摘要
以100mL/L的三氯乙酸-甲醇(体积比为50∶50)混合液提取组织中的药物,采用C18固相萃取小柱净化,使用氯甲酸芴甲酯,在0.1mol/L的硼酸缓冲液(pH10)中进行柱前衍生化,反应15min,直接进样。荧光检测,激发波长为260nm,发射波长为315nm,流动相为V乙腈∶V四氢呋喃∶V水=87∶4∶13,流速为1mL/min。动物组织中黏菌素含量为0.05～1.00μg/g时,黏菌素的含量与其峰面积之间存在良好的线性关系(r2>0.990),在猪、鸡的肌肉、肝、肾组织中按0.05、0.15、1.00μg/g3个添加水平做黏菌素的回收率试验,其回收率≥80%,变异系数≤12%。结果表明,该方法重复性好,灵敏度高,简便,可用于动物组织中黏菌素残留的检测。
A high performance liquid chromatographic（HPLC） method was developed with fluorescence detector for the determination of colistin in animal tissues. The sample treatment consisted of protein precipitation with 10% trichloroacetic acid-methanol（50 ： 50, v/v）, purification with C18 SPE cartridges, and derivatization with 9-fluorenylmethyl chloroformate in borate buffer（pH10）. The products were detected by HPLC with fluorescence detector at an excitation wavelength of 260 nm and an emission wavelength of 315 nm. The mobile phase consisted of acetonitrile-tetrahydrofuran-water（87 ： 4 ： 13, v/v/v） and the flow rate was 1.0 mL/min. Within the range of 0.05 to 1.00μg/g in tissue,good linearity was obtained（r^2 〉0. 990）. The recoveries from fortified liver,muscle and kidney at three levels （0.05,0.15 and 1.00μg/g） were higher than 800/oo ,with excellent RSD（≤12%）. The results showed that the developed method was of good reproducibility, high sensitivity,and expedience and could be applied to the determination of colistin residue in animal tissues.
出处
《中国兽医科学》
CAS
CSCD
北大核心
2009年第5期461-464,共4页
Chinese Veterinary Science
基金
农业部兽药残留检测标准制定项目
