A Highly Sensitive Method for the Determination of Thiophanate Methyl, Cyromazine, and Their Metabolites in Edible Fungi
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A Highly Sensitive Method for the Determination of Thiophanate Methyl, Cyromazine, and Their Metabolites in Edible Fungi by Ultra-Performance Liquid Chromatography Using Accelerated Solvent Extraction and Cleanup with Solid-Phase Extraction Xingqiang Wu & Xusheng Ge & Shuxuan Liang & Hanwen Sun
Received: 14 April 2013 / Accepted: 5 July 2013 # Springer Science+Business Media New York 2013
Abstract A highly sensitive ultra-performance liquid chromatographic method with diode-array detection was developed for residue determination of thiophanate methyl (TM), cyromazine (CYR), and their metabolites, carbendazim (MBC) and melamine (MEL). Edible fungi samples were treated using accelerated solvent extraction (ASE) followed by cleanup with solid-phase extraction (SPE). Under optimized conditions, good linearity was achieved with a correlation coefficient (r2) of ≥0.9998. The limit of quantification was 0.36, 0.24, 0.4, and 0.5 μg kg−1 for MEL, CYR, MBC, and TM, respectively. The intra- and interday precisions (in terms of the relative standard deviation (RSD)) of the four analytes were in the range of 2.3–4.5 and 3.1–6.3 %, respectively. The recoveries for TM, MBC, CYR, and MEL in four edible fungi samples at three spiked levels of 0.6, 6, and 20 μg kg−1 for TM and MBC and 0.4, 4, and 20 μg kg−1 for CYR and MEL were in the range of 82–105 % with RSDs below 5.6 %. The proposed method can be used for the routine determination of CYR and MEL in edible fungi with high sensitivity and accuracy as well as low consumption of reagents. Keywords Ultra-performance liquid chromatography . Accelerated solvent extraction . Solid-phase extraction . Thiophanate methyl . Cyromazine . Metabolite . Edible fungi X. Wu : X. Ge : S. Liang : H. Sun (*) College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China e-mail: [email protected] X. Ge Biochemical Department of Baoding University, Baoding 071000, China
Introduction Edible fungi have nourishing and hygienical function. They are often used to reduce the blood pressure to appropriate level, lower blood cholesterol level, and enhance human immunity, deeply loved by the vast number of consumers. The use of edible fungis gets more and more attention because of their medicinal and nutrient value. However, there are some potential security risks of pesticide residues in edible fungi because of its own characteristics and some aspects of illegal operations in planting, the product deep-processing and circulation. Thiophanate methyl (TM) and its metabolite, carbendazim (MBC) are applied at different growing stages to control fungal diseases in edible fungi. TM and MBC could cause endocrine disruption, embryotoxic and teratogenic effects (Yang et al. 2011). Cyromazine (CYR) is a triazine pesticide used for fly control in crop production and animal feed, by inhibiting insect growth. Melamine (MEL) is a metabolite of CYR and formed via dealkylation reactions in both plants and animals (Cook and Hut
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