2026/07/25 by Ronald Borja, Ronald F. Borja, Antonio Cascajosa-Lira +8
Agricultural and Biological Sciences · Biochemistry, Genetics and Molecular Biology · Environmental Science · #Aquatic Ecosystems and Phytoplankton Dynamics #Bacterial Identification and Susceptibility Testing #Cylindrospermopsin #Extraction (chemistry) #Liquid–liquid extraction #Pesticide Residue Analysis and Safety #Quantitative analysis (chemistry) #Urine
paper · doi:10.1016/j.microc.2026.119204
published in Microchemical Journal 228, 119204 (Elsevier BV)
openalex publication_date 2026/07/25 · crossref created 2026/07/25 · openalex created_date 2026/07/26 · openalex updated_date 2026/07/30 · crossref deposited 2026/07/30 · crossref indexed 2026/07/30 · crossref issued 2026/09/01 · crossref published 2026/09/01 · crossref published-print 2026/09/01
Cylindrospermopsin (CYN) is an emerging cyanotoxin of public health concern due to its widespread occurrence and multiple toxic effects. Reliable analytical methods for its detection in biological matrices are essential for toxicokinetic and exposure studies, yet validated approaches remain limited. The aim of this study was to develop, to the best our knowledge, the first fully validated solid-phase extraction (SPE) method with Ultra-High-Performance Liquid Chromatography coupled with Tandem Mass Spectrometry (UHPLC-MS/MS) for the detection and quantification of CYN in serum and urine. The method included systematic evaluation of matrix-specific preparation steps, including precipitation, pH, centrifugation, followed by SPE with graphitized carbon cartridges. The method showed excellent linearity (1–500 μg L −1 ), high sensitivity, and low limits of detection (LOD) and quantification (LOQ): 0.010 μg L −1 and 0.034 μg L −1 in serum, and 0.012 μg L −1 and 0.040 μg L −1 in urine, and minimal matrix effects, ensuring reliable quantification in serum and urine. Recovery values ranged from 94.52% to 101.71% (serum), and from 74.96% to 98.81% (urine); and these values, as well as the precision data obtained, met AOAC criteria across all concentrations, outperforming previous attempts due to key extraction improvements. Robustness of the method was also confirmed. Additionally, it has been effectively applied for the extraction and quantification of CYN in serum and urine samples from Wistar rats orally or intraperitoneally exposed to CYN in the laboratory. Overall, the method provides a sensitive and reliable tool for toxicokinetic studies, enabling accurate assessment of CYN exposure in biological matrices.