title: Development of a single-run analytical method for the detection of ten multiclass emerging contaminants in agricultural soil using an acetate-buffered QuEChERS method coupled with LC-MS/MS.
abstract: This study was undertaken to develop and validate a single multiresidue method for the monitoring of ten multiclass emerging contaminants, viz. ceftiofur, clopidol, florfenicol, monensin, salinomycin, sulfamethazine, sulfathiazole, sulfamethoxazole, tiamulin, and tylosin in agricultural soil. Samples were extracted using an acetate-buffered, modified quick, easy, cheap, effective, rugged, and safe method followed by liquid chromatography with tandem mass spectrometric analysis in positive ion mode. Separation on an Eclipse Plus C18column was conducted in gradient elution mode using a mobile phase of methanol (A) and distilled water (B), each containing 0.1% formic acid and 5 mM ammonium formate. The linearity of the matrix-matched calibrations, expressed as determination coefficients, was good, with R2≥ 0.9908. The limits of quantification were in the range 0.05-10 μg/kg. Blank soil samples spiked with 4 × and 20 × the limit of quantification provided recovery rates of 60.2-120.3% (except sulfamethoxazole spiked at 4 × the limit of quantification, which gave 131.9%) with a relative standard deviation < 13% (except clopidol spiked at 20 × the limit of quantification, which gave 25.2%). This method was successfully applied to the monitoring of 51 field-incurred agricultural loamy-sand soil samples collected from 17 provincial areas throughout the Korean Peninsula. The detected and quantified drugs were clopidol (≤ 4.8 μg/kg), sulfathiazole (≤ 7.7 μg/kg), sulfamethazine (≤ 6.6 μg/kg), tiamulin (≤ 10.0 μg/kg), and tylosin (≤ 5.3 μg/kg). The developed method is simple and versatile, and can be used to monitor various classes of veterinary drugs in soil.
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Young-Jun
authors.initials: YJ
authors.lastname: Lee
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Jeong-Heui
authors.initials: JH
authors.lastname: Choi
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.|Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, Giza, Egypt.
authors.forename: A M
authors.initials: AM
authors.lastname: Abd El-Aty
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Hyung Suk
authors.initials: HS
authors.lastname: Chung
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Han Sol
authors.initials: HS
authors.lastname: Lee
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Sung-Woo
authors.initials: SW
authors.lastname: Kim
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Md Musfiqur
authors.initials: MM
authors.lastname: Rahman
authors.affiliation: Chemical Safety Division, Department of Agro-Food Safety and Crop Protection, National Institute of Agricultural Science, Wanju, Republic of Korea.
authors.forename: Byung-Jun
authors.initials: BJ
authors.lastname: Park
authors.affiliation: School of Applied Biosciences, Kyungpook National University, Daegu, Republic of Korea.
authors.forename: Jang-Eok
authors.initials: JE
authors.lastname: Kim
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.
authors.forename: Ho-Chul
authors.initials: HC
authors.lastname: Shin
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Buk-gu, Gwangju, Republic of Korea.
authors.forename: Jae-Han
authors.initials: JH
authors.lastname: Shim
mesh_terms: D000085:Acetates / Q000737:chemistry; D002853:Chromatography, Liquid; D004784:Environmental Monitoring / Q000379:methods*; D057230:Limit of Detection; D056910:Republic of Korea; D012987:Soil / Q000737:chemistry*; D012989:Soil Pollutants / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D019155:Veterinary Drugs / Q000032:analysis
chemical_list: D000085:Acetates; D012987:Soil; D012989:Soil Pollutants; D019155:Veterinary Drugs
keywords: Acetate-buffer extraction method; Agricultural soil; Quantification; Tandem mass spectrometry; Veterinary drugs