Home Physical Sciences Green synthesis of La2O3–LaPO4 nanocomposites using Charybdis natator for DNA binding, cytotoxic, catalytic, and luminescence applications
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Green synthesis of La2O3–LaPO4 nanocomposites using Charybdis natator for DNA binding, cytotoxic, catalytic, and luminescence applications

  • Rajendran Muthukumar Sivaraman , Kirubaharan Daphne Jacinth Gracia , Seth Sheeba Thavamani EMAIL logo , Thomas Peter Amaladhas ORCID logo EMAIL logo , Sandhanasamy Devanesan and Mohamad Saleh AlSalhi
Published/Copyright: October 1, 2024
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 13 Issue 1

Abstract

A one-step biosynthetic pathway for the fabrication of La2O3–LaPO4 nanocomposites (NCs) was developed, employing Charybdis natator. The structure and phase changes of the NCs were confirmed, and their diverse applications were explored. The peaks at 206, 332, and 442 nm in UV-DRS studies confirmed the formation of La2O3–LaPO4 NCs. Fourier transform infrared spectral analysis revealed La–O stretching at 716 cm−1 and the presence of PO 4 3 − bands at 532, 560, 578, and 618 cm−1. X-ray diffraction patterns showed a hexagonal phase of La2O3 with peaks at 2θ 11.04 and 28.57 and monoclinic LaPO4 phases at 2θ = 18.79 and 41.88. X-ray photoelectron spectroscopy data showed binding energy peaks at 836.04 and 852.77 eV, corresponding to 3d5/2 and 3d3/2 of the lanthanum. The average particle size from HR-TEM analysis was 28.95 nm after annealing at 800°C and SAED patterns confirmed their crystalline nature. The high affinity of the NCs towards ctDNA was established by a binding constant value of 2.08 (mg·mL−1)−1. Under UV exposure, 96% degradation efficiency for methyl orange within 120 min at pH 4 was displayed, with a rate constant of 2.72 × 10−2 min−1 affirming their photocatalytic potential. Their biocompatibility was assessed through MTT assay and luminescence characteristics were evaluated.

Keywords: La2O3–LaPO4 nanocomposites; Charybdis natator ; DNA binding; cytotoxicity; methyl orange degradation

1 Introduction

Nanoparticles (NPs) have ignited a revolution in this new era of technology. The biosynthesis of NPs is a fascinating area of nanotechnology that leverages biological systems to produce and control the synthesis of NPs. Plasmonic NPs, pure and doped metal oxide NPs, and nanocomposites (NCs) are synthesized using plant biometabolites [1,2] from roots, leaves, seeds, and stems [3,4,5]. Microorganisms such as prokaryotic bacteria, fungi, yeast, marine weeds, and plant materials are frequently used as capping and reducing agents in the production of nanomaterials (NMs) through biosynthetic routes [6,7]. Recently, rare earth metal-based NMs have garnered significant scientific interest due to their distinctive physical, chemical, optical, electrical, and luminescence properties. Metals and metal oxides of rare earths are associated with high melting point, high density, and conductivity. Consequently, these materials find applications across various domains [8,9]. Though a wide range of lanthanone metal oxides have been explored, lanthanum oxide (La2O3) gains significance owing to its progressive, engineering, and industrial applications [10]. It possesses distinct features such as negligible toxicity, notable stability, high dielectric constant, p-type semiconductivity, narrow bandwidths, high quantum yields, large Stokes shifts, long-lived emissions, excellent biocompatibility, and a wide band gap [11]. The wide-ranging utilization of NMs based on lanthanum oxide has piqued significant interest across a spectrum of disciplines. These include photocatalysis, gas sensors, supercapacitors, photoelectrochemical cells, Li-ion batteries, magnetic resonance imaging, optical devices, biomedicines, coatings, biosensors, optical bioprobes, biolabeling, and numerous other domains [12,13]. NCs of lanthanum oxide with different metal oxides find applications in electrochemical energy storage and photocatalytic removal of phenol [14,15]. Owing to the quantum confinement effect, NPs find significant implications in nanoelectronics, which benefit enhanced charge carrier mobility due to discrete energy levels, light-emitting diodes (LEDs), lasers [16], photodetectors, solar cells [17], batteries, fuel cells, fluorescence sensing and labelling [18,19,20].

Multiple approaches, including sol–gel, solvothermal, sonochemical, hydrothermal, solution combustion, precipitation methods, and microwave radiation, can be employed for the synthesis of La2O3 NPs [12]. Extracts of Physalis angulata [21], Andrographis paniculata [22], Nothopanax scutellarium [23], Eucalyptus globulus [24], Couroupita guianensis [25], Moringa oleifera [26], Centella asiatica, and Tridax [10] have been used for the biosynthesis of La2O3 NPs. Degradation of methyl orange (MO) [27,28,29] and methylene blue [30] using lanthanum oxide composites have been reported under dark and irradiation. Adsorptive removal of Congo red and phosphate using La2O3 NPs [31,32] and diclofenac using polyacrylamide/gelatin–FeLaO3 NCs [33] has been reported.

Lanthanum phosphate (LaPO4) has gained pronounced demand among other orthophosphates owing to its beneficial photophysical properties, including its high refractive index, photochemical stability, and weak solubility. The 4f–5d and 4f–4f electronic transitions in LaPO4 seem to be more significant because they yield robust narrow emission bands, which in turn produce a distinctive array of colours when incorporated into multi-phosphor devices [34]. Additionally, due to its excellent mechanical resistance and desirable thermal stability, LaPO4 has wide technological applications such as LEDs, illumination, laser, health care, and solar-powered devices [8].

