Abstract
The manufacture, modification, and application of surface-functionalized Fe3O4 nanoparticles in the extraction and isolation of antibiotics are reviewed in this paper. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) can be used to characterize the morphological features of Fe3O4 nanoparticles, while Fourier Transform Infrared Spectrometer (FTIR) and X-ray diffractometry (XRD) can be used to determine the crystalline shapes and distinctive functional groups of these particles. We gathered a lot of data to investigate the effects of experimental parameters like pH, adsorbent dosage, contact time, and ionic strength on the extraction of antibiotics from Fe3O4 magnetic nanoparticles. We additionally talked about the mechanism of action of magnetic nanoparticles for the extraction of separated antibiotics and how they are utilized in practical detection methods. This work concluded with an overview of the potential for environmental friendliness and dispersion of functionalized Fe3O4 nanoparticles, as well as potential challenges and directions.
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Introduction
Inorganic nanoparticles exhibiting superparamagnetic characteristics are referred to as magnetic nanoparticles (MNPS). These include metal oxide nanoparticles, rare-earth permanent magnetic nanoparticles, and single-phase metal (such as Fe, Co, and Ni) and their alloy nanoparticles1. Researchers have been focusing a lot of attention on magnetic nanoparticles (MNPs) lately because of their high surface energy, high specific surface area, tiny size effect, and strong magnetic reaction. MNPs can be given appropriate surface properties, less direct contact with cell membranes, and reduced MTT cytotoxicity by adding functional groups like thiols, imidazoles, carboxyl groups, etc. to their surface or coating them with biocompatible materials2. This has a lot of potential for both in vitro and in vivo biomedical applications, including drug delivery3, catalysis4, cell labeling5, and bioseparation6. In addition, iron (Fe) oxide Fe3O4 represents a magnetic nanomaterial which can be particularly useful in a range of fields due to its unique magnetic properties, good biocompatibility, flexibility in preparation methods, easily functionalized surfaces, environmental stability, and reasonable price7.
Antibiotics are a class of secondary metabolites with active antigenic pathogens produced by higher plants and animals, or by microorganisms throughout their daily lives. Based on their chemical structure and mode of action, antibiotics can be classified into the following groups: β-lactam antibiotics, aminoglycosides, macrolides, tetracyclines, and quinolones8. Since antibiotics have a unique ability to prevent and control disease, promote development, and lessen the need for specific nutrients in the culture body, they are widely employed in agricultural production, animal husbandry, aquaculture, and disease prevention9. Monitoring the presence of antibiotic residues in environmental samples is crucial because overuse of antibiotics in recent years has been shown to impair human metabolism, produce toxicity to aquatic organisms, increase bacterial drug resistance, and even lead to the emergence of “superbugs“10. These developments directly endanger human health and the environment. Consequently, it is crucial to effectively monitor the presence of antibiotic residues in environmental samples11,12,13.
Many nations and international organizations have developed pertinent rules and laws, such as prohibiting the use of specific antimicrobial growth promoters and setting maximum residual limits for antibiotics, in order to successfully protect human health and food safety14. The National Standard for Food Safety Maximum Residue Limits of 41 Veterinary Drugs in Food (GB 31650.1–2022) standard, for instance, was released by China in 202215. The Regulation Designating Antimicrobial Agents or Groups of Antimicrobial Agents Reserved for the Treatment of Certain Infections in Humans (EU) 2022/1255 was formally implemented by the European Union on February 9, 2023. This regulation states that the use of antibiotics, antivirals, and an antiprotozoal drug for the treatment of human infections should not be included in veterinary products in order to protect the efficaciousness, availability, and accessibility of antibiotics16.
Currently, common antibiotic detection methods include high performance liquid chromatography-mass spectrometry (HPLC-MS), gas chromatography-mass spectrometry (GC-MS), and other large-scale instrumental methods17, microbiological methods, immunoassay methods18, and biosensor methods19. Both benefits and drawbacks of these approaches exist. For example, Large-scale instrumental methods can detect antibiotics in the environment quantitatively and accurately, but they have drawbacks as well, including costly equipment, labor-intensive and time-consuming pre-treatment procedures, the need for professional technicians, and complex operation20. Microbiological methods have low specificity, poor sensitivity, and long detection times21. Immunoassay can achieve rapid detection, but it has drawbacks, including poor antibody stability and high preparation costs22. Biosensor method has high sensitivity, good selectivity, and high accuracy, but the test results are easily influenced by the environment23. The accuracy of the detection results is significantly influenced by the sample pretreatment step performed before to instrumental analysis24. Fe3O4 magnetic nanomaterials are characterized by large specific surface area, low toxicity and reusability, which can effectively realize the rapid separation and enrichment concentration of the measured substance and the detection probe in the sample matrix, and can be used in the sample pretreatment stage25. As a new form of nanomaterial, Fe3O4 magnetic nanoparticles have significant potential for environmental remediation of various contaminants due to their cost-effectiveness and flexibility when compared to conventional materials, as well as their ability to easily immobilize other adsorbents on their surfaces to boost their activity26.
Fe3O4 magnetic nanoparticles are primarily made using hydrothermal27, sol-gel28, electrochemical29, and chemical co-precipitation30 processes. Of all the synthesis techniques, co-precipitation is currently the most applied28. Features including size, shape, and composition, as well as process variables like pH, reaction temperature, iron salts, and the ionic nature of the medium, all affect the properties of magnetic nanoparticles31. Fe3O4 magnetic nanoparticles themselves, however, have flaws including rapid oxidation and agglomeration, therefore surface modification and functionalization are typically required to lessen inter-particle interactions32. This can help to increase the adsorption performance of the composites and, to some extent, the adsorption efficiency of the targets, in addition to effectively preventing the agglomeration, corrosion, and oxidation of the magnetic nanoparticles33. Organic materials, inorganic nanoparticles, and framework materials are the primary components used in the surface functionalization modification of Fe3O4 magnetic nanoparticles34.
