Earticle

초록

영어

To establish and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for therapid and accurate quantitation of diarrhetic shellfish poisoning (DSP) toxins, we compared the results from differentmobile phases and columns used for their analysis and collision energies for MS/MS experiments. Clear peaks of okadaicacid (OA) and dinophysistoxin-1 (DTX1) were obtained by using a mobile phase comprising aqueous acetonitrilecontaining 2mM ammonium formate and 50 mM formic acid. The collision energies were optimized to facilitate the mostsensitive detection for each toxin, namely, OA, DTX1, pectenotoxin-2 (PTX2), or yessotoxin (YTX). Further, the maximumion response was obtained at a collision energy of 48V for OA and DTX1. We compared the analytical performance ofC8 and C18 columns. A wide range of toxins namely, OA, DTX1, PTX2, and YTX, except DTX3, were detected by boththe columns. Although DTX3 was only detected by the C8 column, we found that the C18 column was also suitable forthe quantitation of OA and DTX1 the toxins responsible for inducing diarrhea. The limit of detection of OA and DTX1by the established LC-MS/MS conditions was 1ng/g, and the limit of quantitation of the toxins under the same conditionswas 3ng/g. The process efficiencies were 91-118% for oysters (Crassostrea gigas) and 96-117% for mussels (Mytilusgalloprovincialis) further, we observed no significant effect of matrix during the ionization process in LC-MS/MS. Thecomparison between mouse bioassay (MBA) and LC-MS/MS yielded varying results because low concentrations of OAand DTX1 were detected by LC-MS/MS in some shellfish samples, which provided positive results on MBA for DSP. Theanalysis time required by MBA for DSP analysis can be reduced by LC-MS/MS.

한국어

설사성패류독의 신속정밀 분석조건 확립을 위하여 LC-MS/MS를 사용하여 이동상, 분석용 column 및 collision energy 등을 변화시키면서 시험하였다. 50mM formic acid와 2mM ammoniumformate가 함유된 acetonitrile 수용액을 이동상으로 사용하였을 때OA와 DTX1이 검출되었다. Collision energy는 독소 성분에 따라달리하는 것이 다성분 동시분석에 적합하였으며 OA와 DTX1 고유의 fragment ion들은 48V 정도에서 최적의 intensity로 확인되었다. Column의 종류에 따라서는 C8 column의 경우 OA, DTX1,DTX3, PTX2 및 YTX 모두 검출 가능하였으나 실제 검출 대상이 OA와 DTX1인 경우에는 일반적으로 사용되는 C18 column도적합한 것으로 확인되었다. 본 연구에서 확립한 LC-MS/MS 분석조건의 검출한계는 OA와 DTX1 모두 1ng/g, 정량한계는 각각 3ng/g이었고, 표준독 성분을 첨가한 시료에서 process efficiency는굴의 경우 91-118%, 진주담치에서는 96-117%이었고, matrix의 영향은 거의 없었다. 마우스 시험에서 양성을 나타낸 시료를 LC-MS/MS법으로 분석한 결과, 일부 시료에서만 OA 및 DTX1이 검출되어 두 시험법의 독성은 일치하지 않았으며 LC-MS/MS법은마우스 시험법보다 하루 이상 분석시간을 단축할 수 있었다.

목차

Abstract
 서 론
 재료 및 방법
 결과 및 고찰
 요 약
 문 헌

키워드

저자

• 이가정 [ Ka Jeong Lee | 국립수산과학원 식품안전연구단(Food Safety Research Center, National Fisheries Research and Development Institute) ]
• 스즈키 도시유키 [ Toshiyuki Suzuki | 일본 중앙수산연구소(Biochemistry and Food Technology Division, National Research Institute of Fisheries Science, Fisheries Research Agency,Yokohama, Japan) ]
• 김풍호 [ Poong Ho Kim | 국립수산과학원 식품안전연구단(Food Safety Research Center, National Fisheries Research and Development Institute) ]
• 오은경 [ Eun Gyoung Oh | 국립수산과학원 식품안전연구단(Food Safety Research Center, National Fisheries Research and Development Institute) ]
• 송기철 [ Ki Cheol Song | 국립수산과학원 식품안전연구단(Food Safety Research Center, National Fisheries Research and Development Institute) ]
• 김지회 [ Ji Hoe Kim | 국립수산과학원 양식환경연구소(Aquaculture Environment Research Institute, National Fisheries Research and Development Institute) ] Corresponding author

참고문헌

발행기관

간행물

표지보기 관심저널 등록

• 간행물명

  한국식품과학회지 [Korean Journal of Food Science and Technology]

• 간기

  격월간

• pISSN

  0367-6293

• 수록기간

  1969~2011

• 십진분류

  KDC 574 DDC 664