Therapeutic drug discovery primarily relies on the tendency of NMs to bind to DNA. The tiny molecules interact with DNA either through covalent or non-covalent interactions. Electrostatic interactions, groove binding, and van der Waals interactions are the three primary types of non-covalent interactions [35]. By virtue of the interaction/cleavage, NMs gain value, which further enables them to function as vital medicines [36].

The majority of industries, including food, textile, plastics, paper and pulp, and pharmaceutical sectors, create residual effluents that include substantial quantities of organic dyes. Raw industrial effluents significantly disrupt the food chain and are severely mutagenic and carcinogenic to aquatic creatures. MO (C14H14N3NaO3S) is an aromatic anionic hazardous dye that is widely used in the textile industry. It can irritate the skin and eyes and significantly harm the respiratory system. High concentrations of MO dye found in industrial effluents pollute natural water sources directly, affecting aquatic flora and fauna. Catalytic degradation of MO into non-hazardous substances is a crucial action required to address industrial pollution in the present scenario [37,38,39]. This work focusses on the efficient degradation of MO to non-toxic end products with high conversion efficiency [40].

Amidst several treatment procedures, advanced oxidation methods have been added to standard water purification processes, including photo-Fenton, Fenton, sonolysis, ozonolysis, photolysis, and photocatalysis [2]. Each of these methods has its characteristic advantages and disadvantages. Recently, lanthanum-based NMs have been widely used as effective photocatalysts for the degradation of toxic dyes owing to their efficiency [29,30]. Cytotoxicity studies reveal the biocompatible nature of the prepared NCs, which gain an advantage over NCs synthesized over conventional routes.

Charybdis natator, belonging to the Portunidae family and Charybdis genus, is a crab characterized by its brown to orangish colouration and distinctive ridges, particularly known for its swimming abilities. The bioactive components present in C. natator crab are mainly proteins, lipids, carbohydrates, vitamins A and D, and fatty acids [41]. It is rich in essential amino acid content, in which histidine is abundant, and valine is found to be in minimum quantity. The number and sequence of amino acids determine the specificity of a protein [42]. The rich bioactive constituents identified in marine species show antimicrobial, antioxidant, immunomodulatory, and anti-inflammatory activities. Crab is considered one of the seafood delicacies associated with several health benefits owing to the presence of vitamins, proteins, and unsaturated essential fatty acids. Peptides identified in crab species can treat several ailments, including inflammatory bowel disease, migraine, and rheumatoid arthritis. Peptides derived from C. natator can reduce inflammation and substitute potential anti-inflammatory agents [43].

Biosynthesis of NCs of silver and selenium has been reported using Corallina officinalis (red seaweeds) [44]. Marine actinobacterium Micromonospora sp. [45], Sargassum algae [46], and Spatoglossum asperum [47,48] have been used for the biosynthesis of NPs, and their potential applications have been explored. The biosynthesis of metal oxide and metal NPs using plant resources, seaweeds, and algae has been extensively studied, but there has been limited focus on harnessing the potential of edible marine resources [6]. Notably, silver (Ag) and gold (Au) NPs have been successfully synthesized from various marine sources, including sea cucumber (Holothuria scabra) [49], seaweeds [7], algae [50], jellyfish (Nemopilema nomurai) [51], marine invertebrates (polychaetes) [52], and seahorses (Hippocampus spp.) [53]. Selenium NPs (Se NPs) have also been produced from marine oyster (Abalone viscera) [54]. Zinc oxide NPs (ZnO NPs) have been prepared from Penaeus semisulcatus [55] and cerium dioxide NPs (CeO2 NPs) from marine oysters [56]. With an interest in exploring the synthesis of NCs mediated by marine resources, Charybdis natator kindled our interest due to its surplus availability in the coastal areas of Thoothukudi, Tamil Nadu, India, where the work was carried out.

A thorough study of the literature reveals that there is one report on the biosynthesis of CeO2–CePO4 NCs using the leaf extract of Artocarpus heterophyllus [57], and recently we have reported the biosynthesis of CeO2–CePO4 NCs and silver-doped CeO2–CePO4 NCs utilizing an aqueous extract of Penaeus semisulcatus [58]. To the best of our knowledge, this research is the first of its sort to offer a green, rapid, and cost-effective approach for the one-stretch biosynthesis of La2O3–LaPO4 NCs using the aqueous extract of C. natator without the addition of a separate precursor for phosphate ions.

This work focuses on (i) investigating the ability of edible marine crab C. natator for the biosynthesis of La2O3–LaPO4 NCs, (ii) applications of the prepared La2O3–LaPO4 NCs towards degradation of MO dye, (iii) assessing the binding ability of the prepared NCs with ctDNA, and (iv) investigating cytotoxic and luminescence properties of the NCs towards biomedical and photoluminescence applications.

2 Experimental section

2.1 Materials

La(NO3)3·6H2O (99.9%, AR Grade) and Tris HCl (99.0%) were purchased from Sisco Research Laboratories. Type I fibres ctDNA were procured from Sigma Aldrich. The evaluated A 260/A 280 ratio (1.8) confirmed that the ctDNA was highly pure without any impurities. Sodium chloride (Emparta ACS grade, ≥99.0%) was procured from Merck Ltd. MO dye (ACS reagent, dye content of 85.0%) was procured from Sigma Aldrich. pH adjustments were carried out using 0.1 M HCl solution for MO dye degradation studies. All chemicals were utilized as procured.

