Analysis Method Development for Bound-MCPD

3-MCPD 지방산에스테르 분석법

  • Woo, Sung-Min (Imported Food Analysis Division, Center for Food and Drug Analysis, Gyeongin Regional Korea Food&Drug Administration) ;
  • Oh, Jae-Ho (Imported Food Analysis Division, Center for Food and Drug Analysis, Gyeongin Regional Korea Food&Drug Administration) ;
  • Jang, Young-Mi (Imported Food Analysis Division, Center for Food and Drug Analysis, Gyeongin Regional Korea Food&Drug Administration) ;
  • Kim, Mee-Hye (Imported Food Analysis Division, Center for Food and Drug Analysis, Gyeongin Regional Korea Food&Drug Administration)
  • 우성민 (경인지방식품의약품안전청, 수입식품분석과) ;
  • 오재호 (경인지방식품의약품안전청, 수입식품분석과) ;
  • 장영미 (경인지방식품의약품안전청, 수입식품분석과) ;
  • 김미혜 (경인지방식품의약품안전청, 수입식품분석과)
  • Received : 2010.09.15
  • Accepted : 2010.10.27
  • Published : 2010.12.31

Abstract

Toxicity of 3-MCPD that comes from food manufacture and processing is well-known. Recent studies reported that 3-MCPD fatty acid ester which is formed by metabolic material was 10~2000 times as much as 3-MCPD in food. This study made analysis method of 3-MCPD fatty acid esters by recent research and laboratory work, and determined the content of 3-MCPD and 3-MCPD fatty acid esters in sources and meat processing products. 3-MCPD fatty acid esters were analysed by GC/MS, which were hydrolyzed from fatty acid and then transferred 3-MCPD was extracted and reacted with derivative subject. As a result of analysis method validation, LOD was 5.4ppb, LOQ was 9.0ppb.

연구에서는 식품 중에 bound-MCPD를 측정하기 위해 지방을 추출하고, 메탄올에 녹인 황산으로 $60^{\circ}C$, 4hr 가수분해하여 모두 3-MCPD로 전환시켜 분석등하는 실험법을 개발하였다. 기존의 논문과 비교하였을때 분석시간이 더 빠르고, 현재 식품공전에 등재된 3-MCPD 시험법에 접목시킨 시험법이다. 분석가능한 선형구간은 3-MCPD로서 10ppb(ug/kg)-2ppm(mg/kg), 이며 반복성이 상대표준편차 5%이내, 재현성의 상대표준편차는 선형구간에서 10%이내이다. 기기적인 LOD는 5.4ppb, LOQ 9.0ppb이며 회수율은 3-MCPD 85.53%, bound-MCPD 82.97%이다.

Keywords

References

  1. T. Homonnai, G. Paz, A. Sofer, G.A. Yedwab and P.F. Kraicer,, A direct effect of alpha - chlorohydrin on motility and metabolism of ejaculated human spermatozoa, Contraception, 12, pp579-588 (1975). https://doi.org/10.1016/0010-7824(75)90019-0
  2. Jan velisek, Jiri Davidek, Vladislav Kubelka, Gustav Janicek, Zdenka Svobodova, and Zdenka Simicova, New chlorine- containing organic compounds in protein hydrolysates, J.Agric.Food Chem., 28, pp1142-1144 (1980). https://doi.org/10.1021/jf60232a022
  3. Janis Cerbulis, Owen W. Parks, Ray H. Liu, Edwin G. Piotrowski, and Harold M. Farrel, Jr., Occurrence of diesters of 3-chloro-1,2-propanediol in the neutral lipid fraction of goats' milk. J. Agric. Food. chem., 32, pp474-476 (1984). https://doi.org/10.1021/jf00123a013
  4. Veronika Divinova, Blanka Svejkovska, Marek Dolezal and Jan Velisek., Determination of free and bound 3-chloropropane- 1,2-diol by gas chromatography with mass spectrometric detection using deuterated 3-chloropropane-1,2-diol as internal standard., Czech J. Food Sci., 22, pp182-189 (2004).
  5. Veronika Divinova, Marek Dolezal and Jan Velisek, Free and bound 3-chloropropane-1,2-diol in coffee surrogates and malts. Czech J. Food Sci, 25, pp39-47 (2007).
  6. JECFA, Joint FAO/WHO Expert Committee and Food Additives Fifty-seventh meeting Rome., 5-14 June (2001).
  7. C.M. Breitling-UtzMann, H. Hrenn, N.U. Haase, G.M. Unbehend., Influence of dough ingredients on 3-chloropropane- 1,2-diol (3-MCPD) formation in toast, Food. addit. contam, 22, pp 97-103 (2005). https://doi.org/10.1080/02652030500037936
  8. Z. Zelinkova, B. Svejkovska, J. Velisek, M. Dolezal., Fatty acid esters of 3-chloropropane-1,2-diol in edible oils, Food. addit. contam, 23, pp 1290-1298 (2006). https://doi.org/10.1080/02652030600887628