Chem. J. Chinese Universities ›› 2025, Vol. 46 ›› Issue (4): 20240514.doi: 10.7503/cjcu20240514

• Analytical Chemistry • Previous Articles     Next Articles

Preparation of TLC-SERS Hyphenated Substrate and Application in Monitoring Organic Reactions

LU Beibei, ZHANG Chenjie, XU Minmin, YAO Jianlin()   

  1. College of Chemistry,Chemical Engineering and Materials Science,Soochow University,Suzhou 215123,China
  • Received:2024-11-20 Online:2025-04-10 Published:2025-01-07
  • Contact: YAO Jianlin E-mail:jlyao@suda.edu.cn
  • Supported by:
    the National Natural Science Foundation of China(22172109);the Natural Science Foundation of the Jiangsu Higher Education Institutions of China(21KJA150009)

Abstract:

Surface-enhanced Raman spectroscopy(SERS) has become a powerful analytical technique due to its high sensitivity, strong specificity, and non-destructive in situ detection. However, there are still great challenges for rapid detection with SERS in mixed systems. Herein, a large-area Au@SiO2 monolayer film with highly homogeneous was prepared by the liquid-liquid interface self-assembly method, and was transferred to the plate as SERS substrate. By combining the SERS with thin layer chromatography(TLC) techniques, a novel TLC-SERS hyphenated technology was constructed to overcome the difficulty of detection in mixed systems and allowed to realize the rapid separation and high-sensitivity detection. Studies on the stability and uniformity of the built-in Au@SiO2 SERS substrates were performed. It demonstrated that the problems of secondary diffusion of separation spots and interference of silica gel background in the previous TLC-SERS hyphenated technology were dissolved successfully. The new TLC-SERS hyphenated technology was explored to monitor the Suzuki coupling reaction process of phenylboronic acid and 3-bromopyridine. The overlap of different species on the hyphenated plate and the by-product were recognized according. Furthermore, it was successfully used to separate and identify the selective 1,2-dialkylation reaction products without standard samples. The result revealed that SERS played the important role in characterizing the structure of the spots separated by TLC and distinguishing the corresponding information for overlapping spots. The present hyphenated technology based on the novel combined substrate can be developed as a promising tool for solving the problems of separation on mixtures and fast monitoring the organic chemical reactions.

Key words: Thin-layer chromatography, Surface-enhanced Raman spectroscopy, Hyphenated technology, Au@SiO2, Organic reaction

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