title: A statistical approach to determine fluxapyroxad and its three metabolites in soils, sediment and sludge based on a combination of chemometric tools and a modified quick, easy, cheap, effective, rugged and safe method.
abstract: An effective method for the quantification of fluxapyroxad and its three metabolites in soils, sediment and sludge was developed using ultrahigh performance chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). Both the extraction and clean-up steps of the QuEChERS procedure were optimised using a chemometric tool, which was expected to facilitate the rapid analysis with minimal procedures. Several operating parameters (MeCN/acetic acid ratio in the extraction solution (i.e., acetic acid percentage), water volume, extraction time, PSA amount, C18 amount, and GCB amount) were investigated using a Plackett-Burman (P-B) screening design. Afterward, the significant factors (acetic acid percentage, water volume, and PSA amount) obtained were optimised using central composite design (CCD) combined with the desirability function (DF) to determine the optimum experimental conditions. The optimised procedure provides high-level linearity for all studied compounds with correlation coefficients ranging between 0.9972 and 0.9999. The detection limits were in the range of 0.1 to 1.0μg/kg and the limits of quantitation (LOQs) were between 0.5 and 3.4μg/kg with relative standard deviations (RSD) between 2.3% and 9.6% (n=6). Therefore, the developed protocol can serve as a simple and sensitive tool for monitoring fluxapyroxad and its three metabolites in soil, sediment and sludge samples.
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
authors.forename: Shasha
authors.initials: S
authors.lastname: Li
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China. Electronic address: liuxingang@caas.cn.
authors.forename: Xingang
authors.initials: X
authors.lastname: Liu
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
authors.forename: Yulong
authors.initials: Y
authors.lastname: Zhu
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
authors.forename: Fengshou
authors.initials: F
authors.lastname: Dong
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
authors.forename: Jun
authors.initials: J
authors.lastname: Xu
authors.affiliation: Institute of Agro-products Processing Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China.
authors.forename: Minmin
authors.initials: M
authors.lastname: Li
authors.affiliation: State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing 100193, PR China. Electronic address: zhengyongquan@ippcaas.cn.
authors.forename: Yongquan
authors.initials: Y
authors.lastname: Zheng
mesh_terms: D000577:Amides / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000191:economics; D003627:Data Interpretation, Statistical; D019015:Geologic Sediments / Q000032:analysis*; D057230:Limit of Detection; D012722:Sewage / Q000032:analysis*; D012984:Software; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods; D014867:Water / Q000737:chemistry
chemical_list: D000577:Amides; D012722:Sewage; D012987:Soil; D012989:Soil Pollutants; D014867:Water; C000591719:fluxapyroxad
keywords: Experimental design; Fluxapyroxad; Metabolites; Sediment; Sludge; Soils