2.2 Preparation of C. natator extract

From the coast of the Gulf of Mannar, Thoothukudi, Tamil Nadu, India, live C. natators were trapped using a crab net fishing technique. A copious amount of water was used to eliminate the crab carapace and other debris. The protein-rich flesh portion of C. natator was retrieved and rinsed with double distilled water. Finally, 100 mL of double distilled water was added to 30 g of weighed flesh and subjected to heating at 40°C in a water bath for 10 min. The fresh extract thus prepared was used for the synthesis after the supernatant was separated via Whatman No. 41 filter paper.

2.3 Biosynthesis of La2O3–LaPO4 NCs

Lanthanum nitrate hexahydrate (0.433 g) was dissolved in 100 mL of double distilled water (0.01 M). To this lanthanum precursor solution, 100 mL of the freshly prepared C. natator extract (1:1 v/v) was gradually added dropwise while being stirred magnetically, and the mixture was heated to 60°C in a water bath for 1 h. The freshly synthesized white gel was then stirred on a magnetic stirrer for an additional 2 h at 1,500 rpm. The NC was subsequently centrifuged and thoroughly washed with bidistilled water to achieve purity. To derive NCs, the pure NC gel was air-dried (labelled as LaNC@T1), and then LaNC@T1 was finely powdered using mortar and pestle and annealed for 2 h at 800°C (labelled as LaNC@T2) (Scheme 1).

Scheme 1 Schematic illustration of the synthesis of La2O3–LaPO4 NCs.
Scheme 1

Schematic illustration of the synthesis of La2O3–LaPO4 NCs.

2.4 Characterization

Emission characteristics of the prepared NCs were investigated using a JASCO FP-8300 spectrofluorometer. The UV-visible diffuse reflectance spectra (UV-vis DRS) of the synthesized NCs were recorded using a JASCO V-650 model UV-visible spectrophotometer. The crystallinity of the NCs was examined by recording X-ray diffraction (XRD) patterns using an X’Pert Pro-PAnalytic Diffractometer. Fourier transform infrared (FT-IR) spectra of the dried crab extract and NCs were recorded in the 4,000–400 cm−1 range using a Shimadzu 8400S model FT-IR spectrophotometer employing the KBr pellet method. X-ray photoelectron spectroscopy (XPS) was performed using a Thermo-Fisher ESCALAB XI+ instrument, with a monochromatic Al-Kα X-ray source and a constant analyser energy of 26 eV to ascertain the chemical state of each element. The annealed NCs were subjected to high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED) measurements using a JEOL 2100F instrument with an accelerating potential of 200 kV. MO degradation studies were performed using HEBER, HML-LP88 model photoreactor with 8 × 8 W UV lamp intensity and 254 nm wavelength.

2.5 ctDNA binding studies of LaNC@T2

A ctDNA stock solution was prepared by dissolving 10 mg of ctDNA in a buffer solution of 5 mM Tris HCl, which was prepared by dissolving a calculated quantity in 50 mM NaCl. The prepared stock solution of ctDNA was maintained at 4°C and utilized for the experiments. About 10 mg of LaNC@T2 in 30 mL of double-distilled water was subjected to magnetic stirring to facilitate the effective dispersion of the NCs in an aqueous medium. A total of 100 μL of freshly prepared ctDNA solution was mixed and stirred for 1 min at 25°C at different volumes (from 0.2 to 1.8 mL) of dispersed LaNC@T2. The spectral changes in the ctDNA-NC mixture were measured by UV-vis spectral studies [59,60].

2.6 Evaluation of cytotoxicity of LaNC@T2

The biocompatible nature of LaNC@T2 was ascertained by MTT assay in L6 cell lines [61] (S1). The percentage of cell viability of LaNC@T2 was assessed using Eq. 1:

(1) Cell   viability   %   = Average absorbance of the treated cells Average absorbance of the control × 100

2.7 Photocatalytic degradation of MO dye using LaNC@T2

The catalytic capability of LaNC@T2 towards the degradation of MO dye using ultraviolet light (λ = 254 nm) was examined in a photoreactor. To facilitate the study, 50 mL of MO dye of 1 × 10−5 M concentration was magnetically stirred with 10 mg of LaNC@T2 for 30 min under dark conditions at 25°C to attain adsorption equilibrium. Furthermore, the mixture was exposed to UV light in a photoreactor in a long quartz cuvette. From this, 2 mL aliquots were taken out at regular intervals of 10 min and centrifuged at 3,000 rpm. The absorbance of the supernatant dye solution was monitored using a UV-vis spectrophotometer. The optical absorption data of MO at 462 nm were used to determine the concentration of MO dye. The degradation efficiency was calculated using Eq. 2:

(2) Degradation efficiency = C 0 − C C 0 × 100

where C 0 and C are the initial concentration of MO and the concentration after exposure to UV light, respectively.

3 Results and discussion

Protein phosphorylation refers to the addition of a phosphate group to an amino acid residue of a protein, which alters the structural conformation of proteins, thereby modifying their activity by activation or deactivation. Serine, tyrosine, and threonine of the crab extract present in eukaryotes and histidine present in prokaryotes are the most common amino acids that are reported to be in a phosphorylated form [62]. The muscle tissues of crabs have been reported to contain proteins (82.35%), lipids (7.25%), and carbohydrates (5.39%) [41], as well as minerals such as phosphorus (0.29%), potassium (0.38%), sodium (0.29%), magnesium (0.038%), iron (0.035%), calcium (0.12%), and trace amounts of copper and zinc [63]. On the addition of C. natator extract to La(iii) precursor, the protein gets adsorbed to the La2O3 gel formed (Section 2.3). Barton’s reagent was employed to estimate the phosphorus content present in the flesh of marine fishes [62,64]. The phosphate content present in the crab extract plays a key role in stabilizing a part of La(iii) as LaPO4, and hence, nanosize La2O3 formation is accompanied by simultaneous formation of LaPO4 in the NC.

