Gold Precursor Research Articles

Highly sensitive multiplexed colorimetric lateral flow immunoassay by plasmon-controlled metal-silica isoform nanocomposites: PINs.

Lateral flow assay (LFA) systems use metal nanoparticles for rapid and convenient target detection and are extensively studied for the diagnostics of various diseases. Gold nanoparticles (AuNPs) are often used as probes in LFAs, displaying a single red color. However, there is a high demand for colorimetric LFAs to detect multiple biomarkers, requiring the use of multicolored NPs. Here, we present a highly sensitive multiplexed colorimetric lateral flow immunoassay by multicolored Plasmon-controlled metal-silica Isoform Nanocomposites (PINs). We utilized the localized surface plasmon resonance effect to create multi-colored PINs by precisely adjusting the distance between the NPs on the surface of PINs through the controlled addition of reduced gold and silver precursors. Through simulations, we also confirmed that the distance between nanoparticles on the surface of PINs significantly affects the color and colorimetric signal intensity of the PINs. We achieved multicolored PINs that exhibit stronger colorimetric signals, offering a new solution for LFA detection with high sensitivity and a 33 times reduced limit of detection (LOD) while maintaining consistent size deviations within 5%. We expect that our PINs-based colorimetric LFA will facilitate the sensitive and simultaneous detection of multiple biomarkers in point-of-care testing.

Ultrapure gold recovery from electronic waste as nanoparticles immobilized in hydrogel matrix

Solid-supported gold nanoparticles possess significant value as economical and eco-friendly catalysts due to their durability and reusability. Conventional methods to synthesize heterogeneous catalysts require the use of expensive gold precursors, diminishing their economic viability. Recovering gold directly as nanoparticles immobilized in a solid matrix from electronic waste (e-waste) provides a promising economic solution. However, the greater abundance of other metal ions in e-waste solutions makes this task challenging, demanding more selective approaches. This study presents a cost-effective one-pot synthesis of gold nanoparticles immobilized in a hydrogel matrix from e-waste solutions, circumventing the need for gold precursors. The fabricated hydrogel exhibits exceptionally selective gold reduction, producing well-distributed and highly pure (23.78 K) gold nanoparticles inside the hydrogel matrix. The fine control in nanoparticle diameters from 22 to 35 nm was achieved by tuning the monomer compositions of the hydrogel. These hydrogel-supported gold nanoparticles demonstrate reusable catalytic properties, indicating their potential sustainability and industrial compatibility. This approach addresses the economic challenges of synthesizing solid-supported gold nanoparticles and offers a sustainable pathway.

Polyvinyl alcohol assisted citrate based reduction of gold(III) ions: Theoretical design and experimental study on green synthesis of spherical and biocompatible gold nanoparticles

In this study, we demonstrate the synthesis of small gold nanoparticles (typically 8-10 nm) through a green synthesis approach. This method involves utilizing chloroauric acid as the gold precursor, trisodium citrate as a mild reducing and co-capping agent, and polyvinyl alcohol (PVA), as a co-capping and shape-directing agent. This novel synthesis method stands alone as a protocol that involves just mixing the reagents at room temperature and allowing the reaction to proceed at ambient temperature without any disturbance. In the absence of PVA, spherical particles are not formed and the reaction mixture slowly turns black followed by precipitation.The synthesis process was meticulously tracked using time-resolved monitoring of the growth of the localized surface plasmon resonance (LSPR) by UV-vis spectroscopy and transmission electron microscopy. The as-prepared colloidal gold solution was bright red, attributed to the small size (≤ 10 nm) and spherical geometry of nanoparticles. This colloidal solution could be stored indefinitely at room temperature without precipitation or a change in its absorption profile. The nanoparticles remained stable in adverse conditions such as 100 mM NaCl solution, 1×PBS and cell culture medium. Additionally, they could be easily loaded with drugs like doxorubicin by adsorption. The particles were thoroughly characterized using a range of techniques, including UV-vis spectroscopy, attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), high-resolution transmission electron microscopy (HRTEM), hyperspectral-enhanced dark field microscopy (HEDFM), dynamic light scattering (DLS), and X-ray photoelectron spectroscopy (XPS). Cell viability tests conducted on 2D cell lines and 3D spheroids revealed negligible toxicity even at high concentrations. Furthermore, we demonstrate that an advanced version of conventional diffusion-limited aggregation (DLA) schemes, which allows individual clusters to move freely within a domain to form larger aggregates, can effectively replicate the intricate interactions between chloroauric acid, trisodium citrate, and PVA, the agents involved in the synthesis of gold nanoparticles.