Fe3O4 magnetic nanoparticle modification and applications
Functionalized modification of organic materials
High dispersibility, water solubility, and biocompatibility are characteristics of functionalized nanoparticles created by organic small molecule moiety capping modification. These particles can be categorized into three types based on the type of functional groups: amino-functionalized magnetic nanoparticles35, carboxyl-functionalized magnetic nanoparticles36, and sulfhydryl-functionalized magnetic nanoparticles37. Chitosan38, polyethyleneimine39, polyethylene glycol40, and other copolymers41 are the most common organic polymer-coated modification materials. However, additional materials including glucose42, starch43, and peptides44 are also utilized for modification. Table 1 displays the adsorption properties of iron-based nanomagnetic beads that have had organic components functionalized for a range of antibiotics.
The study conducted by Pratibha et al.45 involved the synthesis of recyclable Fe3O4 functionalized MIL101 (Fe) chitosan composite particles for the purpose of eliminating antibiotics such as tetracycline (TC), doxycycline (DC), and ciprofloxacin (CFX) from aqueous streams. The findings indicated that the removal efficiency of each antibiotic was greater than 99%, and the particles demonstrated significant regeneration over a period of up to five cycles. Selen et al.46 prepared chitosan grafted SiO2/Fe3O4 (Chi-SiO2/Fe3O4) nanoparticles for the adsorption of ciprofloxacin (CPX) from water, and the experimental data showed that the adsorption process was more in line with the nonlinear Langmuir isothermal model, with the maximum theoretical adsorption at 298 K being 100.74 mg/g. Yixuan Wang et al.47 developed Fe3O4@P-AC composites via co-precipitation with fungal bran as the raw material. The results showed that the adsorption of ceftazidime corresponded to the quasi-secondary kinetic model, and the adsorption process was dominated by chemisorption, with Fe3O4@P-AC achieving 94.87% adsorption efficiency. Dopamine can self-polymerize in weak alkaline conditions, forming a layer of securely attached Polydopamine (PDA)on the surface of NPs without pretreatment, making it easy to functionalize with metal nanoparticles48. Tan et al.49 prepared polydopamine-coated graphene oxide/ Fe3O4 (PDA@GO/Fe3O4) imprinted nanoparticles using Sarafloxacin as a template by dopamine self-polymerization (Fig. 1), and the 10–20 nm imprinted PDA film was uniformly covered on the surface of GO/ Fe3O4, Transmission electron microscopy (TEM) allows for the characterization of the material’s morphology (Fig. 2), This magnetic nanoparticle provided selective binding sites, and it could be rapidly and selectively Fluoroquinolone antibiotics in water may be extracted swiftly and selectively using magnetic separation technology, with a removal efficiency of more than 95%. Lin et al.50 prepared a hollow mesoporous magnetic Fe3O4@HMPDA submicron particles with large specific surface area, pore volume and good adsorption performance, and the results showed that the maximum equilibrium adsorption of Adriamycin (DOX) and tetracycline hydrochloride (TCH) on Fe3O4@HMPDA particles were 123.634 mg/g and 150.809 mg/g, respectively, were in accordance with the Langmuir model and quasi-secondary kinetic adsorption, and the removal rates were still above 40% after six times of recycling, which indicated that the particles had good recycling performance.
Schematic diagram of the preparation of PDA@GO/ Fe3O4 nanoparticles49.
TEM images of GO/Fe3O4 (A), PDA@GO/Fe3O4 (B), PDA@GO/Fe3O4 (C), and NPDA@GO/Fe3O4 (D)49.
Functionalized modification of inorganic materials
SiO251,52, inorganic adsorbents such carbon nanotubes53, graphene54, metal oxides like alumina, metallic materials55, and biomaterial like Microalgal biochar56are the primary components used to create composite nanoparticles of inorganic materials. Because SiO2 is non-toxic, harmless, and has good biocompatibility, SiO2 composite magnetic nanoparticles have been studied the most out of all of them. Additionally, the surface of SiO2 contains a large number of unsaturated dangling bonds or silica hydroxyl groups, which makes it easier to coat or graft other functionalized substances for further functionalization modification57. Table 2 displays the adsorption characteristics of iron-based nanomagnetic beads that have had inorganic components functionalized for a range of antibiotics.
Using an in-situ precipitation method, Zhang et al.58 prepared Fe3O4@graphene (Fe3O4@G) magnetic nanocomposites for the removal of hygromycin and tetracycline from aqueous solutions. The results demonstrated that the removal efficiencies of Fe3O4@G in lake water, tap water, and pond water were 95.45%, 96.68%, and 89.82% for oxytetracycline (OTC), and 98.77, 98.23, and 89.09% for tetracycline (TC). The adsorbent and analytes are appropriate for OTC and TC removal due to their π-π interactions and cation-π bonding. The Fe3O4@SiO2@C14mimBF4 magnetic hybrid semi cellular solid-phase extraction system was built by Ye et al.59 and when combined with ultra-high-performance liquid chromatography (UHPLC), it can realize the rapid adsorption of four sulfonamides. The established methods’ limits of detection (LOD) were in the range of 1.21–2.25 µg/L, and the recoveries of the water spiked with the standards were in the range of 70%～100%. Reduction of environmental impact, simplicity, speed, and ease of analyte elution are some of the technical advantages of this approach over conventional solid phase extraction (SPE) techniques. To investigate its adsorption performance and environmental variables for tetracyclines (TCs), Zhang60 and colleagues developed Fe3O4-loaded peanut shell magnetic biochar (Fe3O4/BC). Fe3O4/BC demonstrated good adsorption performance for TCs, with an adsorption rate of over 85%.
