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J Korean Soc Environ Eng > Volume 37(5); 2015 > Article
J Korean Soc Environ Eng 2015;37(5): 262-268. doi: https://doi.org/10.4491/KSEE.2015.37.5.262
MEPS-GC/MS를 이용한 농약류 동시 수질분석
이기창1, 이원태2
1경상북도보건환경연구원
2금오공과대학교 환경공학전공
Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent
Ki-chang Lee1, Wontae Lee2
1Gyeongsangbuk-do Institute of Health and Environment
2Department of Environmental Engineering, Kumoh National Institute of Technology
Corresponding author  Wontae Lee ,Tel: 054-478-7636, Fax: 054-478-7859, Email: wtlee@kumoh.ac.kr
Received: March 18, 2015;  Revised: April 13, 2015;  Accepted: May 15, 2015.  Published online: May 31, 2015.
ABSTRACT
This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using 30 µL of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and 0.08~0.59 µg/L, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of 0.5~5.0 µg/L. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.
Key Words: Organochlorine Pesticides, Carbaryl, Micro Extraction by Packed Sorbent (MEPS), Polystyrene Divinylbenzene (PDVB), Gas Chromatography Mass Spectrometry, Limit of Quantification
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