Heteronanotrimers by Selective Photodeposition of Gold Nanodots on Janus-Type Cu2‒ xS/CuInS2 Heteronanocrystals.

This study focuses on the development of environmentally friendly Au-Cu2-xS/CuInS2 heteronanotrimers. The chosen strategy relies on the laser photodeposition of a single gold nanodot (ND) onto Janus Cu2- xS/CuInS2 heteronanocrystals (HNCs). This method offers precise control over the number, location, and size (5 to 8nm) of the Au NDs by adjusting laser power for the career production, concentration of hole scavenger for charge equilibration in redox reactions, and gold precursor concentration, and exposure time for the final ND size. The photoreduction of gold ions onto HNCs starts systematically at the Cu2- xS tip. The Au deposition then depends on the CuInS2 segment length. For short HNCs, stable Au-Cu2- xS/CuInS2 heteronanotrimers form, while long HNCs undergo a secondary photo-induced step: the initial Au ND is progressively oxidized, with concomitant deposition of a second gold ND on the CuInS2 side, to yield Au2S-Cu2- xS/CuInS2-Au heteronanotrimers. Results are rationalized by quantitative comparison with a model that describes the growth kinetics of NDs and Au-Cu2- xS transformation and emphasizes the importance of charge separation in predicting selective deposition in heteronanotrimer production. The key parameter controlling Au-Cu2‒ xS/CuInS2 HNCs is the photoinduced electric field gradient generated by charge separation, which is tailored by controlling the CuInS2 segment size.

Plasma and radiation mediated green synthesis of gold Nanoparticles-immobilized bio-template based catalytic reactor ‘AuNICaR’: Mechanistic insights, catalytic performance and reusability analysis

The present work reports a green, non-thermal plasma-based approach for efficient synthesis of a gold nanoparticles (Au NPs) Immobilized Catalytic Reactor “AuNICaR” via a novel, efficient, indigenously developed process termed “Plasma Assisted Synthesis and Simultaneous Immobilization (PASSI)”, using isopropanol to enhance the reducing plasma environment. Au NPs were synthesized and simultaneously immobilized onto a cellulose based bio-template pre-functionalized via radiation induced grafting of 2,3-epoxypropylmethacrylate (EPMA) onto a nonwoven cellulose (NWC) substrate. The process entails minimal wastage of expensive gold precursor and eliminates use of external chemicals (reducing and stabilizing agents). Samples were characterized by 13C NMR, FTIR, XPS, TGA, DSC, SEM-EDS, BET, and EDXRF analysis. Catalytic activity was assessed by spectrophotometrically monitoring the reduction of p-nitroaniline (PNA) in presence of NaBH4. DFT calculations established the interaction between Au NPs and EPMA groups of the bio-template to be occurring in ratios of 1:1 and 1:2, with 1:1 being more stable. ANN modelling was also invoked to investigate the effect of simultaneous variation of plasma process parameters on the catalytic performance. AuNICaR was demonstrated for catalytic reduction of pollutants: PNA, p-nitrophenol (PNP) and methyl orange (MO) azo dye in both batch and continuous flow mode. Over 25000 mL of cumulative pollutant feed with concentrations ranging from 0.06 mM − 2 mM was treated at a flow rate of 540 mL.h−1, using a single catalyst batch after intermittent washing with water. With excellent storage stability of > 12 months and > 92 % retention in catalytic activity post multiple cycles, AuNICaR certifies as a potentially inexhaustible catalytic system for cost-effective pollutant treatment.

Gold nanoparticle-mediated nanosecond laser-induced polystyrene carbonization with luminescent products

A highly soluble Au(I) gold precursor is used to produce a nanocomposite material consisting of a polystyrene matrix and gold nanoparticles. Irradiation of such a material with nanosecond laser pulses at the plasmon resonance wavelength leads to the formation of black spots containing luminescent products of carbonization. HR TEM analysis and Raman spectroscopy confirm disordered carbon. A simple model, based on laser heating of a nanoparticle to a temperature of more than 2000 K and stabilization of this temperature by the endothermic process of polystyrene carbonization, fits well with the dependence of the luminescent signal increment on the laser fluence.