Functionalized modification of frame materials
Metal-organic frameworks61 and covalent organic frameworks62 are the primary building blocks for functionalized modified magnetic nanoparticles. Metal-Organic Frameworks (MOFs) are hybrid materials made up of metal ions or metal clusters with organic ligands. They have the ability to adsorption enrichment63, catalytic degradation64, fluorescence65, drug delivery66, and generation of electrochemical signals67. As a result, they have a good chance of being used in the quick detection and removal of drug residue68. Due to their excellent structural regularity, highly ordered pore sizes, intrinsic porosity, large specific surface area, and abundance of reactive functional groups, covalent organic frameworks (COFs) are an emerging class of porous crystalline polymeric materials. However, their limited synthesis methods and difficulty in synthesizing make them difficult to work with69. Table 3 displays the adsorption characteristics of iron-based nanomagnetic beads that have been altered by functionalizing framework materials for a range of antibiotics.
Fe3O4-MOF199 prepared by Li Hanle et al.70 has a large specific surface area (749.19 m2/g), good thermal stability, and a constant ortho-octahedral form. The results of the adsorption experiments showed that the adsorption process was well represented by the Freundlich adsorption kinetic equations and the pseudo-second-order kinetic model. Fe3O4-MOF199 material was used to absorb lincomycin at low concentrations in the waters of Haihe and Jinhe, with a clearance rate of up to 80%. The magnetic metal-organic skeleton Fe3O4@Cu3(BTC)2 was studied and synthesized by Li et al.71 and used as a magnetic solid-phase extraction adsorbent for the enrichment of TCs. This was used in conjunction with tandem mass spectrometry and liquid chromatography to determine four tetracycline drug residues in natural waters, with recoveries ranging from 70.3 to 96.5% and relative standard deviations (RSDs) of 3.8–12.8%. Fe3O4/Zn3(BTC)2 and Fe3O4/Cu3(BTC)2 were synthesized by Yu72 and colleagues in order to study the adsorption performance of the two Magnetic Metal-Organic Frameworks (MMOFs) materials on ciprofloxacin, respectively. With the maximum removal rate of 72.15% and the ability to retain 31.45% after five reuses, Fe3O4/Zn3(BTC)2 proved to have the best adsorption performance of CIP, according to the study’s findings. This suggests that it has good regeneration and reusability. According to these studies, it is possible to enrich water with antibiotics in a straightforward, quick, and highly concentrated manner using magnetic solid-phase extraction based on MMOFs. This will increase the practical use of MMOFs in the pretreatment of samples before environmental pollutant analysis.
Covalent organic frameworks are less frequently used in the pretreatment of antibiotic extraction and isolation than metal-organic frameworks, and their practical use is severely constrained by their drawbacks, which include difficult synthesis, rapid agglomeration, and low recyclability73. Many researchers have tried to create magnetic COF composites (MCOF) in recent years by combining COF with magnetic materials. These composites inherit the benefits of both materials, demonstrating their great potential as adsorbents for the removal of antibiotic contaminants, having a high specific surface area and magnetic separation ability, and being highly reusable74. Presently, Zhang et al.75 created a highly fluorinated porphyrin covalent organic skeleton magnetic adsorbent (FPy-COF@PDA@Fe3O4) by employing covalently bonded three-dimensional porous structure with pyridine groups (-Py) (FPy-COF) as a shell layer for magnetic solid-phase extraction (MSPE)of fluoroquinolones and polydopamine (PDA)-grafted Fe3O4 nanospheres as a magnetic core. For the sensitive quantification of trace levels of six fluoroquinolones (FQs) in milk samples, an MSPE approach in conjunction with high performance liquid chromatography with ultraviolet detector (HPLC-UV) was devised. The six FQs in milk down to 2.3 ng·mL− 1 were detected with good linearity, precision, wide concentration range, and low detection limit (S/N = 3) by the devised MSPE-HPLC technique. The extraction recoveries ranged from 77.8 to 110.4% for various spiked concentrations in milk samples with RSD less than 9.7%. With a more intricate adsorption mechanism and a comparatively greater extraction rate than other materials, this magnetic covalent organic framework is a recently published study with significant research significance.
Mixing modifications
Several researchers have altered the surface functionalization of magnetic nanoparticles using a mixture of three materials-organic materials, inorganic nanoparticles, and framework materials-to improve the performance and extraction efficiency of iron oxides76. Table 4 displays the different antibiotics’ adsorption characteristics for the modified iron-based magnetic nanobeads functionalized with mixed components.