3.1 UV-vis DRS analysis

The C. natator-derived NCs were subjected to UV-vis DRS analysis in the range of 200–900 nm, and the results are shown in Figure 1. LaNC@T1 shows a minor peak at 210 nm, an intense sharp peak at 282 nm, and humps around 340 and 398 nm, and a broad tail extending up to 800 nm. The characteristic signals at 340 and 398 nm correspond to charge-transfer (O2−/La3+) absorption [30]. The highest absorption intensity at 282 nm can be attributed to the presence of tryptophan within the protein structure. Proteins primarily absorb UV light between 180 and 230 nm due to π → π∗ transitions within the peptide bonds. In the range of 230–300 nm, the absorption is mainly influenced by the aromatic side chains of tryptophan (Trp), tyrosine (Tyr), and phenylalanine (Phe) residues [65]. These protein moieties show maximum UV absorption at 280, 275, and 258 nm, respectively, though they exhibit high sensitivity in their optical characteristics to their chemical environment [66]. To substantiate this, the UV-vis spectra of the extract were recorded at different concentrations, and they exhibited peaks at 241 and 279 nm (S2).

Figure 1 UV-DRS spectra of LaNC@T1 and LaNC@T2 NCs. Inset: Tauc’s plot.
Figure 1

UV-DRS spectra of LaNC@T1 and LaNC@T2 NCs. Inset: Tauc’s plot.

LaNC@T2 shows broad peaks at 332 and 442 nm due to charge-transfer (O2−/La3+) absorption [30]. The shift in the absorption wavelength exhibited by the NC after annealing is due to the quantum confinement effect [30]. The peaks at 210 and 206 nm for LaNC@T1 and LaNC@T2, respectively, are due to LaPO4 [67].

The band gap energy was evaluated to be 5.20 and 5.26 eV for LaNC@T1 and LaNC@T2, respectively, using Tauc’s equation, which is in accordance with the literature [68,69]. Owing to the quantum confinement effect, La2O3 NPs exhibit higher band gap and smaller size [68]. Previous studies have shown that due to the higher band gap, La2O3 finds utility in energy storage, electronics, automobiles, catalysis, water treatment, hydrogen production, and CO2 reduction [10]. LaPO4 is reported to possess a band gap of 5.11 eV [70].

3.2 FT-IR spectral analysis

The FT-IR spectra of C. natator extract, LaNC@T1, and LaNC@T2 are depicted in Figure 2. The FT-IR spectrum of the C. natator extract shows a broad band at 3,445 cm−1 due to O–H stretching vibrations of traces of water molecules. The sharp bands located at 1,643 and 1,663 cm−1 are associated with the carbonyl stretching of the amide I group of the protein. The presence of the amide II group is further confirmed by the sharp band identified at 1,514 cm−1. The sharp peaks located at 1,191 and 1,397 cm−1 confirm the presence of the amide III group. The C–H stretching of the aromatic group is confirmed by a signal at 1,454 cm−1 and N–H stretching is observed at 2,939 cm−1. The sharp bands in the range of 897–618 cm−1 are associated with peptide skeletal stretch [71,72,73].

Figure 2 FT-IR spectra of (a) C. natator extract, (b) LaNC@T1, and (c) LaNC@T2.
Figure 2

FT-IR spectra of (a) C. natator extract, (b) LaNC@T1, and (c) LaNC@T2.

In the FT-IR spectrum of LaNC@T1, the broad signal located at 3,569 cm−1 confirms O–H/N–H stretching vibrations, which indicates absorbed moisture on the surface of the NCs [10]. The signal observed at 698 cm−1 is linked with La2O3 stretching [11]. The C–H stretching band is observed at 1,442 cm−1 and the N–H stretching is observed at 2,936 cm−1 [71]. The sharp peaks identified at 536 and 615 cm−1 correspond to the bending vibrations of the O–P–O bonds of the phosphate group. Stretching vibrations associated with the P–O bonds in the phosphate groups are located at 988 and 1,067 cm−1 [67].

In the FT-IR spectrum of LaNC@T2, the signal located at 716 cm−1 corresponds to La–O stretching vibration [26,30]. The bending vibrations associated with O–P–O bonds of the phosphate groups are observed as sharp bands at 532, 560, 578, and 618 cm−1. The sharp bands located at 948, 989, and 1,091 cm−1 also arise from the stretching vibrations of the P–O bond within the phosphate group and are correlated with the monoclinic phase of LaPO4 [74]. The increase in the number of bands in the FT-IR spectra of LaNC@T2 in this region is attributed to the 9-fold coordination of lanthanum atoms in the monoclinic phase of LaPO4. The distortions occurring in the tetrahedral phosphate groups further contribute to the increase in the FT-IR peaks of LaPO4 in the monoclinic phase [67,74–76]. This corroborates with the results from UV-DRS studies, confirming the change in the phase of LaPO4 from hexagonal to monoclinic on annealing at 800°C.

3.3 XRD analysis

XRD patterns of LaNC@T1 and LaNC@T2 delineated in Figure 3 show typical peaks of the La2O3 and LaPO4 phases. The 2θ values of the well-defined diffraction peaks, along with the crystallographic (hkl) planes, are listed in S3.

Figure 3 XRD patterns of (a) LaNC@T1 and (b) LaNC@T2.
Figure 3

XRD patterns of (a) LaNC@T1 and (b) LaNC@T2.