Single laser synthesis of gold nanoparticles-polypyrrole-chitosan on laser-induced graphene for ascorbic acid detection

The simultaneous synthesis of gold nanoparticles (AuNPs) and graphene by laser ablation was demonstrated. The in-situ synthesis was performed by laser ablation of a polymer substrate covered with a gold precursor dispersion. The gold precursor was prepared in a copolymer solution of pyrrole (Py) and chitosan (Chi) to improve the nucleation of gold embedded on the laser-induced graphene electrode (LIGE). The morphology of AuNPs-pPy-Chi/LIGE was studied by scanning electron microscopy and characterized electrochemically by cyclic voltammetry. A comprehensive investigation of the electrochemical and physical features of the AuNPs-pPy-Chi/LIGE was carried out. The parameters of differential pulse voltammetry were adjusted to enhance the response to ascorbic acid (AA). The AuNPs-pPy-Chi/LIGE produced two linear ranges: from 0.25 to 5.00 and 5.00–25.00 mmol L−1. The limit of detection was 0.22 mmol L−1. Hundreds of electrodes were tested to demonstrate the excellent reproducibility of the AuNPs-pPy-Chi/LIGE fabrication. Overall, the proposed electrode allows the successful detection of AA in orange juice products with acceptable accuracy (recoveries = 97 ± 2 to 109.1 ± 0.7). The preparation strategy of the proposed AuNPs-pPy-Chi/LIGE could be adapted to detect other compounds or biomarkers.

Facile Fabrication of SERS Substrates by the Electrodeposition Method to Detect Pesticides with High Enhancement Effect and Long-Term Stability.

In this study, surface-enhanced Raman scattering substrates were investigated by the electrodeposition method to detect low concentrations of pesticides via the electrodeposition method with different agents from silver and gold precursors on APTES-modified ITO glass. A dual-potential method supplied three electrodes and was performed with a nucleation potential of 0.7 V for 2 s and a growth potential of -0.2 V for 500 s. The Ag film produced by the electrodeposition approach has great surface uniformity and good SERS signal amplification for the thiram insecticide at low concentrations. Interestingly, the ITO/APTES/Ag substrate extensively increased the sensitivity than the other investigated ones, thanks to the adequate assistance of amino groups of APTES in the denser and hierarchical deposition of Ag NPs. These observations were additionally elucidated via finite-difference time-domain (FDTD) calculation. For thiram, the detection was set at 10-8 M with an enhancement factor of up to 3.6 × 107 times. Comparing the SERS spectra of thiram at concentrations of 10-3, 10-4, and 10-5 M with a relative standard deviation (RSD) of less than 7.0% demonstrates excellent reproducibility of the ITO/APTES/Ag substrate. In addition, the special selectivity of the ITO/APTES/Ag substrate for thiram demonstrates that these nanostructures can identify pesticides with extreme sensitivity.

Growth‐Induced Extinction Development of Gold Nanoclusters as Signal Transducers for Quantitative Immunoassays

AbstractSignal transducers are crucial in bioassay platforms for converting target detection into recordable signals. Commonly used color development for immunoassays involves enzymes and colorimetric substrates. However, due to cost and environmental issues, practical point‐of‐care testing requires alternative signal transducers. Growth‐induced extinction (absorption and scattering) of gold nanoclusters (AuNCs) is proposed as a novel approach for quantitative immunoassays. AuNCs devoid of localized surface plasmon resonance (LSPR) are used as seeds for growth reactions. Through reactions with a growth solution comprised of gold precursor and mild reductant, AuNCs of varying concentrations underwent controlled growth, resulting in nanoparticles of different sizes exhibiting distinct LSPR‐mediated extinction bands. Notably, the seed concentration exhibited a robust correlation with the resulting extinction of the grown particles on a small scale of 110 µL for a 96‐well microplate platform. To demonstrate this signal transduction mechanism, immunosorbent assays are performed using the conjugates of AuNC and detection antibody. The sandwich‐type assay successfully quantified a model antigen, human immunoglobulin G (hIgG), by monitoring LSPR wavelength and absorbance. This assay demonstrated a working range of 0.001–1 µg mL−1 and limit of detection of 1.19 ng mL−1. Signal transducers using the growth of AuNCs offer new alternative candidates for immunoassay platforms.

