CN117185456A - Method for removing kanamycin by utilizing abiotic humification - Google Patents
Method for removing kanamycin by utilizing abiotic humification Download PDFInfo
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- CN117185456A CN117185456A CN202311177638.8A CN202311177638A CN117185456A CN 117185456 A CN117185456 A CN 117185456A CN 202311177638 A CN202311177638 A CN 202311177638A CN 117185456 A CN117185456 A CN 117185456A
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- kanamycin
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- tea polyphenol
- remover
- fermentation
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- 229930027917 kanamycin Natural products 0.000 title claims abstract description 56
- 229960000318 kanamycin Drugs 0.000 title claims abstract description 56
- SBUJHOSQTJFQJX-NOAMYHISSA-N kanamycin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CN)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O[C@@H]2[C@@H]([C@@H](N)[C@H](O)[C@@H](CO)O2)O)[C@H](N)C[C@@H]1N SBUJHOSQTJFQJX-NOAMYHISSA-N 0.000 title claims abstract description 56
- 229930182823 kanamycin A Natural products 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000002699 waste material Substances 0.000 claims abstract description 28
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 26
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 26
- 241001122767 Theaceae Species 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000855 fermentation Methods 0.000 claims abstract description 15
- 230000004151 fermentation Effects 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims 1
- 239000010802 sludge Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 241000233866 Fungi Species 0.000 abstract description 4
- 150000001413 amino acids Chemical class 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 235000015097 nutrients Nutrition 0.000 abstract description 2
- 102000004169 proteins and genes Human genes 0.000 abstract description 2
- 108090000623 proteins and genes Proteins 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000001212 derivatisation Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 4
- ZWLUXSQADUDCSB-UHFFFAOYSA-N phthalaldehyde Chemical compound O=CC1=CC=CC=C1C=O ZWLUXSQADUDCSB-UHFFFAOYSA-N 0.000 description 4
- 150000003141 primary amines Chemical group 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 238000009303 advanced oxidation process reaction Methods 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004021 humic acid Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229940054441 o-phthalaldehyde Drugs 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000009283 thermal hydrolysis Methods 0.000 description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229940126574 aminoglycoside antibiotic Drugs 0.000 description 1
- 239000002647 aminoglycoside antibiotic agent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000007344 nucleophilic reaction Methods 0.000 description 1
- 239000010826 pharmaceutical waste Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Abstract
The invention discloses a method for removing kanamycin by utilizing abiotic humification, which belongs to the technical field of antibiotic waste innocent treatment, and comprises the steps of adding a remover and a catalyst into kanamycin waste, and adjusting pH to be alkaline for reaction; the remover comprises tea polyphenol, and the catalyst comprises MnO 2 . The method can achieve the highest removal rate of more than 99.0% for kanamycin in the kanamycin fermentation wastewater and kanamycin fermentation fungus residues, reduces the decomposition of organic matters in the waste treatment process, and is more environment-friendly; more nutrient components such as amino acid, protein and the like in the waste can be reserved in the treatment process, so that the subsequent recycling is facilitated; the tea polyphenol source can be wastewater rich in tea polyphenol, so that waste treatment with waste is expected to be realized; in conclusion, the method has low requirements on operation and equipment and good treatment effect, and is a clean and sustainable kanamycin removal methodIs a novel method of (a).
Description
Technical Field
The invention relates to the technical field of innocent treatment of antibiotic wastes, in particular to a method for removing kanamycin by utilizing abiotic humification.
Background
Kanamycin is a typical aminoglycoside antibiotic and is an important drug for treating serious infection of aerobic gram-negative bacillus. As with other antibiotics, kanamycin is accompanied by contamination during production and use of kanamycin. Especially, the pharmaceutical wastes (including fermentation wastewater and fermentation fungus residues) of kanamycin are directly discharged into the environment without being effectively treated, so that on one hand, kanamycin in the wastes possibly enters the human body through a food chain to influence the health of the human body, and on the other hand, kanamycin in the environment can form selective pressure on environmental microorganisms so as to screen or promote the growth of drug-resistant bacteria, thereby bringing potential safety hazards to human society. Therefore, the treatment of kanamycin in waste is of great importance.
Traditional waste treatment methods include incineration, physical and chemical treatment or microbiological treatment. For organic-resistant wastes, pretreatment is generally adopted to primarily remove antibiotic residues for recycling, including anaerobic digestion or composting, wherein the mainstream pretreatment methods include thermal hydrolysis and advanced oxidation processes, which can effectively remove antibiotics in the wastes, but high equipment, energy input or medicament cost increase the burden of treating the wastes of related enterprises; in addition, during the treatment, other organic matters can be oxidized and decomposed, and the processes are often accompanied with CO 2 Or NO x Thereby causing new environmental problems.
