<p>In this study, a green synthesis methodology to synthesize molybdenum disulfide (MoS<sub>2</sub>) nanostructures using plant extracts as biogenic reducing and stabilizing agents. Eruca sativa (arugula) and <i>Corchorus olitorius</i> (jute mallow) aqueous extracts were used as natural reducing agents whereas the garlic extract was used as a complementary source of bio-sulfur and thioacetamide under mild reflux conditions. To clarify the mechanistic action of each extract: <i>E. sativa</i> and <i>C. olitorius</i> are mainly capping/reducing agents as they contain high levels of phenolic and flavonoid compounds, and garlic provides organosulfur compounds that supplement the source of sulfur when nucleating MoS<sub>2</sub>. The MoS<sub>2</sub> nanostructures formed under the influence of different factors were characterized with the help of XRD, XPS, SEM, AFM, UV-Vis, Raman spectroscopy, and zeta potential analysis. XRD was used to confirm that hexagonal 2&#xa0;H-MoS<sub>2</sub> (JCPDS No. 37-1492) with nanocrystallites sizes of 6.9–11.5&#xa0;nm had been formed. XPS analysis showed typical Mo 3d, and S 2p binding energies confirming the + 4 oxidation state of Mo and the presence of sulfide ions (S 2p -), with no evidence of Mo 6p +. SEM and AFM revealed particle sizes of 31–90&#xa0;nm and surface roughness (Sa) of 9.1–33.9&#xa0;nm, respectively. The characteristic E¹₂g and A₁g vibrational modes of 2&#xa0;H-MoS<sub>2</sub> at the approximate frequencies of 382&#xa0;cm<sup>− 1</sup> and 407&#xa0;cm<sup>− 1</sup> respectively, with an interchange of frequencies (25&#xa0;cm<sup>− 1</sup>) confirming few-layer nanostructures. Quantum confinement was evident, as shown by optical bandgap values (2.9–3.1&#xa0;eV). High colloidal stability was verified by Zeta potential (&lt; -30 mV). Antibacterial testing against Staphylococcus aureus (ATCC 25923) and Escherichia coli (ATCC 25922) by agar well diffusion demonstrated that the synthesized MoS<sub>2</sub> nanostructures have enhanced inhibition zones (19.7–20.3&#xa0;mm against S. aureus) compared to the crude extracts (typically 8–12&#xa0;mm). Statistical analysis (one-way ANOVA, Tukey test, <i>p</i> &lt; 0.05) indicated that there were significant differences among samples.</p>

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Phytochemical-mediated synthesis of 2 H-MoS₂ nanostructures for antibacterial activity: correlation between plant extract composition and quantum confinement

  • Bilal K. Al-Rawi,
  • Dalya H. Hamad

摘要

In this study, a green synthesis methodology to synthesize molybdenum disulfide (MoS2) nanostructures using plant extracts as biogenic reducing and stabilizing agents. Eruca sativa (arugula) and Corchorus olitorius (jute mallow) aqueous extracts were used as natural reducing agents whereas the garlic extract was used as a complementary source of bio-sulfur and thioacetamide under mild reflux conditions. To clarify the mechanistic action of each extract: E. sativa and C. olitorius are mainly capping/reducing agents as they contain high levels of phenolic and flavonoid compounds, and garlic provides organosulfur compounds that supplement the source of sulfur when nucleating MoS2. The MoS2 nanostructures formed under the influence of different factors were characterized with the help of XRD, XPS, SEM, AFM, UV-Vis, Raman spectroscopy, and zeta potential analysis. XRD was used to confirm that hexagonal 2 H-MoS2 (JCPDS No. 37-1492) with nanocrystallites sizes of 6.9–11.5 nm had been formed. XPS analysis showed typical Mo 3d, and S 2p binding energies confirming the + 4 oxidation state of Mo and the presence of sulfide ions (S 2p -), with no evidence of Mo 6p +. SEM and AFM revealed particle sizes of 31–90 nm and surface roughness (Sa) of 9.1–33.9 nm, respectively. The characteristic E¹₂g and A₁g vibrational modes of 2 H-MoS2 at the approximate frequencies of 382 cm− 1 and 407 cm− 1 respectively, with an interchange of frequencies (25 cm− 1) confirming few-layer nanostructures. Quantum confinement was evident, as shown by optical bandgap values (2.9–3.1 eV). High colloidal stability was verified by Zeta potential (< -30 mV). Antibacterial testing against Staphylococcus aureus (ATCC 25923) and Escherichia coli (ATCC 25922) by agar well diffusion demonstrated that the synthesized MoS2 nanostructures have enhanced inhibition zones (19.7–20.3 mm against S. aureus) compared to the crude extracts (typically 8–12 mm). Statistical analysis (one-way ANOVA, Tukey test, p < 0.05) indicated that there were significant differences among samples.