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Eco-Friendly Miniaturized Solid Phase Microextraction for Pesticide Analysis in Grapes
Mereke Alimzhanova1, Yerkanat Syrgabek1,2, Pedro Antonio Garcia Encina3
1Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, Almaty, Kazakhstan.
Journal of Separation Science
|July 1, 2025
Summary
A new miniaturized headspace solid-phase microextraction (Mini-HS-SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) efficiently detects ten pesticides in grapes. This environmentally friendly technique offers accurate quantification for food safety.
Area of Science:
- Analytical Chemistry
- Environmental Science
- Food Safety
Background:
- Pesticide residues in food pose significant health risks.
- Accurate and sensitive detection methods are crucial for monitoring.
- Existing methods may lack environmental friendliness or miniaturization.
Purpose of the Study:
- To develop a simple, environmentally friendly, and miniaturized method for pesticide analysis in grapes.
- To identify and quantify ten specific pesticides using Mini-HS-SPME and GC-MS.
- To validate the method's performance and evaluate its environmental impact.
Main Methods:
- Miniaturized headspace solid-phase microextraction (Mini-HS-SPME) technique.
- Gas chromatography-mass spectrometry (GC-MS) for detection and quantification.
- Optimization of extraction parameters (temperature, time, fiber, pH, salt, sample volume).
Main Results:
- Successful identification and quantification of ten pesticides in grape samples.
- Optimized conditions: 200 µL sample, PDMS 100 µm fiber, 90°C, 30 min.
- Validated method with linearity (5-1000 ng mL⁻¹), good recovery, and accuracy.
- Low limits of detection (0.09-3.0 ng mL⁻¹) and quantification (0.2-10.1 ng mL⁻¹).
Conclusions:
- The developed Mini-HS-SPME-GC-MS method is effective for pesticide analysis in grapes.
- The method is miniaturized, environmentally friendly, and suitable for practical application.
- Evaluation using GAPI, AGREEprep, and BAGI tools confirms its applicability and eco-friendliness.