Li77 isolated five fluoroquinolones from water samples using a combination of magnetic solid-phase extraction (MSPE) and ultra performance liquid chromatography (UPLC) with synthesized Fe3O4@Cys@MIL125-NH2 as the adsorbent. The results demonstrated low detection limits (0.05–0.2 µg/L), spiked recoveries of 83.8-109.4%, and RSDs. With an RSD of less than 8.9%, the recoveries ranged from 83.8 to 109.4%. The authors, Ding et al.78 created novel water-stable IL-COOH/Fe3O4@Zr-MOFnanocomposites (Fig. 3) by encapsulating hydrophobic carboxyl-functionalized ionic liquid (IL-COOH) in prepared Fe3O4@Zr-MOFs and introducing polydopamine-functionalized Fe3O4, which showed a maximum adsorption capacity of 438.5 mg/g for ofloxacin. This process involved layer-by-layer modification to build a core-shell structure for controlled growth of Zr-MOFs. Infrared spectroscopy (FTIR) and X-ray diffractometry (XRD) can be used to know the characteristic functional groups and crystal shapes, which can assist in determining whether the synthesis process of the composite material is successful or not (Figs. 4 and 5) .A magnetic metal-organic framework compound-aptamer probe was used by With a detection range of 0.001 to 10 ng/mL and a lowest detection limit of 0.3 ng/mL (S/N = 3), Wu et al.79 created a chloramphenicol bionic colorimetric sensor based on a magnetic metal-organic framework compound-aptamer probe. The spiked recoveries of the actual samples ranged from 86.9 to 93.5% and were unaffected by other antibiotics. Mohammadi et al.80 synthesized P(St-b-AAc) diblock copolymer was conducted with a reversible addition fragmentation transfer (RAFT) method and combined with Fe3O4 to synthesize poly(styrene-block-acrylic acid) diblock copolymer/ Fe3O4 magnetic nanocomposite (abbreviated as P(St-b-AAc)/ Fe3O4)), which showed that the maximum removal of ciprofloxacin was 97%. The maximum removal of ciprofloxacin was 97.5%. Through the use of the co-precipitation method, Danalıoğlu et al.81 created a novel adsorbent Fe3O4/activated carbon/chitosan (MACC: magnetic activated carbon/chitosan) and evaluated its ability to adsorb ciprofloxacin, erythromycin, and amoxicillin. According to theoretical calculations, MACC has an adsorption capacity of 90.10, 178.57, and 526.31 mg/g for three frequently used hazardous antibiotics above, respectively.
Reprinted with permission from78. Copyright (2021) American Chemical Society.
Schematic of the preparation steps of ILs/ Fe3O4@Zr-MOFs.
Reprinted with permission from78. Copyright (2021) American Chemical Society.
FT-IR spectra of OFL and (A) HOOC-IL, (B) NH2-IL, (C) HO-IL and (D) Be-IL.
Reprinted with permission from78. Copyright (2021) American Chemical Society.
(A–C) XRD of Zr-MOFs, Fe3O4@Zr-MOFs and IL-COOH/Fe3O4@Zr-MOFs.
Other magnetic nanoparticles for antibiotic extraction
Other magnetic nanoparticles also have an equally good adsorption capacity for antibiotics, in addition to the widely utilized Fe3O4 magnetic nanoparticles. Table 5 illustrates the different magnetic nanoparticles’ adsorption capabilities for different antibiotics. For instance, functionalized zirconium-based MOF and graphene oxide (GO) were used in the hydrothermal synthesis of new adsorbent UIO-66-(OH)2/GO composite nanoparticles by Sun et al.82. The findings demonstrated that at a solution concentration of 20 mg/L, the adsorption effectiveness of UIO-66-(OH)2/GO on the tetracycline hydrochloride (TC) pollutant reached 94.88%.By using microwave radiation, Poormand et al.83 synthesized CoFe2O4/hexagonal boron nitride (h-BN) nanocomposites that were hybridized with MIL-53 (Al) metal-organic skeleton in a brief amount of time (20–30 min). The antibiotics tetracycline (TC) and ciprofloxacin (CIP) had maximal adsorption capacities of 625.00 mg/g and 270.27 mg/g, respectively, and 100% adsorption rate. According to this recently published study, magnetic composite nanoparticles exhibit greater specific surface area, adsorption capacity, and adsorption efficiency when compared to other conventional materials. This further supports the remarkable potential of magnetic composite nanoparticles for the pre-treatment of antibiotics. The adsorption of tetracycline antibiotics increased with an increase in the magnetite content and degree of cross-linking of the MSPP nanocomplexes, according to Okoli in their84 synthesis of magnetic starch by in situ co-precipitation of Fe2+ and Fe3+ and preparation of magnetic starch polyurethane polymer nanocomposites (MSPP) with 4,4-methylene diphenyl diisocyanate. Ahmed et al.85 used ultrasonication to manufacture polyvinylpyrrolidone (PVP) ternary nanocomposites (PMGO), which were then successfully used as a model drug species for the removal of tetracycline (TC). PMGO is a modified magnetic CuFe2O4-graphene oxide (GO). The maximal adsorption capacity of PMGO, as determined by the Sips model, was 193.8 mg/g, best matching the actual data. Guan et al.86 created ZnFe2O4/CNTs magnetic composites by chemically depositing ferrite nanoparticles onto the surface of multi-walled carbon nanotubes using carbon nanotubes, iron nitrate, and zinc nitrate. Tetracycline hydrochloride was then adsorbed onto the composites, which demonstrated an adsorption capacity of 21.8 mg/g under ideal circumstances and a pollutant removal rate of up to 54.5%. When Bao87 and colleagues wrapped molecular sieve MCM-48 around the surface of CoFe2O4 using a self-assembly technique, they created a novel type of magnetic nanocomposite CoFeM48 with a “core/shell” structure. The composite performed well in the water when it came to the adsorption of five common sulfonamide antibiotics. Both the π-π electron conjugation between the ordered silica structure of the molecular sieve shell and the sulfonamide and the hydrogen bonding force between the functional groups on the surface of CoFeM48 and the sulfonamide explain the good adsorption performance of CoFeM48 on five common sulfonamide antibiotics in water.