The diffraction patterns show sharp and intense peaks, which reflect the crystallinity and purity of the prepared NCs. In the case of LaNC@T1, characteristic peaks corresponding to La2O3 are located at 2θ values 11.52° and 31.39° contributing to unit cell planes (001) and (003) [29]. This confirms the formation of a hexagonal structure of lanthanum oxide with a P-31m space group (JCPDS 73-2141) [11,13]. Furthermore, the strong signals observed at 19.60° and 41.85° correspond to the (011) and −(103) planes of lanthanum phosphate in the composite.

The XRD pattern of LaNC@T2 confirms the hexagonal phase of La2O3 due to the characteristic peaks at 2θ =11.04, 26.80, 28.57, 30.96, 40.82, 45.69, 51.91, and 69.49°, corresponding to the (001), (100), (011), (003), (102), (110), (103) and (104) planes. Furthermore, the monoclinic lanthanum phosphate present in the NC was confirmed by 2θ signals at 18.79, 21.15, 34.34, 36.63, 41.88 and 48.29° representing the (011), −(111), −(202), (112), −(103), and −(132) planes with P21/n space group (JCPDS 32-0493) [77]. The diffraction patterns of LaNC@T1 and LaNC@T2 match perfectly with hexagonal La2O3 and monoclinic LaPO4 with a very mild shift in 2θ, confirming the formation of NCs. The particle sizes of LaNC@T1 and LaNC@T2 were calculated as 4.36 and 38.63 nm, respectively, using the Debye–Scherrer formula.

3.4 XPS analysis

XPS analysis was performed to examine the chemical states of La, O, and P present on the surface of the NCs. Spectral data were recorded in a survey scan between 0 and 1,000 eV, and deconvolution was performed employing Gaussian–Lorentzian line shapes. Figure 4 represents the deconvoluted 3d XPS spectrum of LaNC@T2. The characteristic signals associated with lanthanum, oxygen, and impurity carbon species are observed in the XPS spectrum, and no other elements are found. Signals corresponding to lanthanum 3d5/2 and 3d3/2 are located at higher binding energies, viz., 836.04 and 852.77 eV, respectively, with a spin–orbit splitting of 16.8 eV. In addition, satellite peaks are observed at 839.34 and 856.11 eV, which correspond to the final state. The broad O 1s signal observed at 531.10 eV is further broadened with enhanced intensity by increasing the annealing temperature owing to lattice oxygen and OH, indicating a hygroscopic state of La2O3 [78]. The P 2p core level spectrum shows a broad signal centred at 133.55 eV (P 2p1/2), which confirms P5+ ions (Figure 4c), indicating the presence of pentavalent phosphorous in LaPO4 [70,79].

Figure 4 XPS of LaNC@T2: (a) survey spectrum and core level spectra of (b) La 3d, (c) P 2p, and (d) O 1s.
Figure 4

XPS of LaNC@T2: (a) survey spectrum and core level spectra of (b) La 3d, (c) P 2p, and (d) O 1s.

3.5 EDX analysis

The EDX spectra of LaNC@T1 and LaNC@T2 are shown in Figure 5, and they feature the signatures of lanthanum, oxygen, and phosphorus. The NCs show a major peak at 4.65 keV, corresponding to lanthanum both for the air-dried and annealed (800°C) samples. Minor peaks located at 0.66, 0.82, 1.03, 5.05, and 5.37 keV also confirm the presence of lanthanum in the NCs. The distinct peak observed at 0.52 keV confirms the presence of oxygen [12]. The prominent peak evident at 2.01 keV further justifies the presence of phosphorus in the NCs [70]. Literature reports hint that phosphorus present in the extract can serve as a precursor for the LaPO4 phase of the NCs, and amino acids present in the extract are identified as the source of phosphate. The presence of 12.7% phosphorus in the LaNC@T2 NC identified by EDX studies substantiates this fact further.

Figure 5 EDX images of (a) LaNC@T1 and (b) LaNC@T2.
Figure 5

EDX images of (a) LaNC@T1 and (b) LaNC@T2.

3.6 HR-TEM analysis

The surface morphology of LaNC@T2 was examined by HR-TEM analysis, and the micrographs are presented in Figure 6. The observation of lattice fringes in the TEM images and ring-like structures observed in the SAED pattern indicates the high crystallinity of the prepared NCs. The particles are spherical in nature, and the average particle size is 26.65 nm. These findings are consistent with the XRD study results.

Figure 6 (a)–(d) HR-TEM images of LaNC@T2 at different magnifications, (e) SAED pattern, and (f) histogram representing particle size distribution.
Figure 6

(a)–(d) HR-TEM images of LaNC@T2 at different magnifications, (e) SAED pattern, and (f) histogram representing particle size distribution.

3.7 Fluorescence study

Room-temperature photoluminescence of LaNC@T2 was recorded in the solid phase. The solid fluorescence spectra of LaNC@T2 at different excitation wavelengths are shown in Figure 7. On varying the excitation wavelength from 210 to 300 nm, maximum emission intensity was observed at an excitation wavelength of 220 nm.

Figure 7 Fluorescence spectra of solid LaNC@T2 (λ ex = 210–300 nm).
Figure 7

Fluorescence spectra of solid LaNC@T2 (λ ex = 210–300 nm).