3D Superstructures Consisting of Intersecting Gold Lamellae Formed by a Micelle‐Mediated Anisotropic Growth Approach

3D superstructures (3DSs) have attracted increasing interest because of the collective synergistic effects of individual building units, but their customization relies on tedious multistep strategy or high‐end nanofabrication technology. Herein, for the first time, a facile block copolymer micelle‐mediated anisotropic growth approach is reported to fabricate gold 3DSs consisting of tunable and intersecting lamellae with sawtooth‐like edges. The preparation of the 3DSs depends on the mediation of reduction kinetics of gold precursors and adsorption of block copolymer micelles on gold crystal surfaces using disulfiram as ligands. The thickness of lamellae in the 3DSs is controllable from ≈21 to 102 nm by adjusting the weight fraction of the micellar hydrophobicity blocks and the composed lamellar number is regulated from ≈3 to ≈30. Additional morphologies, such as a dendritic mesoporous structure and meatball‐like shapes, are obtained through controlling the extent of micelle swelling. Finite‐difference time‐domain simulations demonstrate that the unique 3DSs of gold lamellae with sawtooth‐like edges form abundant hotspots giving rise to surface‐enhanced Raman scattering (SERS). The 3DSs exhibit strong electromagnetic field enhancement and excellent performance as SERS substrates for detecting 4‐mercaptobenzoic acid.

Synthesis of Gold Nanoparticles over CoAl Mixed Oxide for Ethanol Oxidation Reaction.

Catalytic total oxidation is an effective technique for the treatment of industrial VOCs principally resulting from industrial processes using solvents and usually containing mono-aromatics (BTEX) and oxygenated compounds (acetone, ethanol, butanone). The aim of this work is to deposit gold nanoparticles on CoAl mixed oxide issued from layered double hydroxide (LDH) precursor by using the deposition precipitation (DP) method, which is applied with two modifications, labeled method (A) and method (B), in order to enhance the interaction of the HAuCl4 precursor with the support. Method (A) involves the hydrolysis of the HAuCl4 precursor after addition of the support, while in method (B), the gold precursor is hydrolyzed before adding the support. The two methods were applied using as support the CoAl mixed oxide and the LDH precursor. Samples were characterized by several physical chemical techniques and evaluated for ethanol total oxidation. Method (B) allowed the ethanol oxidation activity to be enhanced for the resulting Au/CoAlOx catalysts thanks to the high surface concentration of Co2+ and improved reducibility at low temperature. The presence of gold permits to minimize the formation of by-products, notably, methanol, allowed for a total oxidation of ethanol at lower temperature than the corresponding support.

Hydrothermal synthesis of regular and flaky gold particles for printed electronics

In this study, the gold precursors were rapidly reduced by hydroxy compound and micron-sized flaky gold powder was obtained under hydrothermal conditions. Isopropyl alcohol was selected as solvent and reducing agent after investigating the effect of reducing agent on the morphology of the gold powder. The influence of reaction concentration and temperature on the particle size and morphology of gold powder were researched. By controlling the reaction concentration and temperature, the prepared gold particles have regular flaky structure with the diameter of about 5 μm and the sintered gold conductor paste shows excellent conductivity and sintering density.

NOVEL APPROACH FOR ONE-POT SELF-ASSEMBLED MONOLAYER PREPARATION OF GOLD TIPPED CdSe/CdS NANORODS

In this study, CdSe/CdS nanorods (NRs) were synthesized via hot injection method to perform simultaneous self-assembly studies with gold tip formation on the nanorods. In this new approach, we propose and demonstrate reductant chemical and gold organosol-free synthesis of gold-tipped nanocrystals on the subphase. Instead of gold organosol usage, gold precursor was prepared by addition of gold source into subphase, and photocatalytic reduction of gold on the tip of nanorods was achieved by exciting the samples under UV-light excitation. Reduction of gold nanoparticles on the tip of NRs was also tried by heating effect, which results in nanopillar formation. The optical properties of these nanorods were determined by spectrophotometric measurements, and gold-tipped nanorods were imaged by TEM analysis. This method enables self-assembly of nanorods and following gold tip formation on the subphase, and it can pave the way to prepare well-defined metal-tipped oriented surfaces that can be used for optical and photocatalysis applications.

