高效液相色谱法测定中华绒螯蟹主要组织中双氟沙星及其代谢产物沙拉沙星方法  

RP-HPLC determination of difloxacin and its metabolite in tissues of Chinese mitten-handed crab(Eriocheir sinensis)

作　　者：李海迪[1] 杨先乐[1] 胡鲲[1] 王翔凌[1] 

机构地区：[1]上海海洋大学水产与生命科学院农业部渔业动植物病原库,上海201306

出　　处：《药物分析杂志》2009年第7期1142-1147,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家十一五科技支撑计划"渔药安全使用技术和新型渔药制剂开发"(2006BAD03B04)

摘　　要：目的:建立高效液相色谱法(RP-HPLC)测定中华绒螯蟹(Eriocheir sinensis)肌肉、肝胰腺、精巢、卵巢组织中双氟沙星及其代谢产物沙拉沙星测定方法,并用于双氟沙星及其代谢产物在中华绒螯蟹体内的药代动力学研究。方法:色谱柱为ZOR-BAX SB-C18(150mm×4.6mm,5μm);流动相:乙腈-0.030mol·L-1四丁基溴化氨(5∶95),用磷酸调节至pH3.1;流速:1.5mL.min-1;紫外检测波长:276nm;柱温:40℃。结果:双氟沙星在肌肉、肝胰腺、精巢和卵巢中回收率分别为(94.3±3.8)%、(78.9±4.5)%、(80.9±1.8)%、(75.5±2.3)%,沙拉沙星的回收率分别为(82.5±2.6)%、(92.8±4.7)%、(79.9±3.8)%、(80.6±4.4)%。日内精密度小于4.7%,日间精密度小于5.8%。双氟沙星的检测限为0.01μg.g-1,沙拉沙星的检测限为0.02μg.g-1。结论:本法灵敏度高,重复性好,能够快速可靠地测定双氟沙星及其代谢产物的浓度,适用于双氟沙星及其代谢产物沙拉沙星在中华绒螯蟹体内药代动力学研究。Objective： To eatablish a method for the content determination of difloxacin and its metabolite sarafloxaein in muscle, hepatopancreas, spermary, ovary of Chinese mitten - handed crab （ Eriocheir sinensis） by RP - HPLC, and apply it to the pharmacokinetic study of difloxacin. Methods：HPLC instrument was adopted with C18 reversed - phase column（ 150 mm ×4. 6 mm,5 μm）and monitored by UV. The mobile phase was composed of acetonitrile - 0. 030 mol·L^-1 tetrabutylammonium bromide （5： 95 ） , adjusted pH to 3.1 by phosphate, eluated with a flow rate of 1.5 mL ·min^- 1, detection wavelength was 276 nm and column temperature was 40 ℃. Results： The recovery of difloxacin in muscle, hepatopancreas, spermary, ovary were found to be （ 94. 3 ±3.8 ） % , （ 78.9 ±4. 5 ） % , （ 80. 9 ±1.8）%,（75.5 ±2.3）% and sarafloxacin were（82.5 ±2.6）%,（92.8±4.7）%,（79.9 ±3.8）%,（80.6 ±4. 4）% ,respectively. The intra- day precision RSD was low at 4. 7% ;The interday precision RSD was low of 5.8%. The lowest detected limit of difloxaein was 0. 01 μg·g^-1 ,and that of sarafloxacin was 0. 02 μg·g^-1. Conclusions：The method has good sensitivity, precision, and simple to detect difloxaein and its metabolite , it is suitable for pharmacokinetic studies of difloxacin and its metabolite tissues in Chinese mitten - handed crab （ Eriocheir sinensis）.

关 键 词：中华绒螯蟹 高效液相色谱法 双氟沙星 沙拉沙星 

分 类 号：R917[医药卫生—药物分析学]