HPLC를 이용한 식육류의 잔류 테트라싸이클린계 항생물질의 동시 분석법

Simultaneous determination of residual tetracyclines in beef, pork and chicken meats by high performance liquid chromatography

A rapid, sensitive, and simultaneous analytical method for redsidual tetracyclines(OTC, TC, CTC, and DC) in beef, pork, and chicken meats by high performance liquid chromatography was presented. Tetracyclines(TCs) were extracted from spiked sample with 0.1M Na₂EDTA Mcllvaine buffer and defatted with n-hexane, then the filtered extract was passed through an activated C18 cartridge. After a water rinse, TCs were eluted with methanol and the eluate was evaporated at 45℃ water bath to dryness and redissolved with mobile phase for the injection into HPLC. In HPLC analysis, the samples were chromatographed on a C8 column using 0.01M oxalic acid-acet-onitrile-methanol(7 : 2 : 1) at a flow rate of 1.0ml/min. For the determination of TCs, sample and standard solutions (20㎕) were injected and peak area was measured. Total analytical time was 16 minutes. The results were as follows ; 1. The standard calibration curve of four TCs showed linear(γ²≥0.995) in the range of 0.1~1ppm for OTC and TC and 0.25~1ppm for CTC and DC. 2. The recovery rates in spiked samples were 56.6~81.4%(CV 6.0~12.8%) for OTC, 55.5~74.4% (CV 5.3~10.7%) for TC, 57.7~68.5%(CV 6.4~13.1%) for CTC and 51.6~67.9%(CV 6.8~14.1%) at 0.1~0.2ppm, respectively. 3. Peak resolution was good enough to seperate four tetracyclines. 4. The lowest detectable levels in samples were 0.05ppm for OTC and TC and 0.1ppm for CTC and DC. Therefore, this method can be applicable to identify residual tetracyclines in meat qualitatively as well as quantitatively and also be complementary to bioassay.