Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Simultaneous Determination of Aflatoxins and Ochratoxin A in Pork by LC-MS/MS

LC-MS/MS를 이용한 돼지고기 중 총아플라톡신 및 오크라톡신 A 동시분석법 확립

  • Paek, Ockjin (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Park, Songyi (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Park, Ki Hun (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Kim, Sheen-Hee (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Suh, Saejung (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Yoon, Hae Jung (Food Standard Division, Food Safety Policy Bureau, MFDS)
  • 백옥진 (식품의약품안전평가원 식품위해평가부 오염물질과) ;
  • 박송이 (식품의약품안전평가원 식품위해평가부 오염물질과) ;
  • 박기훈 (식품의약품안전평가원 식품위해평가부 오염물질과) ;
  • 김신희 (식품의약품안전평가원 식품위해평가부 오염물질과) ;
  • 서세정 (식품의약품안전평가원 식품위해평가부 오염물질과) ;
  • 윤혜정 (식품의약품안전처 식품안전정책국 식품기준과)
  • Received : 2016.03.15
  • Accepted : 2016.06.02
  • Published : 2016.06.30
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Abstract

Aflatoxins and ochratoxin A (AFTs and OTA) are secondary fungal metabolites produced by several moulds, mainly by Aspergillus flavus by Aspergillus ochraceus and Penicillium verrucosum, and these toxins can be transferred to animals and humans through the ingestion of contaminated feed and food. This study was to develop the analytical method for determination the levels of AFTs ($B_1$, $B_2$, $G_1$ and $G_2$) and OTA in pork. The AFTs and OTA were analyzed simultaneously by electrospray ionization in positive ion mode and mass reaction monitoring (MRM) after solid phase extract (SPE) columns clean-up. Performance characteristics, such as accuracy, precision, linear range, limit of detection (LOD) and quantification (LOQ), were also determined. Matrix-matched standard calibration was used for quantification, obtaining the recoveries in the range of 67.3~108.2% with the relative standard deviations of < 20%. Limits of detection and quantification were also estimated, obtaining the limits of quantification ranged in $0.7{\sim}1.3{\mu}g/kg$. The results of the inter-day study, which was performed with pork samples for 3 days, showed an accuracy of 92.0~109.9%. The precisions (expressed as relative standard deviation values) for the inter day variation were 2.6~17.8%. The method developed in this study was able to carry out the analysis with the satisfactory intensity and accuracy.

돼지고기 중 5종의 곰팡이독소(아플라톡신 $B_1$, $B_2$, $G_1$, $G_2$ 및 오크라톡신 A)를 분석하기 위해 0.1% 개미산을 함유한 50% 아세토니트릴용액으로 추출한 후 고체상추출칼럼을 이용하여 정제하고, LC-MS/MS로 동시 정량할 수 있는 시험법을 마련하였다. 분석조건으로 측정한 5종의 곰팡이독소 matrix-matched 표준곡선식에서 모두 상관계수 0.998이상의 상관관계를 나타내었다. 5종의 곰팡이독소 2배의 정량한계에서 10배의 정량한계로 첨가한 시료에서 평균 회수율은 72.1~109.9%로 실험 결과들이 EU 가이드라인에서 제시하는 유효성 확인을 위한 기준을 만족함으로써 시험법의 신뢰성을 확보할 수 있었다. 충청지역 유통되고 있은 돼지고기 20건에 대한 총아플라톡신 및 오크라톡신A에 대한 오염도 조사결과 정량한계 미만으로 조사되었다.

Keywords

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