The emission spectrum of LaNC@T2 (λ ex = 220 nm) shows the most prominent peak at 468 nm and minor peaks at 398, 424, 440, 452, 480, 538, 586, 618, 688, 712, 730, 762, and 842 nm. In successive excitation wavelengths, a similar trend is observed with less intensity emission peaks. Crystalline La2O3 is unable to emit light from the inner atomic 4f shell due to the absence of electrons in the 4f shell of La3+ [30]. Cation vacancy defects are responsible for emission characteristics of the NC, which is observed at 468 nm. Transitions between induced defects of metal oxides, O 2p band, and near band edge account for the violet emission observed between 400 and 430 nm [29]. Singly ionized oxygen vacancies and the emission resulting due to radiative recombination of photogenerated holes combine with electrons in oxygen vacancies, accounting for the luminescence mechanism [68]. Furthermore, the disordered phase of LaPO4 with defects also shows emission at 468 nm. Natarajan et al. have attributed the photoluminescence of LaPO4 to defects in lanthanum interstitials and oxygen vacancies [75].

Excitation of an electron to the conduction band (CB) due to photon irradiation results in the formation of singly ionized oxygen vacancies. The excited electron in the CB on energy loss reoccupies the electron hole in the valence band (VB) through localized defects [67,75]. This mechanism for photoluminescence displayed by LaNC@T2 is depicted in Figure 8.

Figure 8 Mechanism for luminescence of LaNC@T2.
Figure 8

Mechanism for luminescence of LaNC@T2.

4 Applications

4.1 DNA-binding studies of LaNC@T2

Maximum absorbance is observed at 260 nm for blank ctDNA corresponding to π–π* transition, which arises from electronic transitions of chromophores associated with purine and pyrimidine moieties of ctDNA [80]. The concentration of LaNC@T2 was increased while fixing the ctDNA concentration, and the absorbance spectra were recorded and the results are portrayed in Figure 9. A negligible shift of λ max to 259 nm, along with an increase in absorption intensity, is observed with an increase in the concentration of LaNC@T2, which indicates the complex formation of the prepared NCs with ctDNA [81].

Figure 9 Optical spectra of ctDNA at different concentrations of LaNC@T2 (0.2–1.8 mL of 10 mg/30 mL dispersion). Inset: plot of 1/(A–A 0) vs 1/[NCs].
Figure 9

Optical spectra of ctDNA at different concentrations of LaNC@T2 (0.2–1.8 mL of 10 mg/30 mL dispersion). Inset: plot of 1/(A–A 0) vs 1/[NCs].

A linear increase in absorbance is noticed with increasing concentration of the NCs. The Benesi–Hildebrand equation (Eq. 3) was employed to establish the interaction between ctDNA and the NCs. The binding constant is calculated as 2.08 (mg·mL−1)−1, which confirms binding interaction between the prepared NCs and ctDNA [36]:

(3) 1 A obs − A 0 = 1 A C − A 0 + 1 K ( A C − A 0 ) [ NCs ]

4.2 Cytotoxicity studies of LaNC@T2

The cell viability with increasing concentrations of LaNC@T2 was studied, and the results are presented in Figures 10 and 11. A maximum of 99.00% viability is observed with concentrations of 6.25 and 12.5 µg·mL−1. The percentage cell viabilities are found to be 97.52, 97.13, and 96.53% for LaNC@T2 concentrations of 25, 50, and 100 µg·mL−1, respectively, using Eq. 1, as depicted in Figure 10. Cytotoxicity studies clearly indicate that LaNC@T2 derived from marine crabs does not have a significant effect on the L6 cell line, and no discernible toxicity is noticed.

Figure 10 Evaluation of the cytotoxic effect of LaNC@T2 (6.25–100 µg·mL−1).
Figure 10

Evaluation of the cytotoxic effect of LaNC@T2 (6.25–100 µg·mL−1).

Figure 11 Cytotoxic results for LaNC@T2: (a) control, (b)–(f) various concentrations of LaNC@T2 (6.25–100 µg·mL−1) incubated with the L6 cell line.
Figure 11

Cytotoxic results for LaNC@T2: (a) control, (b)–(f) various concentrations of LaNC@T2 (6.25–100 µg·mL−1) incubated with the L6 cell line.

4.3 Photodegradation studies of MO dye using LaNC@T2

Photocatalytic degradation of MO dye by LaNC@T2 NCs using UV light was investigated. MO dye shows maximum absorption at 462 nm, which shows a gradual decrease in absorbance with a shift in λ max from 462 to 454 in 60 min (Figure 12b and c) on exposure to UV irradiation in the presence of the synthesized NCs. The decrease in absorbance with time of irradiation and the variation of ln(C 0/C t) with irradiation time for LaNC@T2 are presented in Figure 12. After optimization studies, maximum degradation of MO (1 × 10−5 M) was observed with 10 mg/50 mL of NCs. The extent of degradation in 60 min was calculated to be 79, 42, and 56% at pH of 4, 7, and 10 (Eq. 2, Figure 12d), respectively. The degradation was almost completely achieved, i.e. up to 96% in 2 h and at a pH of 4 (Figure 12a). The efficiency of degradation is found to be 91.1% by monitoring the total organic carbon (TOC) before and after photocatalytic studies.

Figure 12 Degradation of MO (1 × 10−5 M) using LaNC@T2 (10 mg): (a) pH = 4, (b) pH = 7, (c) pH = 10, and (d) the percentage of degradation at different pH values.
Figure 12

Degradation of MO (1 × 10−5 M) using LaNC@T2 (10 mg): (a) pH = 4, (b) pH = 7, (c) pH = 10, and (d) the percentage of degradation at different pH values.

The plot of ln(C 0/C t) vs irradiation time confirms that photocatalytic degradation of MO dye obeys pseudo-first-order kinetics in accordance with Langmuir–Hinshelwood kinetics (Eq. 4):

(4) ln C = − k t + ln C 0

where C and C 0 are the concentrations of MO before and after degradation, and k represents the first-order rate constant [7]. The apparent rate constants are calculated from the slopes of the plots depicted in Figure 12. The first-order rate constants at pH 4 and 7 (Figure 12b) and 10 (Figure 12c) are calculated to be 2.72 × 10−2 min−1, 8.42 × 10−3 min−1, and 1.28 × 10−2 min−1.

