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


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.


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

SPGHB5_2019_v51n1_12_f0001.png 이미지

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.

SPGHB5_2019_v51n1_12_f0002.png 이미지

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.

SPGHB5_2019_v51n1_12_f0003.png 이미지

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

SPGHB5_2019_v51n1_12_t0001.png 이미지

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

SPGHB5_2019_v51n1_12_t0002.png 이미지

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

SPGHB5_2019_v51n1_12_t0003.png 이미지


Supported by : 강원대학교


  1. Bieber TI, Trehy ML. Dihaloacetonitriles in chlorinated natural waters. Vol. 4, pp. 85-96. In: Water Chlorination-Environmental Impact and Health Effects. Jolley RJ, Brungs WA, Cotruvo JA, Cumming RB, Mattice JS, Jacobs VA (ed.) Ann Arbor Science Publisher, Ann Arbor, MI, USA (1983)
  2. Cardador MJ, Gallego M. Effect of the chlorinated washing of minimally processed vegetables on the generation of haloacetic acids. J. Agr. Food Chem. 60: 7326-7332 (2012)
  3. Cardador MJ, Gallego M. Static headspace-gas chromatography-mass spectrometry for the simultaneous determination of trihalomethanes and haloacetic acids in canned vegetables. J. Chromatogr. A 1454: 9-14 (2016)
  4. Coroneo V, Carraro V, Marras B, Marrucci A, Succa S, Meloni B, Pinna A, Angioni A, Sanna A, Schintu M. Presence of trihalomethanes in ready-to-eat vegetables disinfected with chlorine. Food Addit. Contam. Part A 34: 2111-2117 (2017)
  5. Huang AT, Batterman S. Sorption of trihalomethanes in foods. Environ. Int. 36: 754-762 (2010)
  6. Jo MJ, Jeong A-R, Kim HJ, Lee N, Oh SW, Kim YJ, Chun HS, Koo M. Microbiological quality of fresh-cut produce and organic salads. Kor. J. Food Sci. Technol. 43: 91-97. (2011)
  7. Jung S, Kim D, Lee G, Yun SS, Lim HS, Jung YR, Kim H. Evaluation of measurement uncertainty for quantitative determination of chlorite and chlorate in fresh-cut vegetables using ion chromatography. Korean J. Food Sci. Technol. 49: 591-598 (2017)
  8. Kang TM, Cho S-K, Park JY, Song KB, Chung MS, Park JH. Analysis of microbial contamination of sprouts and fresh-cut salads in a market. Korean J. Food Sci. Technol. 43: 490-494 (2011)
  9. Kim DS, Jung S, Lee G, Yun SS, Lim HS, Kim H. Ion chromatographic determination of chlorite and chlorate in chlorinated food using a hydroxide eluent. Anal. Sci. Technol. 30: 57-67 (2017)
  10. Kim HY, Oh SW, Chung SY, Choi SH, Lee JW, Yang JW, Seo EC, Kim YH, Park HO, Yang CY, Ha SC, Shin IS. An investigation of microbial contamination of ready-to-eat products in Seoul, Korea. Korean J. Food Sci. Technol. 43: 39-44 (2011)
  11. Korea Food & Drug Administration (KFDA). Suggestion of Safety Management for Residual Chlorine Products in Fresh-Cut-Foods. Osong, Korea (2008)
  12. Korea Food & Drug Administration (KFDA). Guidelines for the Validation of Test Methods for Pharmaceuticals, etc. Osong, Korea (2012)
  13. Ministry of Environment (MOE). Haloacetic Acids-Gas Chromatograph-Mass Spectrometry. ES05552.1a, Sejong, Korea (2012a)
  14. Ministry of Environment (MOE). Haloacetic Acids-Gas Chromatography. ES05552.2a, Sejong, Korea (2012b)
  15. Ministry of Food and Drug Safety (MFDS). Korean Food Additives Codex-5. Usage Criteria by Item. Available from: Accessed Dec. 11, 2018
  16. Olmez H, Kretzschmar U. Potential alternative disinfection methods for organic fresh-cut industry for minimizing water consumption and environmental impact. LWT Food Sci. Technol. 42: 686-693 (2009)
  17. Rivier L. Criteria for the identification of compounds by liquid chromatography-mass spectrometry and liquid chromatography-multiple mass spectrometry in forensic toxicology and doping analysis. Anal. Chim. Acta 492: 69-82 (2003)
  18. Sadiq R, Rodriguez MJ. Disinfection by-products (DBPs) in drinking water and predictive models for their occurrence: a review. Sci. Total Environ. 321: 21-46 (2004)
  19. Schony R. Disinfection by-products: a question of balance. Environ. Health Persp. 118: A466-467 (2010)
  20. Tan H, Sen AC, Wheeler WB, Cornell JA, Wei CI. A kinetic study of the reaction of aqueous chlorine and chlorine dioxide with amino acids, peptides and proteins. J. Food Sci. 52: 1706-1711 (1987)
  21. U.S. Environmental Protection Agency (U.S. EPA). Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Microextraction, Derivatization, and Gas Chromatography with Electron Capture Detection. EPA 815-B-03-002, Washington DC, USA (2003)
  22. U.S. Environmental Protection Agency (U.S. EPA). Available from: Accessed Dec. 11 (2018a)
  23. U.S. Environmental Protection Agency (U.S. EPA). Available from: Accessed Dec. 11 (2018b)