| Matrix solid phase dispersion(MSPD) extraction and HPLC determination of enrofloxacin and ciprofloxacin in pork muscle tissue |
|
Hwan-goo Kang1, Seong-wan Son1, Hye-sook Lee1, Jae-hak Kim1, Myung-haing Cho2 |
1National Veterinary Research Institute
2College of Veterinary Medicine, Seoul National University |
| 시료고체상분산(matrix solid phase dispersion)전처리법과 액체크로마토그라피를 이용한 돈육중 enrofloxacin 및 ciprofloxacin 분석 |
|
강환구1, 손성완1, 이혜숙1, 김재학1, 조명행2 |
1수의과학연구소
2서울대학교 수의과대학 |
|
|
| Abstract |
|
A method for the isolation by matrix solid phase dispersion method and liquid chromatographic determination of enrofloxacin and ciprofloxacin in pork muscle tissue is presented. Blank or enrofloxacin and ciprofloxacin spiked samples(0.5g) containing 0.05g oxalic acid were blended with $C_{18}$(octadecylsilyl derivatized silica) packing material. After homogenization, $C_{18}$/muscle tissue matrix was transferred to glass column made from 10ml glass syringe and filter paper, and compressed to 4~4.5ml volume. A column was washed with 8ml of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8ml and dried, following which enrofloxacin and ciprofloxacin were eluted with 8ml of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278nm. Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of $0.05{sim}1.0{mu}g/ml$ and eluted within 5ml elution volume of methanol from the matrix. Fortified sample containing 0.05g oxalic acid represented more good recoveries than that of control sample. Average percentages of enrofloxacin and ciprofloxacin were $93.30{pm}4.56%$ and $91.84{pm}4.17%$, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and $0.75{mu}g/g$). The interassay variability of enrofloxacin was $6.02{pm}5.33%$ with an intra-assay variability of 4.89% and $6.75{pm}2.68%$ with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was $0.030{mu}g/g$ in the spiked sample. |
| Key Words:
enrofloxacin, ciprofloxacin, pork muscle, MSPD, HPLC |
|
PDF Links
Full text via DOI
Download Citation
