高效液相色谱法分析生物样品中的敌鼠  

Study of Diphacinone in Biological Samples by High Performance Liquid Chromatography/Diode Array Detector

作　　者：杨士云[1] 潘冠民[1] 孟广范[1] 张大明[1] 

机构地区：[1]北京市公安局法医中心,北京100085

出　　处：《色谱》2001年第3期245-247,共3页Chinese Journal of Chromatography

基　　金：北京市公安局科研项目

摘　　要：研究用阴离子交换、氰基及硅胶柱固相萃取技术分离提取血、尿、肝及肾中的敌鼠。以香豆素作内标 ,用高效液相色谱 二极管阵列检测器方法进行分离鉴定。色谱条件 :分析柱为HypersilBDSC18(5 μm ,15 0mm× 4 6mmi.d .) ,保护柱为PhenomenexODS(4mm× 3 0mmi.d .) ;流动相 :A为 0 5 %离子对A水溶液 ,B为 0 5 %离子对A甲醇溶液 ,以梯度淋洗程序分离 ;检测波长为 2 86nm。当敌鼠的质量浓度在 1mg/L～ 10 0mg/L范围时 ,其浓度同其峰面积与内标物的峰面积之比有良好的线性关系 (r=0 9999) ,最小检出限量为 5ng(按S/N =3计 )。An analytical approach has been developed for high performance liquid chromatographic determination of diphacinone extracted from liver,blood,urine and kidney of rabbit by solid phase extraction (SPE) cartridges(using SAX,CN or SILICA GEL) with coumarin as the internal standard Diphacinone was separated by reversed phase gradient chromatography with DAD detection at 286 nm The Analytical column was Hypersil BDS C 18 (150 mm×4 6 mm i.d.,5 μm) and the guard column was Phenomenex ODS(4 mm×3 0 mm i.d.).The mobile phase was a gradient mixture of aqueous solution (A) and methanol solution (B) both containing 0 5% ion pair A . There was a good linear relationship between the concentration of diphacinone and the ratio of peak areas of diphacinone and coumarin (internal standard)( r =0.999?9). The linear range was 1 mg/L 100 mg/L, and the lower detection limit was 5 ng ( S/N =3) The average recoveries of diphacinone in urine, blood and liver were 88 4%( n =3,RSD=1 25%,SPE by CN column),82 2%( n =3,RSD=1 67%,SPE by SAX column), 91 0%( n =3,RSD=2 77%,SPE by SILICA GEL column),respectively

关 键 词：高效液相色谱法 二极管阵列检测器 敌鼠 固相萃取 生物样品 抗凝血鼠药 药物分析 

分 类 号：R978.8[医药卫生—药品] R917[医药卫生—药学]