Disclosure of Invention
The invention aims to provide a method for removing kanamycin by utilizing abiotic humification, which solves the problems in the prior art, can efficiently remove kanamycin content in fermentation wastewater and fermentation fungus residues, has low requirements on operation and equipment and good treatment effect, and provides a novel method for removing kanamycin in clean and sustainable waste.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a method for removing kanamycin by utilizing abiotic humification, which comprises the following steps:
adding a remover and a catalyst into kanamycin waste, and adjusting the pH value to be alkaline for reaction;
the remover comprises tea polyphenol, and the catalyst comprises MnO 2 。
Further, the tea polyphenol is used in an amount of 1.5 to 10 times the mass of kanamycin, and the MnO 2 The amount of (B) is 0.01-0.5 times of kanamycin.
Further, the pH is adjusted to be alkaline by using a hydroxide solution of an alkali metal or an alkaline earth metal.
Further, the pH was adjusted to be alkaline with NaOH solution.
Further, the pH is adjusted to 8.5-9.0.
Further, the reaction conditions include: stirring at 25-80deg.C for 1-48 hr.
Further, the stirring speed is 400-800rpm.
Further, the waste includes fermentation wastewater and fermentation residues.
Further, the method further comprises the step of adjusting the water content of the zymophyte residue containing kanamycin to 85-95% before adding the remover and the catalyst.
The invention discloses the following technical effects:
the method is adopted to remove kanamycin, and experimental results show that the highest removal rate of kanamycin in the kanamycin fermentation wastewater and kanamycin fermentation residues can reach more than 99.0%. Compared with the traditional pollutant treatment processes, such as thermal hydrolysis and advanced oxidation processes, the method for removing kanamycin from waste by utilizing abiotic humification reduces the decomposition of organic matters in the process of treating the waste, thus CO 2 The emission of the equal gas is less, and the environment is more friendly; the method can be carried out in a normal temperature environment, so that the heat cost and the like are low; the method has lower technical requirements on the reactor, and more nutrient components in the waste, such as amino acid, protein and the like, can be reserved in the treatment process, so that the method is beneficial to subsequent recycling; in addition, the tea polyphenol source can be wastewater rich in tea polyphenol, so that waste treatment with waste is expected to be realized. In summary, the treatment method has low operation and equipment requirements and good treatment effect, and is a novel method for removing kanamycin from clean and sustainable waste.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The tea polyphenol (CAS number: 84650-60-2) used in the invention is purchased from Shanghai Michlin Biochemical technology Co., ltd, the purity is 99%, and the product number is T821916; catalyst MnO 2 (CAS number 1313-13-9) available from Shanghai Taitan technologies Co., ltd., purity of 99.9%, cat number 014279804; other reagents are all routinely commercially available.
The technical principle of the invention is as follows:
in alkaline environment, polyphenols pass through MnO 2 Can be converted into quinone substances after catalysis. According to the theory of polyphenols formed by humus, primary amine groups of organic substances (e.g., amino acids, etc.) can undergo nucleophilic reaction with quinone substances to form complex macromolecular humic acid substances. In the method for removing kanamycin in waste by using abiotic humification in the following example, kanamycin has 4 primary amine groups, can be used as an ideal primary amine donor in the abiotic humification process, and tea polyphenol is used as a polyphenol donor, and abiotic humification reaction occurs between the two primary amine groups, so that kanamycin finally becomes a part of macromolecular humic acid substances, and further removal of kanamycin in waste is realized. The specific embodiment is as follows:
example 1
Adding tea polyphenol solution into kanamycin standard solution (kanamycin concentration is 1000 mg/L) to make final concentration of tea polyphenol in kanamycin standard solution be 2000mg/L; adding MnO 2 To MnO 2 The final concentration in the wastewater is 100mg/L; adding NaOH solution to adjust the pH of the solution = 9; the mixture was placed on a thermostatic shaker at 25℃and shaken at 180rpm for 24h.
Example 2
The only difference from example 1 is that the system ph=7 and the reaction time is 48h.
Example 3
The difference from example 1 was only that the reaction temperature was 50℃and the reaction time was 3 hours.
Example 4
As in example 1, the only difference is MnO 2 The addition amount is 0, the reaction temperature is 50 ℃, and the reaction time is 3 hours.
Example 5
Adding tea polyphenol solution into kanamycin fermentation wastewater (kanamycin content is 200 mg/L) to make final concentration of tea polyphenol in wastewater be500mg/L; adding MnO 2 To make MnO in the wastewater 2 The final concentration is 100mg/L; adding NaOH solution to ensure that the pH value of the wastewater is=9; the wastewater was placed on a thermostatic shaker at 25℃and shaken at 180rpm for 24h.