Catalytic decomposition of antibiotics by magnetic nanoparticles
Apart from the fact that specific magnetic nanoparticles can catalyze the breakdown of antibiotics, researchers have discovered that magnetic nanoparticles can also be utilized for the extraction and isolation of antibiotics. Decomposition (especially photocatalytic), oxidation, alkylation, C-C coupling, and dehydrogenation reactions are among the catalytic processes of Fe3O4 nanoparticles. In addition to their great stability and excellent catalytic activity, Fe3O4 nanoparticles are environmentally friendly and easily recyclable, which gives them a major edge over other catalysts when it comes to antibiotic elimination88. Table 6 displays certain magnetic nanoparticles’ catalytic capabilities on a range of antibiotics. For instance, Fe3O4/graphene (Fe3O4/GE) nanocomposites were created by Fang et al.89 using the co-precipitation method. This composite was then mixed with Fe (VI), which is the hexavalent oxidation state of iron, to create the Fe (VI)- Fe3O4/GE system, which was studied for its removal of CIP under 98.5% visible light irradiation. As a multiphase persulfate activator for Fenton-like catalytic breakdown of tetracycline, Ahmad et al.90 produced AC@ Fe3O4/PS, which demonstrated 99.8% removal of TC and 93.2% elimination even after five cycles. Using graphene-WO3-Fe3O4 nanocomposites, Guo et al.91 studied the use of composite catalysis generated by pulsed discharge plasma (PDP) for the removal of thiamphenicol (TAP), achieving the maximum removal efficiency and kinetic constant of 99.3% and 0.070 min-1, respectively. Additionally, same study group92 used graphene-TiO2- Fe3O4 nanocomposites in conjunction with non-thermal plasma to catalyze the breakdown of oxytetracycline (OTC) in water. When the doping quantity of Fe3O4 was 20%, the removal rate could reach as high as 98.1%. The elimination effectiveness of OTC was further enhanced by graphene-TiO2 and graphene-TiO2- Fe3O4 nanocomposites as compared to Fe3O4. Using the synergistic effect of catalyst adsorption, oxidized biochar-loaded magnetite particles (OBC- Fe3O4) produced by Zhou et al.93 activated persulfate and accelerated the breakdown of tetracycline (TC), removing 92.3% of TC in 2 h. The GO/CuBDC-Fe3O4 ternary nanocomposite was prepared by Alamgholiloo et al.94 using a green solvent-thermal technique, and it demonstrated the 98.5% degradation of ciprofloxacin (CIP) in 24 min. Based on the use of magnetic biochar/titanium dioxide (BC/TiO2) composites in the photodegradation of oxolinic acid (OXA) and sulfadiazine (SDZ), Silva et al.95. The outcomes demonstrated the potential of BC/TiO2 magnetic nanocomposites as photocatalysts for the elimination of antibiotics from aquaculture effluent. Nodeh et al.96 synthesized strontium titanium trioxide (SrTiO3) nano cubes and used ultrasonic waves to dope them onto graphene oxide (GO)-based magnetic nanoparticles (MNPs). They then showed that the antibiotics could be removed from aqueous media using this newly created GO/MNPs-SrTiO3 nanocomposite. Wang et al.97 created a novel mussel-inspired magnetic cellulose nanocomposite (MCNF/PDA) by immobilizing Fe3O4 nanoparticles on carboxylated cellulose nanofibers (CNFs) coated with PDA using a chemical deposition method (Fig. 6). This demonstrated excellent catalytic degradation of tetracycline (TC), and its TC degradation was not a single superposition of adsorption and Fenton degradation, but rather their synergistic interaction.
Reprinted with permission from97. Copyright (2020) American Chemical Society.
Magnetic cellulose nanocomposites (MCNF/ PDA) with carboxylated cellulose nanofibers (CNF).
Factors impacting antibiotic extraction and separation using Fe3O4 MNPS
The adsorption of antibiotics by magnetic nanoparticles is a complex multistep process involving diffusion and interaction of antibiotic molecules on the surface and inside the adsorbent. Adsorbent dose, pH, contact time, and starting ions are some of the elements that affect this process98,99,100. (For instance, Fig. 7).
Factors influencing the removal of antibiotics by Fe3O4-based adsorbents (By Figdraw).
pH
Adsorption is influenced by the system’s initial pH, which not only establishes the form of the adsorbate but also changes the adsorbent’s surface charge, greatly boosting or suppressing the adsorption effect and, consequently, the strength of the interaction101,102.CoFe2O4@Au nanoparticles were produced by Thi Ngoc Mai Pham103 et al., who discovered that the adsorption at pH 4.0 for the due to CoFe2O4@Au nanoparticles and the antibiotic meropenem were negatively and positively charged at the isoelectric point, respectively, at pH 4.0, the strongest electrostatic interaction was observed, leading to the highest adsorption efficiency of the antibiotic. In their investigation into the extraction and separation of tetracycline by Fe3O4@[Cu3(BTC)2], Li71 et al. discovered that the tetracycline’s ionization, surface charge density, and the adsorption and dissociation of the functional groups’ active sites were all impacted by the pH of the sample solution, which in turn affected the tetracycline’s extraction efficiency. Fe3O4@[Cu3(BTC)2] is more advantageous for the adsorption of TCs in weakly acidic environments because, in such environments, the negatively charged -COO- formed by the deprotonation of -COOH in Fe3O4@[Cu3(BTC)2] facilitates the electrostatic adsorption of positively charged -NH2 in TCs.
Adsorbent dosage
The ratio of adsorbent to adsorbate generally has a major impact on the overall effectiveness of the adsorption process, and the solid-liquid ratio is one of the most important factors influencing the adsorption process104. Puja105 et al. studied the synthesis of a coral-like Co@Co3O4/C nanohybrid and used it to the adsorption of three distinct antibiotic classes (sulfonamides, quinolones, and tetracyclines). When the dosage of the adsorbent was raised (8 mg, 16 mg, 20 mg, 30 mg, 40 mg, 80 mg, and 1 g), the removal of the adsorbent first increased to a maximum value and then quickly declined while maintaining the other parameters. This has to do with how many active sites for saturation adsorption there are. Li70 et al. created a special core-shell titanium-based metal-organic framework (MOF) functionalized magnetic microsphere Fe3O4@Cys@MIL125-NH2 and used it as an adsorbent for enriching five fluoroquinolones in water samples. Increasing the dosage of Fe3O4@Cys@MIL125-NH2 from 5 mg to 25 mg up to 95% resulted in spiked recoveries of the five FQs, which were attributed to the fact that increasing the adsorbent dosage in the aqueous matrix could accelerate the rate at which analytes diffused from the aqueous phase to the solid phase.
