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. 2024 Mar 27:12:1348423.
doi: 10.3389/fchem.2024.1348423. eCollection 2024.

Self-assembled core-shell nanoparticles with embedded internal standards for SERS quantitative detection and identification of nicotine released from snus products

Yongfeng Tian  1   2 , Lu Zhao  3 , Xiaofeng Shen  1 , Shanzhai Shang  1 , Yonghua Pan  4 , Gaofeng Dong  1 , Wang Huo  5 , Donglai Zhu  1 , Xianghu Tang  5
Affiliations

Self-assembled core-shell nanoparticles with embedded internal standards for SERS quantitative detection and identification of nicotine released from snus products

Yongfeng Tian et al. Front Chem. .

Abstract

Surface enhanced Raman spectroscopy (SERS) is a unique analytical technique with excellent performance in terms of sensitivity, non-destructive detection and resolution. However, due to the randomness and poor repeatability of hot spot distribution, SERS quantitative analysis is still challenging. Meanwhile, snus is a type of tobacco product that can release nicotine and other components in the mouth without burning, and the rapid detection technique based on SERS can reliably evaluate the amount of nicotine released from snus, which is of great significance for understanding its characteristics and regulating its components. Herein, the strategy was proposed to solve the feasibility of SERS quantitative detection based on self-assembled core-shell nanoparticles with embedded internal standards (EIS) due to EIS signal can effectively correct SERS signal fluctuations caused by different aggregation states and measurement conditions, thus allowing reliable quantitative SERS analysis of targets with different surface affinity. By means of process control, after the Au nanoparticles (Au NPs) were modified with 4-Mercaptobenzonitrile (4-MBN) as internal standard molecules, Ag shell with a certain thickness was grown on the surface of the AuNP@4-MBN, and then the Au@4-MBN@Ag NPs were used to regulate and control the assembly of liquid-liquid interface. The high-density nano-arrays assembled at the liquid-liquid interface ensure high reproducibility as SERS substrates, and which could be used for SERS detection of nicotine released from snus products. In addition, time-mapping research shows that this method can also be used to dynamically monitor the release of nicotine. Moreover, such destruction-free evaluation of the release of nicotine from snus products opens up new perspectives for further research about the impact of nicotinoids-related health programs.

Keywords: SERS (surface enhanced Raman spectroscopy); internal standards; liquid-liquid interface; nicotine; snus.

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Conflict of interest statement

Authors YT, XS, SS, GD, and DZ were employed by Technology Center of China Tobacco Yunnan Industrial Co., Ltd. Author YP was employed by Hongta Tobacco (Group) Co., Ltd. The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Figures

SCHEME 1
SCHEME 1
(A) Schematic illustration of the synthesis of Au@4-MBN@Ag NPs. (B) Illustration of self-assembly of Au@4-MBN@Ag NPs at the cyclohexane-H2O interface. (C) Quasi-synchronous extraction and SERS detection of nicotine release from the snus pouch based on liquid-liquid interface self-assembling Au@4-MBN@Ag NPs.
FIGURE 1
FIGURE 1
(A) UV−vis absorption spectra of Au NPs, Au@4-MBN NPs, Au@4-MBN@Ag NPs and Au@Ag NPs (inset: digital photos of the corresponding samples). (B) Typical Raman spectra of Au NPs (without 4-MBN), Au@4-MBN NPs, Au@4-MBN@Ag NPs, Au@Ag NPs (without 4-MBN), and Au@Ag NPs with 4-MBN molecules; (C–J) SEM and corresponding size distributions of Au NPs, Au@4-MBN NPs, Au@4-MBN@Ag NPs and Au@Ag NPs.
FIGURE 2
FIGURE 2
(A) TEM images of Au@4-MBN@Ag NPs with Ag shell thickness of 2.2, 3.6, 6.4, 8.9, 10.1 and 12.2 nm; (B) UV−vis absorption spectra (inset: digital photos) of Au@4-MBN@Ag NPs with different shell thicknesses; (C) Raman spectra of Au@4-MBN@Ag NPs with different shell thicknesses excited with 633 nm laser; (D) Raman intensity of different shell thicknesses of Au@4-MBN@Ag NPs at 2221 cm−1.
FIGURE 3
FIGURE 3
(A) Typical elemental mappings and (B) EDS spectrum of Au@4-MBN@Ag NPs with Ag shell thickness of 6.4 nm. (C) XPS spectra of Au NPs, Au@4-MBN NPs, and Au@4-MBN@Ag NPs, (D–F) High-resolution Au 4f, S 2p, and Ag 3d spectra corresponding to the XPS spectra represented by (I) azure, (II) magenta, and (III) tangerine bars in (C), respectively.
FIGURE 4
FIGURE 4
(A) Illustration of self-assembly at the cyclohexane-H2O interface of Au@4-MBN@Ag and typical SEM characterization image. (B) Illustration of in situ SERS detection based on liquid-liquid interface self-assembling Au@4-MBN@Ag NPs in reaction cell and digital photo. (C) Photo of SERS detection. (D) Typical Raman spectra of Au@4-MBN@Ag NPs, CV with Au@Ag NPs and Au@4-MBN@Ag NPs as substrates, respectively. (E) Typical Raman spectra of Au@4-MBN@Ag NPs, Au@Ag NPs with nicotine standard solution, Au@4-MBN@Ag NPs with nicotine standard solution, and Au@4-MBN@Ag NPs with snus extraction solution, respectively.
FIGURE 5
FIGURE 5
(A) Series of SERS spectra of nicotine in water at different concentrations with liquid-liquid interface self-assembling Au@4-MBN@Ag NPs as the SERS substrates, respectively. (B) and (C) Plot of the SERS intensities at 1029 cm-1 versus the snus concentration over a large concentration range.
FIGURE 6
FIGURE 6
SERS detection of nicotine release from snus based on liquid-liquid interface self-assembling Au@4-MBN@Ag NPs in reaction cell. (A, B) Time-resolution SERS mapping and typical SERS spectra before calibration based on EIS signals; (C, D) Time-resolution SERS mapping and typical SERS spectra after calibration based on EIS signals.
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