Analysis of acidic herbicides in water and soil by using isotope dilution GC-MS/MS

Title
Analysis of acidic herbicides in water and soil by using isotope dilution GC-MS/MS
Authors
정선아김승기표희수
Issue Date
2013-05
Publisher
한국분석과학회
Abstract
2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) are chlorophenoxyacetic acid herbicides used to defoliate broadleaf plants. In the present study, a method was developed to determine of 2,4-D and 2,4,5-T in ground water and soil using gas chromatography-tandem mass spectrometry (GC-MS/MS). In order to increase the recovery percentage, extraction using ether of a solvent was repeated twice and trifluoroaceticanhydride/trifluoroethanol (TFAA/TFE) derivatization was selected. Isotope labeled internal standards of each analytes, 2,4-D(13C6) and 2,4,5-T(13C6) are used to perform qualitiative analysis. The analysis using GC-MS/MS is validated by the analysis of standard spiked water and of standard spiked soil. Instrument detection limit (IDL) of 2,4-D and 2,4,5-T are both 0.5ng/L. Inthewater, method detection limit (MDL) of 2,4-D and 2,4,5-T are 1.36 ng/L and 1.72 ng/L. In the soil, MDL of 2,4-D and 2,4,5-T are 0.13 ng/g and 0.24 ng/g, respectively. The precision results of 2,4-D and 2,4,5-T ranged from 4.32 % to 5.47 % in the water and ranged from 4.27 % to 7.50 % in the soil. The accuracy results of 2,4-D and 2,4,5-T ranged 101.82 % to 107.27 % in the water, ranged from 104.42 % to 96.41 % in the soil. Recoveries were estimated by internal standard that added to samples. The recovery of internal standard from water ranged from 79.1 % - 109.7 % and that from soil ranged 53.2 % - 119.4 %. From the above, analysis of 2,4-D and 2,4,5-T using GC-MS/MS can detect very low concentration of acid herbicides in ground water and soil. This study of acid herbicides analysis of the existing high reproducibility and low detection limits were complementary, and the accurate and precise analysis of the samples is possible.
URI
http://pubs.kist.re.kr/handle/201004/44925
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KIST Publication > Conference Paper
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