Choi Jeong-Heui, Mamun M I R, Abd El-Aty A M, Kim Kyung Tae, Koh Hong-Bum, Shin Ho-Chul, Kim Jin-Suk, Lee Kang Bong, Shim Jae-Han
Natural Products Chemistry Laboratory, Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Science, Chonnam National University, 300 Yongbong-dong, Buk-gu, Gwangju 500-757, Republic of Korea.
Talanta. 2009 Apr 30;78(2):348-57. doi: 10.1016/j.talanta.2008.11.021. Epub 2008 Nov 25.
A supercritical fluid extraction method combined with high-performance liquid chromatography-fluorescence detection was developed for the determination of enrofloxacin, danofloxacin, and ciprofloxacin in pig muscle, lung, and kidney samples. The optimal SFE conditions were 80 degrees C, 300 kg/cm(2), 30% methanol for 40 min as a dynamic extraction time, in addition to 0.2g Na(4)EDTA and 7.0 g sea sand in the extraction vessel. The use of Na(4)EDTA and sea sand on SFE extraction resulted in improvement of the recoveries of ciprofloxacin, a polar and hydrophilic compound, as well as enrofloxacin and danofloxacin. Overall, the recoveries ranged from 86.7 to 113.1% using the Na(4)EDTA/sea sand-assisted SFE extraction method. The Na(4)EDTA/sea sand-assisted SFE-HPLC-FLD validated method was successfully carried out in pig tissues, and proved to be specific, sensitive, reliable, and accurate. The method was also applied satisfactorily for accurate quantitative residue analysis in incurred pig tissues.
建立了一种超临界流体萃取法结合高效液相色谱-荧光检测法,用于测定猪肌肉、肺和肾脏样品中的恩诺沙星、达氟沙星和环丙沙星。最佳超临界流体萃取条件为80℃、300 kg/cm²、30%甲醇、动态萃取时间40分钟,此外在萃取容器中加入0.2 g乙二胺四乙酸四钠和7.0 g海砂。乙二胺四乙酸四钠和海砂用于超临界流体萃取,提高了极性和亲水性化合物环丙沙星以及恩诺沙星和达氟沙星的回收率。总体而言,使用乙二胺四乙酸四钠/海砂辅助超临界流体萃取法的回收率在86.7%至113.1%之间。乙二胺四乙酸四钠/海砂辅助超临界流体萃取-高效液相色谱-荧光检测验证方法在猪组织中成功实施,证明具有特异性、灵敏性、可靠性和准确性。该方法也令人满意地应用于实际猪组织中残留的准确定量分析。