| Multiresidue matrix solid phase dispersion (MSPD) extraction and HPLC determination of tetracyclines in animal muscle tissue |
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Hwan-goo Kang1, Seong-wan Son1, Byung-hoon Cho1, Hye-sook Lee1, Shin-ja Park2, Jae-hak Kim1, Myung-haing Cho3 |
1National Veterinary Research Institute
2College of Natural Science, Kyung-gi University
3College of Veterinary Medicine, Seoul National University |
| 시료고체상분산(matrix solid phase dispersion)전처리법을 이용한 식육중 테트라사이클린계 항생물질 동시정량분석 |
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강환구1, 손성완1, 조병훈1, 이혜숙1, 박신자2, 김재학1, 조명행3 |
1수의과학연구소
2경기대학교 이과대학
3서울대학교 수의과대학 |
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| Abstract |
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Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{sim}1.0{mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{mu}g/g$ for OTC and TC, and $0.1{mu}g/g$ for CTC and DC. |
| Key Words:
MSPD, tetracyclines, HPLC, muscle |
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