In this study, we developed an innovative approach that combines solid phase microextraction (SPME) with surface-enhanced Raman spectroscopy (SERS) to detect pesticide ferbam rapidly. An Au nano-glass capillary was fabricated by coating template-freely synthesized three-dimensional network Au nanostructures (3D-NW AuNSs) on the roughened surface of glass capillary and used for SPME and SERS respectively. Significant Raman signals were obtained by the SPME-SERS method, followed by detection of ferbam in water and orange juice samples with only 1 min SPME process. Results showed that Au nano-glass capillaries could achieve the detection of ferbam with limit of detection of 0.05 μg/L, and coefficient of determination (R2) of 0.9913. The recovery of predicted results was in the range of 88.46–103.29% and the relative standard deviation (RSD) was 3.5–8.2%. This study demonstrated potential capability of the SPME-SERS method for rapid (within 1 min) and sensitive detection of organic compounds in complex matrices. The SERS-active Au nano-glass capillary is easy to carry and operate, and is expected to play a role in the detection of trace pollutants.
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