Time spent in contact
Adsorption time is a crucial measure of an adsorbent’s effectiveness106. A longer adsorption time can lead to resource loss and excessive energy consumption, while a shorter time to remove a given amount of contaminants indicates greater adsorbent performance. Rapid antibiotic binding to the adsorbent and a high adsorption rate occur during the early stages of adsorption because of the large adsorption driving force, the large pollutant concentration difference between the adsorbent’s surface and the internal and external aqueous environment, and the adsorbent’s abundance of active sites107. Al-Musawi108 et al. used iron oxide magnetic nanoparticles (PAC@ Fe3O4-MN) to magnetize powdered activated carbon and studied the adsorption properties of ciprofloxacin (CIP). The numerous reactive sites on PAC@Fe3O4-MN that are open to CIP molecule adsorption were thought to be the reason for the quick removal of CIP during the first hour of the adsorption process. After a contact time of 60 min, there was no discernible change in CIP adsorption, which may have been caused by CIP molecules obstructing the adsorbent pores’ ability to hold on to pore-active sites. Guo109 et al. investigated the adsorptive removal of fluoroquinolone antibiotics in water by MIL-101(Cr)- so3h, a stable mesoporous metal-organic skeleton. The findings demonstrated that during the first five minutes, the adsorption quantity grew quickly, allowing for the removal of over 90% of the FQ molecules; following the adsorption equilibrium, the final removal rate might exceed 99%. This suggests that after a specific amount of time, the adsorption process will approach equilibrium.
Concentration of ions
Due to the limited number of adsorption sites on the adsorbent surface, the binding of the target adsorbent and adsorption sites may be directly or indirectly inhibited or promoted by metal ions and naturally occurring organic matter in the external aqueous environment110. This will affect the target pollutants’ removal efficiency. Zhang111et al. created a montmorillonite magnetic adsorbent (CoFe2O4/MMT) to recover ciprofloxacin (CIP) and tetracycline (TC) from contaminated water. They also decided to investigate the impact of ionic strength on calcium chloride adsorption. The adsorption trends of TC and CIP were similar, and the adsorption decreased steadily as the CaCl2 concentration increased. This was explained by the fact that Ca2+ ions would compete with antibiotics for the active sites on the adsorbent surface, reducing the adsorbent’s capacity for adsorption. Tang112et al. prepared nitrilotriacetic acid modified magnetic chitosan microspheres (NDMCMs) and used them for the removal of tetracycline antibiotics (TC) from wastewater. Using a NaCl solution, researchers examined the impact of ionic strength on the removal of TC by NDMCMs. They found that an increase in NaCl concentration significantly reduced the adsorption capacity of NDMCMs because TC and Na+ in the liquid competed for the effective active sites on the surface of NDMCMs through extrusion, and nitrilotriacetic acid could form a stable chelate with the metal ions, impeding TC’s adsorption property. Moreover, because NaCl compressed the electric bilayer, an increase in its concentration may further weaken the electrostatic interactions between the adsorbent NDMCMs and the TC, thereby decreasing the TC adsorption.
Antibiotic adsorption mechanism using magnetic nanoparticles
In essence, adsorption is an interaction between the adsorbent and adsorbate interface in the context of mass transfer113. Adsorption mechanisms include hydrogen-bonding, van der Waals, electrostatic, π-π, hydrophobic, and other interactions. These interactions arise from the presence of specific groups on the surface of the adsorbent and the target adsorbate, as well as the appropriateness of the pore channels on the adsorbent surface for the size of the target molecules114,115,116—for instance, Fig. 8. These methods are now utilized to explain why Fe3O4-based adsorbents absorb contaminants in the aqueous environment117,118. It is important to remember that Fe3O4 particles only have magnetic properties on their surface and lack numerous groups, therefore the adsorption mechanisms mentioned above frequently take place between the modifier and the pollutant119.
Adsorption mechanism of antibiotics by Fe3O4 based adsorbent (By Figdraw).
Adsorption kinetic, adsorption isothermal, and adsorption thermodynamic models can all be used to further suit the antibiotic adsorption process by Fe3O4-based adsorbents, as is typically the case in studies120. Adsorption can be classified as either physical or chemical based on the principles involved in the adsorption kinetic model. The Quasi-first-order kinetics proposes that the surface diffusion step controls the adsorbent’s adsorption rate on the target, assuming that there is only one type of binding site on the adsorbent surface. On the other hand, the Quasi-second-order kinetics assumes that the chemical adsorption mechanism controls the adsorption rate and that the adsorbent’s surface has two types of adsorption sites121. Furthermore, two additional phases, including the external diffusion mechanism and the internal diffusion mechanism, can be explored using a biexponential kinetic model, which helps to infer if the reaction mechanism of the target with the adsorbent is a multistep process or not122. The Langmuir isothermal adsorption model in the adsorption isothermal model postulates that the adsorption sites on the adsorbent’s surface are distributed with the same properties, that each site is limited to adsorbing a single target molecule, that there is no lateral interaction or spatial site-barrier between the target molecules, and that the adsorption layer is one molecule thick. Conversely, the Freundlich isothermal adsorption model postulates that the adsorption sites are not evenly distributed across the adsorbent’s surface. Additionally, the adsorption process comprises multilayer adsorption with interactions between adsorbed molecules, and the nature of the adsorption sites varies123. Langmuir–Freundlich isotherm was a three-parameter model describes the heterogeneity factor. Redlich-Peterson explains how to combine the Langmuir and Freundlich models. Toth, on the other hand, is an equation derived from the Langmuir model that predicts non-homogeneous phase adsorption patterns at low and high concentrations122. The parameters of adsorption thermodynamics can be used to ascertain the possibility of spontaneous adsorption as well as the size of the thermodynamic trend that results from it124. Adsorption thermodynamics can also be used to examine the impact of various adsorption systems and conditions, including solvent, adsorbent, and adsorbent, on the adsorption process.
