Analytical Methods for Diethylstibestrol and Zeranol in Muscle Foods

근육 식품 중의 diethylstibestrol과 zeranol 분석법

  • Published : 2002.06.01

Abstract

Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

성장 촉진 호르몬제인 DES와 zeranol의 분석을 위한 조건을 검토한 결과는 다음과 같다. 질량분석기의 SIM에서 선택한 이온 중 DES는 $M^+$ 416, $D_8DES$$M^+$ 420, ${\beta}-estradiol$$M^+$ 416, zeranol은 $M^+$ 433이 가장 좋은 응신비를 나타내었고 이들 이온을 선택할 경우 효율적으로 분석이 가능하였다. 강 음이온 교환수지인 Dowex $2{\times}8$, 400 mesh 칼럼 1 cc에 통과시킨 경우 방해물질이 효율적으로 제거되었고 회수율이 가장 높았다. $D_8DES$을 내부표준물질로 사용하여 회수율을 측정한 결과 DES는 $85{\sim}110%$이었고, zeranol은 $75{\sim}110%$이었으며 ${\beta}-estradiol$을 내부표준물질로 사용한 경우 DES의 회수율은 $82{\sim}105%$, zeranol은 $65{\sim}120%$이었다. 또한 $D_8DES$ 대신에 ${\beta}-estradiol$을 내부표준물질로 사용하여 DES와 zeranol을 분석하는 것이 가능하였다. DES와 zeranol의 LOD를 측정한 결과 각각 0.05 ng/g, 0.2 ng/g었으며 LOQ를 측정할 결과 DES는 0.5 ng/g, zeranol은 1.0 ng/g이었다. 국내산과 수입산 쇠고기, 국내산 돼지고기, 닭고기, 오리고기, 양식광어와 양식 송어를 분석한 결과 DES와 zeranol은 잔류되지 않았다.

Keywords

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