Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC

Macrolide계 항생물질 동시분석법 확립 및 모니터링

  • Park, Sang-Ouk (Hazardous Substance Analysis Division, Gwangju Regional Korea Food and Drug Administration) ;
  • Lee, Sang-Ho (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Ahn, Jong-Hoon (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Jung, Young-Ji (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Kim, Seong-Cheol (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Kim, Ji-Yeon (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Keum, Eun-Hee (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Sung, Ju-Hyun (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Kim, Sang-Yub (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Jang, Young-Mi (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration) ;
  • Kang, Chan-Soon (Imported Food Analysis Division, Busan Regional Korea Food and Drug Administration)
  • 박상욱 (광주지방식품의약품안전청 유해물질분석과) ;
  • 이상호 (부산지방식품의약품안전청 수입식품분석과) ;
  • 안종훈 (부산지방식품의약품안전청 수입식품분석과) ;
  • 정영지 (부산지방식품의약품안전청 수입식품분석과) ;
  • 김성철 (부산지방식품의약품안전청 수입식품분석과) ;
  • 김지연 (부산지방식품의약품안전청 수입식품분석과) ;
  • 금은희 (부산지방식품의약품안전청 수입식품분석과) ;
  • 성주현 (부산지방식품의약품안전청 수입식품분석과) ;
  • 김상엽 (부산지방식품의약품안전청 수입식품분석과) ;
  • 장영미 (부산지방식품의약품안전청 수입식품분석과) ;
  • 강찬순 (부산지방식품의약품안전청 수입식품분석과)
  • Received : 2009.12.22
  • Accepted : 2010.01.20
  • Published : 2010.06.30

Abstract

In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

축산물 중 macrolide계 항생물질 3종을 신속분석하기 위하여 효과적인 전처리법을 설정하고 고속액체크로마토그라피(HPLC)를 이용한 동시분석법을 제시하였다. 대상물질은 tilmicosin, tylosin, spiramycin이며, 확립된 분석법을 이용하여 모니터링을 실시하기 위하여 전국 6개 도시인 서울, 부산, 대전, 인천, 대구, 광주에서 수입원산지가 표시된 쇠고기와 돼지고기 및 그 가공품을 수거하여 분석하였다. 전처리법에 있어서 solid phase extraction(SPE)법에 비하여 액상추출법이 더 높은 회수율을 나타내었으며 전처리 단계도 간단하여 대상 항생물질을 분석하기에 적절하였다. 3종의 항생물질 분리를 위한 컬럼은 C18($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$)을 사용하였으며, HPLC 이동상은 0.025M phosphate buffer(pH 2.5) 및 acetonitrile을 이용한 gradient 조건을 설정하였다. UV 검출파장은 spiramycin 경우 232 nm이고, tilmicosin과 tylosin은 288 nm을 이용하였다. 평균회수율은 83.0-90.2%이였으며, 검출한계는 각각 7(spiramycin), 12(tilmiconsin), 12(tylosin) ng/g으로 나타났다. 수입 축산물의 항생물질에 대한 안전성을 검토하기 위하여 국내 유통 중인 수입축산물 및 그 가공품을 대상으로 하여 모니터링을 실시한 결과, 시료는 전국 6개 대도시에서 126건 구입하였으며 모든 시료에서 macrolide계 항생물질이 검출되지 않았다.

Keywords

References

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