuously and vigorously for 30 minutes;
4) Transferring the mixture into a 50ml stainless steel autoclave, reacting at 200 ℃ for 12 h, and naturally cooling to room temperature;
5) Washing black precipitate with water and ethanol for 6 times, and vacuum drying at 60 deg.C for 5 hr to obtain high purity Fe 3 S 4 And (3) nano enzyme.
8. The method of claim 7, wherein the Fe 3 S 4 The thickness of the nano enzyme is 47.92 +/-10.72 nm, and the transverse dimension is 491.10 +/-264.50 nm.
9. Use of the high purity iron sulfide nanoenzyme of any one of claims 1 to 8 in the manufacture of a medicament for the treatment of bacterial, viral or fungal infections.
10. The use according to claim 9, wherein the medicament is a medicament for the treatment of wound healing or vaginitis.
CN202210076014.6A 2022-01-23 2022-01-23 Preparation method and application of high-purity iron sulfide nano enzyme Withdrawn CN115180654A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115152897A (en) * 2022-01-29 2022-10-11 河北金益合生物技术有限公司 Iron sulfide nano enzyme feed additive and preparation method and application thereof

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN109364100A (en) * 2018-08-31 2019-02-22 扬州大学 A kind of nanometer vulcanization iron mixture of high-efficiency antimicrobial and its preparation method and application

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN109364100A (en) * 2018-08-31 2019-02-22 扬州大学 A kind of nanometer vulcanization iron mixture of high-efficiency antimicrobial and its preparation method and application

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LING FANG等: "Metastable Iron Sulfides Gram-Dependently Counteract Resistant Gardnerella Vaginalis for Bacterial Vaginosis Treatment", 《ADVANCED SCIENCE》, vol. 9, pages 1 - 18 *
仇智月: "纳米硫化铁抗菌和清除生物膜的作用与机制研究", 《硕士电子期刊》, no. 02, pages 1 - 74 *
房灵: "硫化铁纳米酶防治细菌性阴道炎效果与机制研究", 《中国博士学位论文全文数据库医药卫生科技辑》, no. 01, pages 23 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115152897A (en) * 2022-01-29 2022-10-11 河北金益合生物技术有限公司 Iron sulfide nano enzyme feed additive and preparation method and application thereof

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