title: Determination of pyrazole and pyrrole pesticides in environmental water samples by solid-phase extraction using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography.
abstract: A solid-phase extraction (SPE) method using multi-walled carbon nanotubes as adsorbent coupled with high-performance liquid chromatography was developed for the determination of four pyrazole and pyrrole pesticides (fenpyroximate, chlorfenapyr, fipronil and flusilazole) in environmental water samples. Several parameters, such as extraction adsorbent, elution solvent and volume and sample loading flow rate were optimized to obtain high SPE recoveries and extraction efficiency. The calibration curves for the pesticides extracted were linear in the range of 0.05-10 μg L(-1) for chlorfenapyr and fenpyroximate and 0.05-20 μg L(-1) for fipronil and flusilazole, with the correlation coefficients (r(2)) between 0.9966 and 0.9990. The method gave good precisions (relative standard deviation %) from 2.9 to 10.1% for real spiked samples from reservoir water and seawater; method recoveries ranged 92.2-105.9 and 98.5-103.9% for real spiked samples from reservoir water and seawater, respectively. Limits of detection (S/N = 3) for the method were determined to be 8-19 ng L(-1). The optimized method was successfully applied to the determination of four pesticides of pyrazoles and pyrroles in real environmental water samples.
authors.affiliation: Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China majiping2012@163.com majiping2001@aliyun.com.
authors.forename: Jiping
authors.initials: J
authors.lastname: Ma
authors.affiliation: Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China.
authors.forename: Xi
authors.initials: X
authors.lastname: Lu
authors.affiliation: Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China.
authors.forename: Yan
authors.initials: Y
authors.lastname: Xia
authors.affiliation: Key Laboratory of Environmental Engineering in Shandong Province, Institute of Environmental and Municipal Engineering, Qingdao Technological University, Qingdao 266033, China.
authors.forename: Fengli
authors.initials: F
authors.lastname: Yan
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D060766:Drinking Water / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D037742:Nanotubes, Carbon / Q000737:chemistry; D010575:Pesticides / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D011720:Pyrazoles / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D011758:Pyrroles / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D060766:Drinking Water; D037742:Nanotubes, Carbon; D010575:Pesticides; D011720:Pyrazoles; D011758:Pyrroles; D014874:Water Pollutants, Chemical; C031280:pyrazole