Antibiotics are typically adsorbed by magnetic nanoparticles through a variety of adsorption processes. Ha125and colleagues, for instance, looked into the elimination of ampicillin (AMP) using a new nano-sized Fe3O4/graphene oxide/aminopropyltrimethoxysilane (FGOA) combination. According to the data, the material absorbed AMP at a significantly higher level than materials that had previously been reported. The primary possible reasons for this phenomenon include hydrophilicity, π-π interactions, and electrostatic attraction. π-π interactions can be seen during the adsorption process because π-electrons are present on the FGOA surface and in the AMP molecule, i.e., when both aromatic rings are present. Highly stable magnetic composites Fe3O4@EDTA@UiO-66-NH2 (FEU) with various core-shell structures were synthesized by Bi126 et al., and their adsorption behavior on methotrexate (MTX) was studied. Zeta potential and X-ray photoelectron spectroscopy investigations, along with GCMC simulations, demonstrated that hydrogen bonding and electrostatic interactions were the primary mechanisms for MTX adsorption on FEU. Tetracycline (TC) was successfully removed from neutral aqueous solutions using Fe3O4 nanoparticles that were produced as magnetic adsorbents by Zhai et al.127. According to their findings, the H atoms of the C-O(H) bonds present on the TCB or D rings and the O atoms of Fe3O4 formed hydrogen bonds to facilitate the adsorption between Fe3O4 and TC. Furthermore, the octahedral position forms stronger hydrogen bonds than the tetrahedral site does. With regard to the design and modification of Fe3O4-based nanoparticles for TC removal, this new knowledge offers a valuable guide and point of reference. Wu128and colleagues investigated and created new magnetic molecularly imprinted chitosan/γ-Fe2O3 composites (MICs) and employed them to extract norfloxacin (NOR) from water. This was explained by the presence of memory cavities with specific forms that NOR molecules could readily adsorb on the MICs, where the NOR molecules would then interact with the -OH in the magnetic material to form three intermolecular hydrogen bonds: -OH-F, -OH-O, and -OH-O. The precise identification of the NOR molecules may be ensured by these hydrogen bonds since their lengths and angles are predetermined during the molecular imprinting process (Fig. 9).
Recognition models of (a) NOR, (b) SD, (c) OFL and (d) phenol at specific localization points in the memory cavity, with the ordinal number in the circle for hydrogen bonding, L for linear bonding, and N for nonlinear bonding128.
Magnetic nanomaterial use in detecting
In contrast to conventional separation techniques, magnetic separation methods have the ability to control the magnetic field and separate and enrich the target with high separation efficiency; extraction can be done in centrifuge tubes, preventing the issue of the extraction column becoming clogged due to excessive impurities in the matrix; the use of fewer organic solvents is environmentally friendly and green; the magnetic beads can be reused after treatment; and functional groups on the magnetic nanoparticles can be modified to improve target recognition129. Based on the above advantages, this method has the potential to be applied to rapid detection. Fe3O4 magnetic nanoparticles are currently mostly used in high performance liquid chromatography (HPLC)130, enzyme-linked immunosorbent assay (ELISA)131, immunochromatography132, biosensor method133, etc. These advantages suggest that this method has the potential to be applied to rapid detection. Furthermore, a lot of studies have employed biosensors as supplemental or alternative analytical methods for antibiotic detection in recent years due to their excellent selectivity, quick detection, and in-situ application134.
Presently, antibiotics may be quickly identified thanks in large part to sensor techniques. For instance, Sahebi135et al. employed ultra-performance liquid chromatography-tandem mass spectrometry and functional imidazolium-based ionic liquid-modified magnetic chitosan nanoparticles to investigate a quick and effective method for the simultaneous preconcentration and determination of 22 antibiotics and their metabolites in milk samples. Every antibiotic exhibited strong linearity, as evidenced by correlation values over 0.995. The suggested approach significantly diminished the matrix effect; typical recoveries varied from 85.9 to 107.5%, with RSD values below 9.2%, and limits of detection (LODs) between 0.04 and 0.19 µg/kg. A quantum dot material MNP-SiO2-QD encapsulating magnetic nanoparticles with exceptional fluorescence characteristics and magnetic responsiveness was created by Chen136 et al., and it can detect antibiotics in less than five minutes. Transmission electron microscopy (TEM) can be used to characterize the morphology of the material, while TEM mapping can clearly see the distribution and proportion of each chemical element. (Figs. 10 and 11) In comparison to alternative magnetically encased quantum dots, the material exhibits enhanced fluorescence intensity and robust recovery capabilities, suggesting possible uses in the area of swift detection of antibiotic residues. With the use of magnets, the mixture was extracted from the supernatant to produce the concentration effect, and the SERS could be directly extracted from the supernatant. Yang137 et al. proposed a novel sensor for the detection of chloramphenicol (CAP) based on competitive surface-enhanced Raman scattering (SERS) immunoassay and magnetic separation. This method used antibody-coupled magnetic beads rather than solid substrate as the support material and separation tool. Making the SERS measurement more stable, reproducible, and dependable is the ability to directly extract the SERS signal from the supernatant. Over a broad concentration range of 1–104 pg/mL, the sensor can detect CAP with speed, accuracy, and sensitivity to spare. Jakubec138et al. created a novel, straightforward electrochemical sensor based on magnetite nanostructures stabilized with carboxymethylcellulose (Fe3O4-CMC) and embellished with nano-sized Au nanoparticles (NPs) (Fe3O4-CMC@Au) to