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. 2024 Feb 7;24(4):1093.
doi: 10.3390/s24041093.

Selective and Accurate Detection of Nitrate in Aquaculture Water with Surface-Enhanced Raman Scattering (SERS) Using Gold Nanoparticles Decorated with β-Cyclodextrins

Zhen Li  1   2   3   4   5 , Yang Hu  1   3   4 , Liu Wang  1   3   4 , Houfang Liu  2   5 , Tianling Ren  2   5 , Cong Wang  1   3   4 , Daoliang Li  1   3   4
Affiliations

Selective and Accurate Detection of Nitrate in Aquaculture Water with Surface-Enhanced Raman Scattering (SERS) Using Gold Nanoparticles Decorated with β-Cyclodextrins

Zhen Li et al. Sensors (Basel). .

Abstract

A surface-enhanced Raman scattering (SERS) method for measuring nitrate nitrogen in aquaculture water was developed using a substrate of β-cyclodextrin-modified gold nanoparticles (SH-β-CD@AuNPs). Addressing the issues of low sensitivity, narrow linear range, and relatively poor selectivity of single metal nanoparticles in the SERS detection of nitrate nitrogen, we combined metal nanoparticles with cyclodextrin supramolecular compounds to prepare a AuNPs substrate enveloped by cyclodextrin, which exhibits ultra-high selectivity and Raman activity. Subsequently, vanadium(III) chloride was used to convert nitrate ions into nitrite ions. The adsorption mechanism between the reaction product benzotriazole (BTAH) of o-phenylenediamine (OPD) and nitrite ions on the SH-β-CD@AuNPs substrate was studied through SERS, achieving the simultaneous detection of nitrate nitrogen and nitrite nitrogen. The experimental results show that BTAH exhibits distinct SERS characteristic peaks at 1168, 1240, 1375, and 1600 cm-1, with the lowest detection limits of 3.33 × 10-2, 5.84 × 10-2, 2.40 × 10-2, and 1.05 × 10-2 μmol/L, respectively, and a linear range of 0.1-30.0 μmol/L. The proposed method provides an effective tool for the selective and accurate online detection of nitrite and nitrate nitrogen in aquaculture water.

Keywords: SERS; aquaculture water; gold nanoparticles; nitrate nitrogen detection; β-cyclodextrin.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
Schematic illustration of reaction of nitrite and OPD under acid conditions.
Figure 2
Figure 2
UV–vis spectrum absorption spectra of AuNPs and SH-β-CD@AuNPs.
Figure 3
Figure 3
The zeta potential of SH-β-CD@AuNPs.
Figure 4
Figure 4
TEM images of SH-β-CD@AuNPs.
Figure 5
Figure 5
Size-distribution histogram of AuNPs (left) and SH-β-CD@AuNPs (right).
Figure 6
Figure 6
Characterization of the detection process. (a) SERS of OPD (100 μmol/L); (b) SERS of NaNO3 solutions (10 μmol/L); (c) SERS of NaNO2 solutions (10 μmol/L); (d) NRS of BTAH derived from the reaction between NO2− and OPD; (e) SERS of BTAH on AuNPs; (f) SERS of BTAH based on SH-β-CD@AuNPs.
Figure 7
Figure 7
(a) Changes in SERS intensity of nitrate ion derivatives at 1660 cm−1; (b) SERS spectra of nitrate ion derivatives at the same concentration within three weeks.
Figure 8
Figure 8
Repeatability of SH-β-CD@AuNP substrate prepared in different batches.
Figure 9
Figure 9
The influence of pH.
Figure 10
Figure 10
(a) The influence of cyclization reaction time; (b) The influence of adsorption time of BTAH on SH-β-CD@AuNPs substrate.
Figure 11
Figure 11
The influence of different concentrations of OPD solutions on the SERS intensity at 1600 cm−1.
Figure 12
Figure 12
SERS spectra of the mixed solution with different concentrations of SH-β-CD@AuNPs.
Figure 13
Figure 13
The influence of interfering ions.
Figure 14
Figure 14
SERS spectra of BTAH at different concentrations of nitrate ions: (a) 0.1, (b) 0.3, (c) 0.5, (d) 0.7, (e) 1, (f) 3, (g) 5, (h) 7, (i) 10, (j) 30, (k) 50 μmol/L.
Figure 15
Figure 15
The calibration curves at 1168, 1240, 1375, and 1600 cm−1.
See this image and copyright information in PMC

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