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KMID : 0359319970370010195
Korean Journal of Veterinary Research
1997 Volume.37 No. 1 p.195 ~ p.202
Matrix solid phase dispersion ( MSPD ) extraction and HPLC determination of enrofloxacin and ciprofloxacin in pork muscle tissue
김재학/Kim, Jae Hak
조명행/강환구/손성완/이혜숙/Cho, Myung Haing/Kang, Hwan Goo/Son, Seong Wan/Lee, Hye Sook
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 10㎖ glass syringe and filter paper, and compressed to 4∼4.5㎖ volume. A column was washed with 8㎖ of hexane and dried under vacuum. Interfering materials were removed by ethylacetate 8㎖ and dried, following which enrofloxacin and ciprofloxacin were eluted with 8㎖ of methanal under gravity. The eluate containing enrofloxacin and ciprofloxacin wase free from interfering compound when analysed by HPLC with UV detection at 278㎚.
Enrofloxacin and ciprofloxacin showed linear response with UV detector at the range of 0.05-1.0㎍/㎖ and eluted within 5㎖ 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 ±4.56% and 91.84 ±4.17%, respectively, for the concentration range(0.05, 0.1, 0.25, 0.5 and 0.75㎍/g). The interassay variability of enrofloxacin was 6.02 ±5.33% with an intra-assay variability of 4.89% and 6.75 ±2.68% with 4.54% for ciprofloxacin. Detection limit of enrofloxacin and ciprofloxacin was 0.030㎍/g in the spiked sample.
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학술진흥재단(KCI)