detect the antibiotic chloramphenicol (CAP). In this instance, AuNPs serve as electron conduction channels to improve electron transport, and CMC is employed as a stabilizer to stop Fe3O4 from aggregating NPs and overcoming the kinetic barrier. With a 97% recovery rate, the nano sensor created for this study can identify CAP in human urine samples. Liu139et al. successfully used a low-cost, straightforward, and extremely sensitive electrochemical sensor based on a gold electrode modified with carboxyl- Fe3O4 to detect tetracycline in milk. The connector nanoparticles (MNP) in this study were made of chitosan (CS). Anti-tetracycline monoclonal antibody (Ab) was immobilized on the surface of the modified electrodes, and the binding of tetracycline to Ab was examined using differential pulse voltammetry. The MNP was employed as a signal amplifier to improve the immunosensor’s sensitivity. The manufactured immunosensors demonstrated a linear current response to target concentrations ranging from 0.08 to 1 ng/mL under ideal working circumstances, with a lower limit of detection of 0.0321 ng/mL (S/N = 3). He140 et al. created a magnetic nanocomposite-modified screen-printed carbon electrode (SPCE) electrochemical immunosensor that is sensitive and selective for the detection of chloramphenicol (CAP). The graphene sheet (GS)-Nafion (Nf) dispersion solution was first applied to the SPCE. Next, employing an external magnetic field to help absorb the Fe3O4-Au nanoparticles (Gold Mag particles (GMP)) encapsulated bovine serum albumin-CAP (BSA-CAP) coupling onto the SPCE, the CAP content was ascertained using competitive immunoassay mode. The findings demonstrated that, with a detection limit of 0.82 ng/mL (S/N = 3), the rate of rise in DPV current (CI%) was proportionate to the CAP concentration, which ranged from 2.0 ng/mL to 200.0 ng/mL. This immunosensor can be used to detect traces of CAP in actual samples. We anticipate that more researchers will be able to commercialize these sensors in the future despite the growing number of patents and research on magnetic nanoparticle-based antibiotic sensors. However, it is still difficult to mass produce the sensors in an economical and efficient manner without appreciably compromising their sensitivity and stability141.
TEM images of (a) the MNPs, (b) MNP–SiO2, and (c,d) MNP–SiO2–QD136.
TEM mapping of MNP–SiO2–QD: (a) a TEM image of MNP– SiO2–QD; (b) Fe element mapping; (c) O element mapping; (d) Si element mapping; (e) Te element mapping; and (f) Cd element mapping136.
Overview and prospects
Thanks to their superparamagnetism, huge surface area, strong surface charge, and tiny size, iron-based magnetic nanoparticles (MNPs) may remove a wide spectrum of contaminants. This research reviews the synthesis and modification of magnetic nanostructures based on iron and their application in the extraction and separation of antibiotics. At the moment, creating magnetic nanoparticles is a complex process. They are prone to agglomeration, which lowers the system’s energy, because of their highly reactive surface structure. The nanoparticles can be stabilized by adding the proper dispersants to lessen this. Future study must focus on addressing the difficulties posed by the synthesis’s intricacies and the magnetic nanoparticles’ propensity for agglomeration. While Fe3O4 adsorbents built by a single modifier are constrained by a single performance, which cannot meet the high requirements of practical applications, different synthesis and modification methods give iron-based magnetic nanoparticles different physicochemical properties and improve their selective adsorption ability. Composite multilayer modification has gained popularity as a research trend, taking into account the two development directions of antibiotic adsorption specificity and versatility. By carefully combining different modifiers with different properties, multifunctional high-performance magnetic adsorbents can be purposefully constructed. This magnetic nanocomposite has tremendous potential for pretreatment of pollutants because it can combine the properties of magnetic materials and other nanoparticles, has a high adsorption and separation capacity, and can be reused with high economic benefits. Antibiotic abuse is more prevalent now, which will not only affect people’s health but also result in some financial losses. Magnetic nanoparticles are a more effective and convenient way to remove antibiotics than other methods, and they have economic applicability. However, because of process limitations, they cannot be used on a large scale. Future research must focus on finding more affordable and environmentally friendly Fe3O4 adsorbents to extract and separate antibiotics.
Data availability
Data is provided within the manuscript or supplementary information files.
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Acknowledgements
All authors express their gratitude to the Key Laboratory of Microbiological Metrology, Measurement & Bio-product Quality Security, State Administration for Market Regulation, College of Life Science, China Jiliang University, for their invaluable support.
Funding
The work was supported by the National Key Research and Development Program of China (2021YFF0602801, project leader Mingzhou Zhang); the Natural Fund Exploration Project of Zhejiang Province (LTGN23B050001, project leader Xianshu Fu).
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M.S.: Writing-original draft, Data curation, Software, Writing-review & editing; X.F.: Writing-original draft, Writing-review & editing; X.B.: Data curation, Software, Validation; X.Y.: Funding acquisition, Conceptualization, Supervision; Z.Y.: Funding acquisition, Methodology; M.Z.: Funding acquisition. Y.Q.: Methodology. All authors have read and agreed to the published version of the manuscript.
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Sun, M., Bai, X., Fu, X. et al. Modification of Fe3O4 magnetic nanoparticles for antibiotic detection. Sci Rep 15, 4751 (2025). https://doi.org/10.1038/s41598-025-87901-z
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DOI: https://doi.org/10.1038/s41598-025-87901-z