The mechanism of photocatalytic degradation of MO with LaNC@T2 in the presence of UV irradiation is proposed as follows: (a) The NCs absorb radiation and excite electrons from the VB to the CB. (b) Water molecules that are chemisorbed on the surface are ionized to hydroxyl ions (OH–), which further react with holes producing hydroxyl radicals (OḢ). The electrons also facilitate the reduction of oxygen to the superoxide radical (O2̇–). (c) The OḢ radicals produced influence the photocatalytic degradation of MO as a result of oxidation, demethylation, and hydroxylation, which leads to the formation of SO 4 2 – , NO3 –, CO2, and H2O [40,82,83]. The reducing potential of electron–hole recombination primarily influences the photocatalytic activity of LaNC@T2. Intrinsic and extrinsic defects present in the prepared NCs significantly increase the separation time for electron–hole recombination.

The operative mechanism suggested for the degradation of MO by LaNC@T2 is presented in Figure 13. The point of zero charge (PZC) was determined to be 7.35. The NCs exhibited maximum degradation efficiency at a pH of 4, which is well below the PZC, which is in accordance with the literature [84]. In an acidic medium, the NCs exhibit a positive charge (at pH less than ZPC) and show strong electrostatic attraction towards MO, which is an anionic dye [85]. However, at basic pH, a negative charge accumulates on the surface of the NCs, which results in electrostatic repulsion with the anionic dye, which shows a drop in the extent of degradation [86]. The degradation efficiency with the pH of the medium is depicted in Figure 12d.

Figure 13 Mechanism for photodegradation of MO by LaNC@T2 under UV irradiation.
Figure 13

Mechanism for photodegradation of MO by LaNC@T2 under UV irradiation.

Reusability of the NCs towards the degradation of MO was examined by recovering the catalyst by filtration, repeated washing, and air drying. The degradation efficiency was retained up to 86% after five cycles of repetition, indicating the recyclability of the catalyst.

4.4 Commission Internationale de l’Eclairage (CIE) studies of LaNC@T2

The CIE chromaticity coordinates for LaNC@T2 were examined using standard protocols to assess the ability of the prepared NC towards photometric features and phosphor applications. The CIE chromaticity coordinates (X = 0.274, Y = 0.28) of LaNC@T2 at an excitation wavelength of 220 nm confirm that the prepared NCs show strong emission in the vicinity of the blue zone, as shown in Figure 14. Therefore, LaNC@T2 can be suggested in a wide variety of applications, including light sources, phosphors, transistors, efficacious luminescence devices, biomedical labels, solar cells, and as an efficient probe for optics, photonics, electronics, fluorescence labels in fingerprints, and display panels owing to their potential luminescing ability and morphologies [87].

Figure 14 CIE chromaticity diagram of LaNC@T2 at λ ex = 220 nm.
Figure 14

CIE chromaticity diagram of LaNC@T2 at λ ex = 220 nm.

5 Conclusions

This work suggests a green biosynthetic route for the synthesis of La2O3–LaPO4 NCs in a single stretch using edible marine crab C. natator. The oxidation states of lanthanum, oxygen, and phosphorus in the NCs were confirmed by XPS results. The average size of the particles was found to be 28.95 nm for LaNC@T2 by HR-TEM images. XRD and FT-IR analyses of NCs confirm the hexagonal phase of La2O3 and the monoclinic phase of LaPO4. These NCs exhibit a remarkable affinity for ctDNA, demonstrating their potential as a therapeutic agent. Cytotoxicity studies conducted through MTT assay affirm the biocompatibility of NCs. In addition, LaNC@T2 was effectively utilized for the substantial catalytic degradation of MO dye on UV exposure. The luminescence attributes of NCs hold promise for future biosensor applications.

tel: +91 461-2310175; fax: +91 461-2310275

Acknowledgements

The authors acknowledge IIT Bombay, SAIF, for HR-TEM analyses and Nanotechnology Research Centre (NRC), SRMIST, for XPS studies. The authors express their sincere appreciation to the Researchers Supporting Project Number (RSP2024R398) King Saud University, Riyadh, Saudi Arabia.

  1. Author contributions: Rajendran Muthukumar Sivaraman: conceptualization, formal analysis, investigation, methodology, validation, visualization, and writing – original draft; Kirubaharan Daphne Jacinth Gracia: data curation, validation, and writing – review and editing; Seth Sheeba Thavamani: data curation, writing – original draft, and writing – review and editing; Thomas Peter Amaladhas: conceptualization, data curation, formal analysis, investigation, methodology, project administration, supervision, validation, visualization, and writing – review and editing; Sandhanasamy Devanesan: data curation and writing – review & editing; Mohamad Saleh AlSalhi: funding acquisition and writing – review and editing.

  2. Conflict of interest: Authors state no conflict of interest.

  3. Data availability statement: The datasets generated during or analysed during the current study are available from the corresponding author on reasonable request.

