Menthol as a thermoresponsive solvent for solidified organic disk extraction of pesticides from wine
MICROCHEMICAL JOURNAL, cilt.225, 2026 (SCI-Expanded, Scopus)
- Yayın Türü: Makale / Tam Makale
- Cilt numarası: 225
- Basım Tarihi: 2026
- Doi Numarası: 10.1016/j.microc.2026.118274
- Dergi Adı: MICROCHEMICAL JOURNAL
- Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, BIOSIS, Chemical Abstracts Core, Chimica, Index Islamicus, Academic Search Ultimate (EBSCO), Engineering Source (EBSCO)
- Ankara Üniversitesi Adresli: Evet
Özet
The widespread use of pesticides in viticulture may result in the persistence of residue levels throughout the winemaking process, raising significant food-safety concerns given the global consumption of wine. The analytical determination of pesticide residues in wine is particularly challenging because of the matrix complexity and the absence of specific maximum residue limits (MRLs) for the final product. In this study, a novel, solvent-minimized and environmentally sustainable analytical method is proposed for the determination of eight pesticide residues in wine samples. The method integrates ultrasound-assisted emulsive liquid-liquid microextraction (UA-ELLME) with solidified organic disk (SOD) technology, employing menthol as a thermoresponsive extractant. Menthol was selected due to its low toxicity, biodegradability, renewable origin, and unique phase-transition behavior. In the proposed approach, menthol is used in its liquid state to promote efficient analyte partitioning during extraction and subsequently solidified to enable rapid phase separation and simplified extract handling. The entire extraction and clean-up procedure is carried out in a single polypropylene tube, requires only 200 mu L of conventional solvent (2-propanol), and is completed in less than 20 min. Following extraction, analytes were quantified by UHPLC-HRMS. The method was fully validated according to ICH guidelines using matrix-matched calibration. Excellent linearity was achieved for all analytes (R-2 > 0.99) over a working range from the limit of quantification (LOQ) up to 100 mu g L-1. Limits of detection ranged from 0.003 to 1.4 mu g L-1, while LOQs were between 0.009 and 4.8 mu g L-1. Precision and accuracy were satisfactory at all tested concentration levels, with relative standard deviations below 14.1% and relative recoveries within +/- 13.1%. The proposed UA-ELLME-SOD method represents the first application of a menthol-based solidified organic disk system to real sample matrices and offers a robust, rapid, and green alternative for the trace-level determination of pesticide residues in wine.