Example 6
Adding water into kanamycin fermentation bacteria residues to adjust the water content of a reaction system to 85%, wherein the kanamycin content in the system is 2000mg/kg, and then adding a tea polyphenol solution to enable the final concentration of tea polyphenol in the reaction system to be 20000mg/kg; adding MnO 2 So that MnO in the fungus residue 2 The final dose of (2) is 1000mg/kg; adding NaOH solution so that the final pH of the reaction system was=9; the reaction system was placed on a thermostatic shaker at 25℃and shaken at 180rpm for 48h.
Example 7
The only difference from example 6 is that the final dose of tea polyphenols in the system was 4000mg/kg, the reaction temperature was 80℃and the reaction time was 6 hours.
Example 8
As in example 6, the difference is only MnO in the system 2 The final dosage of (2) is 1000mg/kg, the final concentration of tea polyphenol in the system is 6000mg/kg, the reaction temperature is 80 ℃, and the reaction time is 6h.
Effect verification
Kanamycin was detected by liquid chromatography, briefly as follows: kanamycin was quantified using a Diode Array Detector (DAD) with o-phthalaldehyde (OPA) as derivatizing reagent. The preparation conditions of the derivatization reagent are as follows: 200mg of phthalic dicarboxaldehyde is dissolved in 40mL of methanol, 800 mu L of triethylamine and 200 mu L of 2-mercaptoethanol are added, and the derivatization reagent can be stored for 7 days at the temperature of minus 20 ℃; the derivatization steps are as follows: the filtered sample and 0.5mL of derivatizing reagent were transferred to LC injection vials and thoroughly mixed. Derivatization was performed in a dark environment at 25 ℃ for 15 minutes, and then the derivatized product was injected into the LC system. Notably, the hydrophobicity of the derivative product requires the use of a non-plastic centrifuge tube as the derivative vessel in this study. In addition, OPA derivatives have poor stability and require tight control of derivatization time for each sample prior to sample introduction and analysis; liquid chromatography parameters: quantification of the derived products was performed using a 1200 series high performance liquid chromatography system (Agilent technologies, inc. of Santa Clara, calif., USA). A Zorbax Eclipse XDB C column (150X 4.6mm,5.0 μm) from Agilent technologies, inc. of Santa Clara, calif. was used. The mobile phase was 1% triethylamine solution (ph=8.2-8.5, adjusted with formic acid) as mobile phase a, mobile phase B was methanol, flow rate was 1.5mL/min, gradient composition was 25% a and 75% B, total run time per sample was 10min. The detection wavelength of DAD was 341nm. The test results of kanamycin removal by the method of examples 1 to 8 are shown in Table 1:
TABLE 1
| Kanamycin removal rate (%) | |
| Example 1 | 99.4 |
| Example 2 | 85.3 |
| Example 3 | 99.6 |
| Example 4 | 92.3 |
| Example 5 | 99.4 |
| Example 6 | 98.9 |
| Example 7 | 97.4 |
| Example 8 | 99.2 |
From the data in Table 1, it can be seen that tea polyphenols were used as polyphenol donors and kanamycin was significantly removed from the system by abiotic humification. Example 4 shows that MnO 2 The progress of the reaction can be promoted; examples 1, 2, 3 show that the reaction needs to be carried out under alkaline conditions; example 5 shows that kanamycin can be effectively removed in a wastewater system; example 7 shows that tea polyphenol dose is a critical factor in order to achieve higher kanamycin removal efficiency in real waste; examples 6 and 8 show that there is a higher kanamycin removal rate at 80 c because tea polyphenols or kanamycin can be adsorbed by impurities in the waste, thus reducing the reaction efficiency and facilitating its desorption at higher temperatures. Even so, the removal rate of kanamycin in the bacterial residues can still be realized at 25 DEG C>98％。
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. A method for removing kanamycin by using abiotic humification, which comprises the following steps:
adding a remover and a catalyst into wastes containing kanamycin, and adjusting the pH value to be alkaline for reaction;
the remover comprises tea polyphenol, and the catalyst comprises MnO 2 。
2. The method according to claim 1, characterized in thatCharacterized in that the dosage of the tea polyphenol is 1.5-10 times of the mass of kanamycin, and the MnO 2 The amount of (B) is 0.01-0.5 times of kanamycin.
3. The method according to claim 1, wherein the pH is adjusted to alkaline with an alkali or alkaline earth metal hydroxide solution.
4. A method according to claim 3, characterized in that the pH is adjusted to alkaline with NaOH solution.
5. The method of claim 4, wherein the pH is adjusted to 8.5-9.0.
6. The method of claim 1, wherein the reaction conditions comprise: stirring at 25-80deg.C for 1-48 hr.
7. The method of claim 6, wherein the stirring is at a rate of 400-800rpm.
8. The method of claim 1, wherein the waste comprises fermentation wastewater and fermentation sludge.
9. The method according to claim 8, further comprising the step of adjusting the moisture content of the fermentation residue containing kanamycin to 85-95% before adding the remover and the catalyst.
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