Size-Dependent Surface Plasmon Resonance of Green Synthesized Gold Nanoparticles Using <i>Mangifera indica</i> Fruit Peel Extract

Gold nanoparticles (AuNPs) have been studied for various applications due to their adjustable surface plasmon resonance (SPR) properties and facile synthesis. AuNP production has predominantly relied on synthetic chemicals to reduce and stabilize gold precursors. There is an increasing demand for environmentally friendly synthesis methods due to ecological concerns. This work introduced a green synthesis approach using Mangifera indica fruit peel extract. Obtained through maceration of dried fruit peels, this extract served as a reducing agent for gold precursors at 80°C. We obtained varying sizes of AuNPs by manipulating the initial concentration of gold ions: 0.1mM, 0.25mM, and 0.5mM. The UV-vis spectroscopy results confirmed the signature SPR peak for AuNPs around 530 nm, with peak shifts highly dependent on the gold ion concentration. The dynamic light scattering (DLS) measurements revealed hydrodynamic diameters of 89.5 nm, 121.5 nm, and 144.5 nm for the various concentrations. The Fourier transform (FTIR) analysis identified the role of inherent phenols and flavonoids in gold precursor reduction. This study emphasizes the potential of Mangifera indica fruit peel extract as a viable alternative for AuNP synthesis. This study could possibly boost the utilization of gold nanoparticles towards applications in biology and medicine as well as environmental remediation.

Synthesis of AuNPs in microemulsion and nano-emulsion systems using aqueous extract of C. chayamansa leaves as reducing agent

This paper explores the synthesis and characterization of gold nanoparticles using various microemulsion and nano-emulsion systems. The pseudo-ternary system consists of an aqueous phase / Brij O10: 1,2-hexanediol (1:1) / castor oil; the aqueous phases include the aqueous extract of Chaya Maya (Cnidoscolus chayamansa) leaves or aqueous extract of Chaya maya leaves combined with the inorganic gold precursor. Chaya maya extract act as a reducing agent for gold (III) ions. The influence of aqueous phase content and surfactant concentration on gold nanoparticles size, morphology, and stability is investigated. Dynamic Light Scattering, Scanning Transmission Electron Microscopy, and UV-Vis spectroscopy are employed to analyze the synthesized gold nanoparticles. The sizes of the gold nanoparticles obtained were influenced by the system composition and are within the range of 19–40 nm. Results indicate that increasing the aqueous phase content generally leads to larger nanoparticle sizes, while higher surfactant concentrations yield smaller nanoparticles. A transition from microemulsion to nano-emulsion is observed at a specific aqueous phase content, marking a shift in nanoparticle size distribution and growth behavior. Additionally, microemulsion and nano-emulsion systems provide stability to gold nanoparticles, as evidenced by measured Zeta potentials indicating negatively charged surfaces conducting to colloidal stability. Also, remark that the use of organometallic precursors is no needed to obtain very good results on nanoparticle size and shape when O/W systems are used to this end. These findings highlight the potential of tailored microemulsion and nano-emulsion systems formulated with low-toxic components for controlling gold nanoparticles properties under mild conditions, contributing to the development of advanced gold nanoparticles-based materials with enhanced functionalities, with implications for diverse applications.

Plasmon-based colorimetric assay using green synthesized gold nanoparticles for the detection of bisphenol A.

Herein, we report a green synthesized gold nanoparticle (AuNPs) based colorimetric detection of bisphenol A (BPA). The AuNPs were synthesized using khat leaf extract as a reducing agent by optimizing factors affecting the AuNPs synthesis, including gold precursor concentration (1mM), and reaction temperature (60°C). The AuNPs characterization was carried out using ultraviolet-visible spectrophotometry and transmission electron microscopy, and it was found spherical with an average particle size of 17.3 ± 3.7nm. A colorimetric nanosensor was developed by conjugation of bio-inspired AuNPs with BPA-specific aptamer for a quick and easy detection of BPA in plastic bottled water. The colorimetric assay relies on the strong affinity of BPA for aptamer, which causes detachment of the aptamer from the AuNPs surface in the presence of BPA inducing AuNPs aggregation. To achieve the colorimetric detection of BPA, the concentrations of NaCl and aptamer were optimized. The detection of BPA was monitored visually using a naked eye, as well as quantitatively using an ultraviolet-visible spectrophotometer. The method visual limit of detection (LOD) was determined to be 0.1ng/mL and reached 0.09ng/mL using ultraviolet-visible spectrophotometer. The method demonstrated very good linearity (R2 = 0.9986) in the range of 0.1-100ng/mL. The proposed method showed high sensitivity to BPA detection in plastic bottled water with 86.7-98.0%, recovery. Therefore, the proposed colorimetric nanosensor can be used for determination of BPA in plastic bottled waters with reliable performance at lower concentrations.

Water-assisted purification during electron beam-induced deposition of platinum and gold.

