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Analysis of Propylen Chlorohydrin in Hydroxypropyl Distarch Phosphate by Accelerated Solvent Extractor (ASE)

가속화용매추출기를 이용한 히드록시프로필인산이전분의 프로필렌클로로히드린 분석방법에 관한 연구

  • Lee, Myung-Ja (Test & Analytical Lab., Pusan Regional Food & Drug Administration) ;
  • Sin, Yeong-Min (Test & Analytical Lab., Pusan Regional Food & Drug Administration) ;
  • Jeong, Eui-Han (Test & Analytical Lab., Pusan Regional Food & Drug Administration) ;
  • Choi, Tae-Jin (Dept. of Microbiology, Pukyong National University) ;
  • Chung, Sook-Hyun (Dept. of Food Biotechnology, Dongseo University) ;
  • An, Won-Gun (Dept. of Biology, Kyungpook National University)
  • 이명자 (부산지방식품의약품안전철 시험분석실) ;
  • 신영민 (부산지방식품의약품안전철 시험분석실) ;
  • 정의한 (부산지방식품의약품안전철 시험분석실) ;
  • 최태진 (부경대학교 미생물학과) ;
  • 정숙현 (동서대학교 식품생명공학과) ;
  • 안원근 (경북대학교 생물학과)
  • Published : 2002.08.01

Abstract

Accelerated solvent extraction (ASE) was used for a rapid and simple extraction of propylenchlorohydrin (PCH) residue in hydroxylpropyl modified starch. The effects of temperature, pressure and extraction solvent on the extraction efficiency were investigated to find the optimal condition of ASE. The optimal conditions for PCH extraction in hydroxylpropyl modified starch were static time of 50 min, purge time of 300 sec, heating time of 5min, temperature of 12$0^{\circ}C$, pressure of 2500 psi, flush (%) with 100 volumes, and ethylacetate as an extraction solvent. The recovery (96.1%) of this method was higher than that (76.4%) of Code of Food Additive. Therefore, the ASE was a good method in both aspects of efficiency and effectiveness.

염소를 함유한 알콜류의 추출 및 분석은 일반적인 알콜류에 비해 비등점이 높아 휘발 또는 증류법을 적용하기 어렵고 특히 히드록시프로필치환전분 중 PCH의 추출은 전분입자와의 에멀션을 형성하므로 어려움이 있다. 따라서 용매를 가온, 가압하여 추출효율을 높이고, 전분의 물성적인 특성으로 인한 여과의 어려움을 해소할 수 있는 가속용매추출기 (ASE)를 사용하여 PCH 분석을 하였다. 온도 40~15$0^{\circ}C$의 변화에 따른 회수율을 측정한 결과 온도 상승에 따라 회수율이 증가하는 경향을 나타내어 12$0^{\circ}C$에서는 96.1%의 회수율을 나타내었다. 압력 변화에 따른 추출효율을 검토한 결과 1500 psi까지는 압력 상승에 따른 회수율의 증가가 뚜렷하여 93.6%였으나 이후에는 완만하게 증가하여 2500 psi에서는 96.1%로 나타났다. 추출용매(초산에틸, 메탄올, 아세톤, 디에틸에테르 및 핵산)에 따른 PCH의 회수율을 측정한 결과 아세톤, 디에틸에테르, 초산에틸은 94% 이상의 회수율을 나타내었고 메탄올 87.3%, 핵산 14.1%로 나타났다. RSD(%)는 초산에틸이 5.6%로 가장 우수하였다. ASE를 이용한 히드록시프로필치환 전분 중 PCH의 최적 추출조건은 온도, 12$0^{\circ}C$; 압력, 2500 psi; 추출용매, 초산에틸, static time, 50분; purge time, 300초; heating time, 5분; flush(%), 100 mL였으며, 이때 회수율은 96.1%이었다.

Keywords

References

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