Analytical Chemistry and Spectroscopy

1. On-Site SERS Determination of Sodium Saccharin in Cigarette Paper via AgNP Substrates Prepared with a Portable USB Device

A novel magnetic agitating heater powered by a standard USB port was developed to enable rapid, on-site synthesis of silver colloid substrates for surface-enhanced Raman scattering (SERS). This compact device allows the preparation of Ag colloids within 15 minutes under mild conditions, eliminating the need for long-term storage and addressing the instability issues typically associated with colloidal substrates.

The freshly prepared substrates demonstrated excellent sensitivity and reproducibility, achieving SERS detection of Rhodamine 6G down to 10⁻⁹ mol L⁻¹ with a relative standard deviation of 5.52% (n = 5). Using the optimized substrate, sodium saccharin was detected with a limit of 1 mg L⁻¹. By introducing potassium thiocyanate (KSCN) as an internal standard, a strong linear correlation (R² = 0.98) was obtained between SERS intensity at 708 cm⁻¹ and sodium saccharin concentration in the range of 20–100 mg L⁻¹.

The method enabled direct extraction of sodium saccharin from cigarette tipping paper simply by immersion in water, followed by rapid SERS detection. Quantitative spike-recovery rates ranged from 95.5–116.7% with RSD values of 2.3–12.6%. The entire detection process, including substrate synthesis, was completed in just 30 minutes. This work demonstrates a practical approach for portable SERS substrate preparation and highlights its potential in real-time monitoring and food safety applications.

2. Dual-spectrum online monitoring of puerarin and total flavonoids contents during the extraction process of Pueraria lobata

In this work, we developed a dual-spectrum online monitoring system combining near-infrared (NIR) and ultraviolet–visible (UV–Vis) spectroscopy for real-time quantitative analysis during the extraction of Pueraria lobata. The system circulates the extraction solution through a pipeline using a peristaltic pump, with portable spectrometers collecting NIR and UV–Vis spectra in seconds before the solution is returned to the flask.

Quantitative models based on partial least squares (PLS) regression were constructed to monitor puerarin and total flavonoid content. The root mean square error of prediction (RMSEP) values demonstrated that dual-spectrum analysis (puerarin: 0.0351 mg/mL, flavonoids: 0.1795 mg/mL) significantly outperformed models based on NIR or UV–Vis alone.

This approach provides a fast, stable, and accurate online monitoring tool for herbal extraction processes. By capturing more comprehensive chemical information than individual spectroscopic methods, the dual-spectrum strategy shows strong potential for broader applications in the quantitative analysis of traditional Chinese medicines.

Publications

  1. Huipeng Deng, Zakir H. Talpur, Kaijun Wang, Yan Kang, Yiping Du, Dongmei Xu, Xinglong Fan, Wei Li , “SERS determination of sodium saccharin content on the tipping paper of cigarettes using AgNP substrates prepared with a USB-power supply device”, Anal. Methods, 2023,15, 4524- 4532
  2. Zhenzhen Xu, Zakir H. Talpur, Wuye Yang, Yinran Xiong, Ting Wu, Yuqi Zhang, Xinyi Shen, Yiping Du, “Dual-spectrum online monitoring of puerarin and total flavonoids contents during the extraction process of Pueraria lobata”, Talanta 248 (2022) 123608
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