Determination of Sulfur Dioxide in Pickles by Acid Distillation-HPLC Method and Monnier Williams Modified Method

산증류-HPLC법과 모니어윌리암스변법을 이용한 절임류중의 이산화황 함량 분석

  • Jung, So-Young (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Il-Young (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Sung-Dan (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jang, Mi-Ra (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chang, Min-Su (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Han, Ki-Young (Food Additives Team, Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 정소영 (서울특별시보건환경연구원 첨가물검사팀) ;
  • 김일영 (서울특별시보건환경연구원 첨가물검사팀) ;
  • 김성단 (서울특별시보건환경연구원 첨가물검사팀) ;
  • 장미라 (서울특별시보건환경연구원 첨가물검사팀) ;
  • 장민수 (서울특별시보건환경연구원 첨가물검사팀) ;
  • 한기영 (서울특별시보건환경연구원 첨가물검사팀)
  • Published : 2003.12.01

Abstract

To assess accurate methods for measuring sulfur dioxide residue in pickles, the acid distillation HPLC-UV method and Monnier Willams modified method were examined. By the acid distillation HPLC-UV method, sulfites released from pickles by acid distillation were absorbed in 1% triethanolamine solution and detected as sulfite ion by HPLC with UV monitoring at 240nm. An anion exchange column was employed with 1.8mM $Ma_2CO_3-1.7mM\;NaHCO_3$ solution as a mobile phase, $84.0{\sim}91.7%$ of sulfite added to pickled radish were recovered. Total sulfite levels from 48 kinds of pickles analyzed by acid distillation HPLC-UV was compared with those analyzed by the Monnier Williams modified method. The Monnier Williams modified method showed higher levels of sulfur dioxide than the acid distillation HPLC-UV method due to the presence of volatile acids in pickles. The concentration of sulfur dioxide was in the range of $N.D{\sim}173.05ppm$ in pickled radish and over 30ppm of sulfur dioxide from 3 samples by the acid distillation-HPLC-UV method.

절임류에 함유된 이산화황함량의 정확한 분석을 위해 산 증류후 HPLC-UV detector를 이용한 방법과 Monnier-Williams변법으로 실험해보았다. 산증류-HPLC-UV법은 절임류중의 아황산염을 산증류 시킨 후 발생하는 이산화황을 1% triethanolamine용액에 흡수시켜 이를 UV 240nm에서 정량하는 것으로서, 고정상은 음이온 교환컬럼을, 이동상으로는 1.8mM $Na_2Co_3$와 1.7mM $NaHCO_3$용액을 사용하였다. 이 방법으로 단무지에 아황산염을 첨가하여 실험 한 결과 $84.0{\sim}91.7%$의 회수율을 얻었다. 시중에 유통되는 48종의 절임류에 대해 모니어윌리암스변법과 산증류-HPLC-UV법을 이용하여 이산화황 함량을 조사해본 결과, 산증류-HPLC-UV법에 비해 모니어월리암스법에서 휘발성 산으로 인해 높은 농도를 나타내었다. 산증류-HPLC-UV법으로 분석한 절임류의 이산화황 농도는 불검출${\sim}173.05ppm$이었고, 기준인 30ppm을 초과하는 제품은 3건이었다.

Keywords

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