title: Simultaneous enantioselective determination of fenbuconazole and its main metabolites in soil and water by chiral liquid chromatography/tandem mass spectrometry.
abstract: A novel and sensitive method was developed for the simultaneous determination of fenbuconazole and its main metabolites enantioselectively using chiral liquid chromatography coupled with tandem mass spectrometry. The separation and determination were performed using reversed-phase chromatography on a cellulose chiral stationary phase, a Chiralcel OD-RH (150 mm×4.6 mm) column, under isocratic conditions at 0.5 mL/min flow rate. The effects of three cellulose-based columns and three amylose-based columns on the separation were also investigated. The elution orders of the eluting enantiomers were identified by an optical rotation detector. The QuEChERS (acronym for Quick, Easy, Cheap, Effective, Rugged and Safe) method and solid-phase extraction (SPE) were used for the extraction and clean-up of the soil and water samples, respectively. Parameters including the matrix effect, linearity, precision, accuracy and stability were evaluated. Under optimal conditions, the mean recoveries for all enantiomers from the soil samples were 82.5-104.1% with 2.7-9.5% intra-day relative standard deviations (RSD) and 5.7-11.2% inter-day RSD at 5, 25 and 50 μg/kg levels; the mean enantiomer recoveries from the water samples were 81.8-104.6% with 2.6-11.4% intra-day RSD and 5.3-10.4% inter-day RSD at 0.25, 0.5 and 2.5 μg/L levels. Coefficients of determination R2≥0.9991 were achieved for each enantiomer in the soil and water matrix calibration curves within the range of 1.0-125 μg/L. The limits of detection (LOD) for all enantiomers in the soil and water were less than 0.8 μg/kg, whereas the limit of quantification (LOQ) did not exceed 2.5 μg/kg. The results of the method validation confirm that this proposed method is convenient and reliable for the enantioselective determination of the enantiomers of fenbuconazole and its main metabolites in soil and water.
authors.affiliation: Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing 100193, China.
authors.forename: Yuanbo
authors.initials: Y
authors.lastname: Li
authors.forename: Fengshou
authors.initials: F
authors.lastname: Dong
authors.forename: Xingang
authors.initials: X
authors.lastname: Liu
authors.forename: Jun
authors.initials: J
authors.lastname: Xu
authors.forename: Jing
authors.initials: J
authors.lastname: Li
authors.forename: Zhiqiang
authors.initials: Z
authors.lastname: Kong
authors.forename: Xiu
authors.initials: X
authors.lastname: Chen
authors.forename: Wencheng
authors.initials: W
authors.lastname: Song
authors.forename: Yunhao
authors.initials: Y
authors.lastname: Wang
authors.forename: Yongquan
authors.initials: Y
authors.lastname: Zheng
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005659:Fungicides, Industrial / Q000737:chemistry* / Q000302:isolation & purification; D009570:Nitriles / Q000737:chemistry* / Q000302:isolation & purification; D012680:Sensitivity and Specificity; D012989:Soil Pollutants / Q000737:chemistry* / Q000302:isolation & purification; D013237:Stereoisomerism; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014230:Triazoles / Q000737:chemistry* / Q000302:isolation & purification; D014874:Water Pollutants, Chemical / Q000737:chemistry* / Q000302:isolation & purification
chemical_list: D005659:Fungicides, Industrial; D009570:Nitriles; D012989:Soil Pollutants; D014230:Triazoles; D014874:Water Pollutants, Chemical; C504383:fenbuconazole