摘要
建立了测定猪血浆及肝脏、肾脏、肌肉等组织中的喹赛多及其代谢物脱二氧喹赛多的高效液相色谱 (HPL C)法。血浆样用甲醇沉淀蛋白后离心取上清液进样测定。组织样先用乙腈匀浆 ,用正己烷脱脂后作 HPL C检测。色谱柱为ODS C1 8柱 ;流动相血浆样测定为乙腈∶水 (2 0∶ 80 ) ,组织样测定为甲醇∶水 (4 2∶ 5 8) ,流速为 1.0 m L / min;紫外检测波长 30 5 nm。药物工作液质量浓度范围为 0 .0 0 5~ 0 .5 0 0 m g/ L 时 ,血浆样品及组织样品测定条件下药物质量浓度与响应值均具良好线性关系 ,相关系数 >0 .999。血浆中药物质量浓度为 0 .0 2、0 .10、0 .5 0 mg/ L 时 ,喹赛多及脱二氧喹赛多的回收率均大于 70 % ,组织中药物含量为 0 .0 5、0 .2 0、1.0 0 μg/ g时 ,肌肉样品的回收率均大于 70 % ,肝脏、肾脏样品则为 5 0 %~ 80 %。本试验条件下 ,喹赛多及其脱二氧代谢物的最低检出质量浓度 ,血浆样品分别为 0 .0 1、0 .0 2mg/ L ,组织样品 2种检测物均为 0 .0 2 5μg/ g。测定了工作液 3种质量浓度 0 .0 1、0 .0 5、0 .2 5 mg/ L的仪器精密度 ,日内相对偏差 <8.0 % ,日间相对偏差 <17.0 %。
A high performance liquid chromatographic(HPLC) method was developed for the determination of cyadox and its metabolite desoxycyadox in swine plasma,liver,kidney and muscle.Plasma sample was mixed with methanol,and then centrifuged and injected on to HPLC column.Tissues sample was homogenized with acetonitrile to extract cyadox and desoxycyadox,and cleaned up by hexane.Cyadox and desoxycyadox was separated on a OSD C 18 column,and quantitated by using UV detector set at 305 nm.The responses for cyadox and desoxycyadox were linear in the range of 0 005 0 500 mg/L with a correlation coefficient of >0 999.The average recoveries of cyadox and desoxycyadox were >70% when added to plasma samples at 0 020,0 100,0 500 ng/L.The mean recoveries of the two compounds from tissues were >70% for muscles,and only 50% 80% for livers and kidneys when fortified with 0 050,0 200,1 000 μg/g.The detection limits for cyadox and desoxycyadox in plasma were 0 010,0 020 mg/L respectively,and was 0 025 μg/g for the two compounds in various tissues.
出处
《中国兽医学报》
CAS
CSCD
北大核心
2003年第4期363-365,共3页
Chinese Journal of Veterinary Science
基金
国家自然科学基金资助项目 ( 3 9870 5 96)
教育部骨干教师培养计划资助项目 ( 2 0 0 0年 )