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Determination of dichloroacetic acid and trichloroacetic acid in fresh-cut salads using gas chromatography-mass spectrometry

GC-MS를 이용한 신선편의 샐러드 중 dichloroacetic acid와 trichloroacetic acid의 분석

  • Kim, Hekap (School of Natural Resources and Environmental Science, Kangwon National University) ;
  • Lee, Seong-gyun (Department of Environmental Science, Kangwon National University) ;
  • Yun, A-hyeon (Department of Paper Science and Engineering, Kangwon National University)
  • 김희갑 (강원대학교 농업생명과학대학 환경융합학부) ;
  • 이성균 (강원대학교 자연과학대학 환경학과) ;
  • 윤아현 (강원대학교 산림환경과학대학 제지공학과)
  • Received : 2018.12.12
  • Accepted : 2019.01.21
  • Published : 2019.02.28

Abstract

Dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA) in fresh-cut salads available from the market were determined by gas chromatography-mass spectrometry (GC-MS). The target compounds in 3 g of acidified homogenates were extracted with 20 mL of methyl t-butyl ether (MTBE). The extract was concentrated to 1 mL and heated for 1 h at $55^{\circ}C$. The analytes were separated using a DB-1701 column and detected with a mass spectrometer. The method detection limit was approximately $6{\mu}g/kg$, and both analytical accuracy and precision were found to be satisfactory. The linearity of the calibration curves expressed as the coefficients of determination was >0.996. The analysis of seven samples using the established method showed that the four samples contained considerable amounts of analytes ($25.4-31.2{\mu}g/kg$ of DCAA and $18.8-46.1{\mu}g/kg$ of TCAA). These results raised a concern about the impact of fresh-cut salad consumption on human health.

Keywords

Dichloroacetic acid;fresh-cut salad;GC-MS;trichloroacetic acid

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Fig. 1. Comparison of peak resolutions between DB-5MS (top, 100 µg/kg) and DB-1701 (bottom, 75 µg/kg) columns. Peak resolution was increased by using the DB-1701 column.

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Fig. 2. Formation of dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA) in fresh-cut vegetables following disinfection with NaClO (100 mg/L Cl2) for 5 min.

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Fig. 3. Calibration curves for determination of dichloroacetic acid (DCAA; left) and trichloroaceetic acid (TCAA; right).

Table 1. Operating conditions of gas chromatograph-mass spectrometer

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Table 2. Method detection limits (MDL), limits of quantitation(LOQ), repeatability (relative standard deviation; RSD), and recovery for dichloroacetic acid (DCAA) and trichloroaceticacid (TCAA)

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Table 3. Ingredient contents and concentrations of dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA) in retail packagedready-to-eat salads

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Acknowledgement

Supported by : 강원대학교

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