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Received: 2024-04-23
Accepted: 2024-08-26
Published Online: 2024-10-01

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  125. Retraction
  126. Retraction of “Biosynthesis and characterization of silver nanoparticles from Cedrela toona leaf extracts: An exploration into their antibacterial, anticancer, and antioxidant potential”
  127. Retraction of “Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)”
  128. Retraction to “Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil”
https://doi.org/10.1515/gps-2024-0092
Keywords for this article
La2O3–LaPO4 nanocomposites; Charybdis natator; DNA binding; cytotoxicity; methyl orange degradation
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Green polymer electrolyte and activated charcoal-based supercapacitor for energy harvesting application: Electrochemical characteristics
  3. Research on the adsorption of Co2+ ions using halloysite clay and the ability to recover them by electrodeposition method
  4. Simultaneous estimation of ibuprofen, caffeine, and paracetamol in commercial products using a green reverse-phase HPTLC method
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  75. Antimicrobial activities and neuroprotective potential for Alzheimer’s disease of pure, Mn, Co, and Al-doped ZnO ultra-small nanoparticles
  76. Green synthesis of silver nanoparticles from Bauhinia variegata and their biological applications
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  78. Eminent Red Sea water hydrogen generation via a Pb(ii)-iodide/poly(1H-pyrrole) nanocomposite photocathode
  79. Green synthesis and effective genistein production by fungal β-glucosidase immobilized on Al2O3 nanocrystals synthesized in Cajanus cajan L. (Millsp.) leaf extracts
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  91. Green synthesis and effective utilization of biogenic Al2O3-nanocoupled fungal lipase in the resolution of active homochiral 2-octanol and its immobilization via aluminium oxide nanoparticles
  92. Eco-friendly RP-HPLC approach for simultaneously estimating the promising combination of pentoxifylline and simvastatin in therapeutic potential for breast cancer: Appraisal of greenness, whiteness, and Box–Behnken design
  93. Use of a humidity adsorbent derived from cockleshell waste in Thai fried fish crackers (Keropok)
  94. One-pot green synthesis, biological evaluation, and in silico study of pyrazole derivatives obtained from chalcones
  95. Bio-sorption of methylene blue and production of biofuel by brown alga Cystoseira sp. collected from Neom region, Kingdom of Saudi Arabia
  96. Synthesis of motexafin gadolinium: A promising radiosensitizer and imaging agent for cancer therapy
  97. The impact of varying sizes of silver nanoparticles on the induction of cellular damage in Klebsiella pneumoniae involving diverse mechanisms
  98. Microwave-assisted green synthesis, characterization, and in vitro antibacterial activity of NiO nanoparticles obtained from lemon peel extract
  99. Rhus microphylla-mediated biosynthesis of copper oxide nanoparticles for enhanced antibacterial and antibiofilm efficacy
  100. Harnessing trichalcogenide–molybdenum(vi) sulfide and molybdenum(vi) oxide within poly(1-amino-2-mercaptobenzene) frameworks as a photocathode for sustainable green hydrogen production from seawater without sacrificial agents
  101. Magnetically recyclable Fe3O4@SiO2 supported phosphonium ionic liquids for efficient and sustainable transformation of CO2 into oxazolidinones
  102. A comparative study of Fagonia arabica fabricated silver sulfide nanoparticles (Ag2S) and silver nanoparticles (AgNPs) with distinct antimicrobial, anticancer, and antioxidant properties
  103. Visible light photocatalytic degradation and biological activities of Aegle marmelos-mediated cerium oxide nanoparticles
  104. Physical intrinsic characteristics of spheroidal particles in coal gasification fine slag
  105. Exploring the effect of tea dust magnetic biochar on agricultural crops grown in polycyclic aromatic hydrocarbon contaminated soil
  106. Crosslinked chitosan-modified ultrafiltration membranes for efficient surface water treatment and enhanced anti-fouling performances
  107. Study on adsorption characteristics of biochars and their modified biochars for removal of organic dyes from aqueous solution
  108. Zein polymer nanocarrier for Ocimum basilicum var. purpurascens extract: Potential biomedical use
  109. Green synthesis, characterization, and in vitro and in vivo biological screening of iron oxide nanoparticles (Fe3O4) generated with hydroalcoholic extract of aerial parts of Euphorbia milii
  110. Novel microwave-based green approach for the synthesis of dual-loaded cyclodextrin nanosponges: Characterization, pharmacodynamics, and pharmacokinetics evaluation
  111. Bi2O3–BiOCl/poly-m-methyl aniline nanocomposite thin film for broad-spectrum light-sensing
  112. Green synthesis and characterization of CuO/ZnO nanocomposite using Musa acuminata leaf extract for cytotoxic studies on colorectal cancer cells (HCC2998)
  113. Review Articles
  114. Materials-based drug delivery approaches: Recent advances and future perspectives
  115. A review of thermal treatment for bamboo and its composites
  116. An overview of the role of nanoherbicides in tackling challenges of weed management in wheat: A novel approach
  117. An updated review on carbon nanomaterials: Types, synthesis, functionalization and applications, degradation and toxicity
  118. Special Issue: Emerging green nanomaterials for sustainable waste management and biomedical applications
  119. Green synthesis of silver nanoparticles using mature-pseudostem extracts of Alpinia nigra and their bioactivities
  120. Special Issue: New insights into nanopythotechnology: current trends and future prospects
  121. Green synthesis of FeO nanoparticles from coffee and its application for antibacterial, antifungal, and anti-oxidation activity
  122. Dye degradation activity of biogenically synthesized Cu/Fe/Ag trimetallic nanoparticles
  123. Special Issue: Composites and green composites
  124. Recent trends and advancements in the utilization of green composites and polymeric nanocarriers for enhancing food quality and sustainable processing
  125. Retraction
  126. Retraction of “Biosynthesis and characterization of silver nanoparticles from Cedrela toona leaf extracts: An exploration into their antibacterial, anticancer, and antioxidant potential”
  127. Retraction of “Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)”
  128. Retraction to “Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil”
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