Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC
2010
Park, S.O., Gwangju Regional Korea Food and Drug Administration, Gwangju, Republic of Korea | Lee, S.H., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Ahn, J.H., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Jung, Y.J., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Kim, S.C., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Kim, J.Y., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Keum, E.H., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Sung, J.H., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Kim, S.Y., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Jang, Y.M., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea | Kang, C.S., Busan Regional Korea Food and Drug Administration, Busan, Republic of Korea
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×4.6 mm, 5 ㎛) 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.
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