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目的建立简便、灵敏、准确的测定尿液中痕量杀鼠萘的固相萃取-高效液相色谱检测方法。方法尿液样品经Oasis(r)HLB小柱富集,以甲醇-甲基叔丁基醚洗脱,挥干溶剂后以甲醇-乙酸为流动相,采用XDB C18柱(150 mm×2．1 mm×5μm)分离,二极管阵列(DAD)308 nm检测。结果杀鼠萘在0．01-10．00 mg/L范围具有良好的线性关系,尿液中定量检测下限为0．005 mg／L,方法回收率为87．5％-98．4％,相对标准偏差小于7．3％。结论该法灵敏度高、操作简便、快速、准确,适用于作业工人的体检与中毒患者的临床诊断检测。
Objective To establish a simple, sensitive and accurate method for the determination of trace warfarin in urine by high performance liquid chromatography (HPLC). Methods Urine samples were concentrated on Oasis HLB cartridge and eluted with methanol-methyl tert-butyl ether. The solvent was evaporated and methanol-acetic acid was used as the mobile phase. The column was packed on an XDB C18 column (150 mm × 2.1 mm × 5μm) separation, diode array (DAD) 308 nm detection. Results There was a good linear relationship between warfarin and naphthalene in the range of 0.01-10.00 mg / L. The limit of quantification in urine was 0.005 mg / L. The recoveries were 87.5% -98.4% The relative standard deviation is less than 7.3%. Conclusion The method is highly sensitive, easy to operate, fast and accurate. It is suitable for the clinical diagnosis and detection of physical examinations and poisoning of workers.