Direct fabrication of pure metallic nanostructures is one of the main aims of focused electron beam-induced deposition (FEBID). It was recently achieved for gold deposits by the co-injection of a water precursor and the gold precursor Au(tfac)Me2. In this work results are reported, using the same approach, on a different gold precursor, Au(acac)Me2, as well as the frequently used platinum precursor MeCpPtMe3. As a water precursor MgSO4·7H2O was used. The purification during deposition led to a decrease of the carbon-to-gold ratio (in atom %) from 2.8 to 0.5 and a decrease of the carbon-to-platinum ratio (in atom %) from 6-7 to 0.2. The purification was done in a regular scanning electron microscope using commercially available components and chemicals, which paves the way for a broader application of direct etching-assisted FEBID to obtain pure metallic structures.

High yield seedless synthesis of mini gold nanorods: partial silver decoupling allows effective nanorod elongation with tunable surface plasmon resonance beyond 1000 nm and CTAB-free functional coating for mTHPC conjugation.

Gold nanorods with small dimensions demonstrate better cellular uptake and absorption efficiency. The ability to synthesize gold nanorods while maintaining a tunable high aspect ratio is challenging as it requires careful control of reaction conditions, often employing additional steps such as pH modification or the use of polymeric additives. We demonstrate a seedless approach for the synthesis of mini (width < 10 nm) gold nanorods with tunable longitudinal surface plasmon resonance from ∼700 nm to >1000 nm and aspect ratios ranging from ∼3 to ∼7 without the use of any polymeric additives or pH modification. A single mild reducing agent, hydroquinone, allowed for up to ∼98% reaction yield from a gold precursor. A mechanism for elongation is proposed based on partial silver decoupling from the reaction. Finally, the particles were coated with various capping agents to allow functionalization and conjugation of mTHPC drug molecules, which are used in photodynamic treatments, and cytotoxic CTAB was removed to increase their biocompatibility.

Fabrication of Chiral Plasmonic Photocatalyst By Circularly Polarized Light and Enantioselective Hydrogen Generation Activity

Introducing chirality in nanostructures has been explored actively in various field, such as sensing, optoelectronics and catalysts, due to its unique chiroptical properties. Especially in photochemistry, considering the synergistic interaction between chiral plasmonics and polarized light, they can be utilized to improve efficiency and selectivity of catalytic reaction. In this work, we synthesized chiral plasmonic photocatalysts, (R)-,(L)- Au/C3N4, through photoreduction of gold precursor on C3N4 substrate under the irradiation of circularly polarized light (CPL) as a means to induce chirality. Then, we demonstrated that the efficiency of hydrogen generation can be increased by matching the chirality of the CPL with the photocatalyst, which was 2-fold enhanced than chiral mismatching conditions. This can be explained by the asymmetric hot carrier formation of chiral plasmonic structures under CPL excitation. Also, the reactivity of water molecule with photocatalyst surface was confirmed through in-situ FT-IR, showing the enhanced interaction under chiral matching conditions. This study could pave the way for advancing chiral light-matter interactions and explore the application of novel device, particularly toward chiral-induced photocatalytic performance.

Efficient Analysis of Small Molecules via Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (LDI-TOF MS) Using Gold Nanoshells with Nanogaps.

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a commonly used technique for analyzing large biomolecules. However, the utilization of organic matrices limits the small-molecule analysis because of the interferences in the low-mass region and the reproducibility issues. To overcome these limitations, a surface-assisted laser desorption/ionization (SALDI), which utilizes nanostructured metallic surfaces, has been developed. Herein, a novel approach for SALDI-MS was proposed using silica@gold core-shell hybrid materials with a nanogap-rich shell (SiO2@Au NGS), which is an emerging material due to its excellent heat-generating capabilities. The gold shell thickness was controlled by adjusting the concentration of gold precursor for the growth of gold nanoparticles. SALDI-MS measurements were performed on a layer formed by drop-casting a mixture of SiO2@Au NGS and analytes. At the optimized process, the gold shell thickness was observed to be 17.2 nm, which showed the highest absorbance. Based on the enhanced SALDI capability, SiO2@Au NGS was utilized to detect various small molecules, including amino acids, sugars, and flavonoids, and the ionization softness was confirmed with a survival yield upon fragmentation. The limits of detection, reproducibility, and salt tolerance of SiO2@Au NGS demonstrate its potential as an effective and reliable SALDI material for small-molecule analyses.