摘要
目的建立高效液相色谱法测定血浆与尿中地西泮浓度。方法采用Agilent Eclipse XDB-C18色谱柱（4．6mm×150mm，5μm），以甲醇-水（65：35）为流动相，流速1．0mL·min^-1，检测波长254nm。结果地西泮和内标物出峰时间分别为3．5和7．3min，分离效果较好；血浆样品中地西泮3种浓度（4．0，8．0，16．0μg·mL^-1）日内和日间RSD均〈6％，尿样中地西泮3种浓度（4．0，8．0，16．0μg·mL^-1）日内和日间RSD均〈5％；血浆中地西泮回收率为95．63％～98．33％，尿样中地西泮回收率为88．33％～95．33％，血清及尿样样品线性范围为2．0～64．0μg·mL^-1，相关系数0．9958。血浆、尿样品地西泮最低检出限分别为2．0及1．5μg·mL^-1。结论该条件可对地西泮中毒患者进行药物快速检测并定量分析。
Objective To set up an HPLC method for the determination of the concentration of diazepam in the blood plasma and urine of patients with diazepam intoxication. Methods An Agilent Eclipse XDB-C18 chromatographic column （4.6 mm × 150 mm, 5 μm） served as the stationary phase; the mobile phase was methanol-water（65 ： 35 ） ; the flow rate, 1.0 mL · min^-1, and the detection wavelenghth , 254 nm. Results The retention times for diazepam and the internal standard were 3.5 min. and 7.3 min. , respectively. The separation was fairly effective. With diazepam concentrations of 4.0, 8.0 and 16.0 μg · mL^-1, the intra-day and inter-day RSD were both smaller than 6% for plasma and smaller than 5% for urine. The rates of recovery of diazepam in the plasma and urine were 95.63% - 98.33% and 88.33% - 95.33%, repectively. The standard calibration curves were linear when the concentrations of diazepam in the plasma and urine samples were within the range of 2.0 - 64.0 μg · mL^- 1, with a correlation efficient of 0. 995 8. The lower limits for the detection of diazepam in the plasma and and wine samples were 2.0 and 1.5 μg · mL^- 1, respectively. Conclusion The method was shown to be feasible for the rapid detection and quantitative analysis of the drug in case of diazepam poisoning.
出处
《医药导报》
CAS
2007年第12期1415-1417,共3页
Herald of Medicine
