title: Simultaneous enantioselective determination of triadimefon and its metabolite triadimenol in edible vegetable oil by gel permeation chromatography and ultraperformance convergence chromatography/tandem mass spectrometry.
abstract: A novel, sensitive, and efficient enantioselective method for the determination of triadimefon and its metabolite triadimenol in edible vegetable oil, was developed by gel permeation chromatography and ultraperformance convergence chromatography/tandem triple quadrupole mass spectrometry. After the vegetable oil samples were prepared using gel permeation chromatography, the eluent was collected, evaporated, and dried with nitrogen gas. The residue was redissolved by adding methanol up to a final volume of 1 mL. The analytes of six enantiomers were analyzed on Chiralpak IA-3 column (150 × 4.6 mm) using compressed liquid CO2-mixed 14 % co-solvents, comprising methanol/acetonitrile/isopropanol = 20/20/60 (v/v/v) in the mobile phase at 30 °C, and the total separation time was less than 4 min at a flow rate of 2 mL/min. Quantification was achieved using matrix-matched standard calibration curves. The overall mean recoveries for six enantiomers from vegetable oil were 90.1-97.3 %, with relative standard deviations of 0.8-5.4 % intra-day and 2.3-5.0 % inter-day at 0.5, 5, and 50 μg/kg levels. The limits of quantification were 0.5 μg/kg for all enantiomers based on five replicate extractions at the lowest fortified level in vegetable oil. Moreover, the absolute configuration of six enantiomers had been determined based on comparisons of the vibrational circular dichroism experimental spectra with the theoretical curve obtained by density functional theory calculations. Application of the proposed method to the 40 authentic vegetable oil samples from local markets suggests its potential use in enantioselective determination of triadimefon and triadimenol enantiomers. Graphical Abstract Chemical structures and UPC(2)-MS/MS separation chromatograms of triadimefon and triadimenol.
authors.affiliation: Institute of Quality and Standard for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|MOA Key Laboratory for Pesticide Residue Detection, Hangzhou, 310021, China.|Zhejiang Citrus Research Institute, Zhejiang Academy of Agricultural Sciences, Taizhou, 318020, China.|College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, 310014, China.
authors.forename: Zhoulin
authors.initials: Z
authors.lastname: Yao
authors.affiliation: Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, 200032, China.
authors.forename: Xiaoge
authors.initials: X
authors.lastname: Li
authors.affiliation: College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, 310014, China.
authors.forename: Yelong
authors.initials: Y
authors.lastname: Miao
authors.affiliation: Zhejiang Citrus Research Institute, Zhejiang Academy of Agricultural Sciences, Taizhou, 318020, China.
authors.forename: Mei
authors.initials: M
authors.lastname: Lin
authors.affiliation: Institute of Quality and Standard for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|MOA Key Laboratory for Pesticide Residue Detection, Hangzhou, 310021, China.
authors.forename: Mingfei
authors.initials: M
authors.lastname: Xu
authors.affiliation: Institute of Quality and Standard for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China.|MOA Key Laboratory for Pesticide Residue Detection, Hangzhou, 310021, China.
authors.forename: Qiang
authors.initials: Q
authors.lastname: Wang
authors.affiliation: Institute of Quality and Standard for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China. zhanghu@mail.zaas.ac.cn.|State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Zhejiang Academy of Agricultural Sciences, Hangzhou, 310021, China. zhanghu@mail.zaas.ac.cn.|MOA Key Laboratory for Pesticide Residue Detection, Hangzhou, 310021, China. zhanghu@mail.zaas.ac.cn.
authors.forename: Hu
authors.initials: H
authors.lastname: Zhang
mesh_terms: D002850:Chromatography, Gel / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005659:Fungicides, Industrial / Q000032:analysis* / Q000378:metabolism*; D057230:Limit of Detection; D008958:Models, Molecular; D010938:Plant Oils / Q000032:analysis*; D013237:Stereoisomerism; D053719:Tandem Mass Spectrometry / Q000379:methods; D014230:Triazoles / Q000032:analysis* / Q000378:metabolism*
chemical_list: D005659:Fungicides, Industrial; D010938:Plant Oils; D014230:Triazoles; C032910:triadimefon
keywords: Absolute configuration; Gel permeation chromatography; Stereoisomeric separation; Triadimefon; Triadimenol; UPC2-MS/MS