Abstract

The residues of deltamethrin (DM) and carbofuran (CBF) in soil is becoming an intractable problem causing soil hardening and environmental pollution. This paper reports a very simple method via improved reduction of chloroauric acid by the trisodium citrate method for fabricating gold nanoparticles (AuNPs), which were used as a surface enhanced Raman scattering (SERS) active colloids with the advantages of ultrasensitivity, reproducibility and chemical stability. The results demonstrated that the limits of detection (LODs) of the DM and CBF were found to be as low as 0.01 mg/L. The SERS intensity showed a good linear relationship with DM (R2 = 0.9908) and CBF (R2 = 0.9801) concentration from 0.01 to 10 mg/L. In a practical application, DM and CBF residues in soil were easily detected by SERS with the flexible AuNPs colloids, and the LODs of DM and CBF were found to be as low as 0.056 mg/kg and 0.053 mg/kg, respectively. Moreover, DM in soil could be qualitatively detected by the characteristic peaks at 560 and 1000 cm−1, and CBF in soil could be qualitatively detected by the characteristic peaks at 1000 and 1299 cm−1. The determination coefficient (R2p) for DM and CBF reached 0.9176 and 0.8517 in partial least squares (PLS) model. Overall, it is believed that the prepared AuNPs can provide technical support for the accurate detection of pesticide residues in soil by SERS technique.

Highlights

  • Pesticides are indispensable means of production in modern agriculture, which have been used to control a large variety of insects, fungi, viruses, and weeds [1,2,3]

  • We describe a very simple method for preparing ultrasensitive and reproducible AuNPs by improved reduction of chloroauric acid by the trisodium citrate method, aiming to basically solve the problems of quantitative detection of DM and CBF residues in soil as well as the improvement of surface enhanced Raman scattering (SERS) determination accuracy

  • DM and CBF residues in soil were detected using Agilent 1290 Ultra High Performance Liquid Chromatography combined with a Photodiode Array Detector (Agilent Technology Co., Ltd., Santa Clara, CA, USA)

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Summary

Introduction

Pesticides are indispensable means of production in modern agriculture, which have been used to control a large variety of insects, fungi, viruses, and weeds [1,2,3]. Et al used the prepared AuNPs (100 mL of 50 mg/L chloroauric acid solution and 4 mL of 5 mg/mL trisodium citrate) as SERS colloids for the detection of DM pesticide in strawberries, the LOD reached 0.1 mg/L [21]. We describe a very simple method for preparing ultrasensitive and reproducible AuNPs by improved reduction of chloroauric acid by the trisodium citrate method, aiming to basically solve the problems of quantitative detection of DM and CBF residues in soil as well as the improvement of SERS determination accuracy. The linear regression equation of Raman characteristic peaks achieved good correlation at 1000 and 1299 cm−1 peaks (0.7681 < R2 < 0.7608) as well, indicating that the Raman characteristic peaks at 1000 and 1299 cm−1 can be determined as quantitative characteristic peaks of CBF in soil

Quantitative Determination of DM and CBF in Soil with PLS
Model Accuracy Verification
Chemicals
Instrumentation
Preparation of Gold Nanoparticles
Preparation of Soil Samples
UHPLC Measurement
SERS Measurement
Spectral Preprocessing Methods
Partial Least Squares Model
Model Evaluation Index
Findings
Conclusions
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