柱切换高效液相色谱法测定尿中苯骈二氮杂类药物  

HPLC for the determination of benzodiazepines in urine using the column-switching technique

作　　者：梁晨[1] 郭幼梅[1] 金琦芸[1] 张玉荣 汪蓉 

机构地区：[1]复旦大学药学院药物分析教研室,上海200032 [2]上海市刑事科学技术研究所,上海200083

出　　处：《中国临床药学杂志》2003年第3期157-160,共4页Chinese Journal of Clinical Pharmacy

摘　　要：目的 :建立尿中 10种常见的苯骈二氮杂类药物 (氯硝西泮、氟硝西泮、艾司唑仑、三唑仑、阿普唑仑、硝西泮、去甲地西泮、奥沙西泮、替马西泮、地西泮 )的柱切换高效液相色谱测定方法。方法 :尿样用磷酸盐缓冲液 1∶1稀释 ,离心后直接进样1 0mL进入预处理柱 ,用水作为预处理流动相 ,然后用分析流动相CH3OH H2 O( 60∶40 )将保留在预处理柱上的药物反冲进入分析柱进行分析。检测波长 (λ)为 2 0 0nm。结果 :氯硝西泮、氟硝西泮、艾司唑仑、三唑仑、阿普唑仑的检测限均为 2ng·mL-1(rSN=3 ) ,线性范围为 10～ 10 0 0ng·mL-1,r≥ 0 .9992 ;硝西泮、奥沙西泮、替马西泮、去甲地西泮、地西泮的检测限为 5ng·mL-1(rSN=3 ) ,线性范围为 2 0～ 10 0 0ng·mL-1,r≥ 0 9993。日内、日间RSD均 <10 % (n =5 )。结论 :本法准确、灵敏、快速、简便 。AIM: To develop a column-switching HPLC for the determination of 10 frequently prescribed benzodiazepines: clonazepam, flunitrazepam, nitrazepam, estazolam, triazolam, alprazolam, oxazepam, temazepam, nordiazepam, and diazepam in urine. METHODS: Urine samples (1.0 mL) were diluted with 1.0 mL phosphate buffer, after centrifugation the samples 1.0 mL were directly injected into a extraction column. After a washing step with the extraction mobile phase (water), the retained benzodiazepines were back-flushed into the analytical column with the analytical mobile phase CH 3OH-H 2O (60∶40). The UV detector was set at λ=200 nm. RESULTS: The limit of detection was 2 ng·mL -1 (r SN=3) for clonazepam, flunitrazepam, estazolam, triazolam, alprazolam and was 5 ng·mL -1 (r SN=3) for nitrazepam, oxazepam, nordiazepam, temazepam, diazepam. The method showed excellent linearity from 10 to 1 000 ng·mL -1 for clonazepam, flunitrazepam, estazolam, triazolam, alprazolam and from 20 to 1 000 ng·mL -1 for nitrazepam, oxazepam, temazepam, nordiazepam, diazepam. The relative standard deviation for between-day and within-day assay was<10% (n=5). The linear correlation coefficient was> 0.999 3. CONCLUSION: The method described is sensitive, rapid, reproducible and simple.

关 键 词：柱切换 高效液相色谱法 测定技术 尿 苯骈二氮杂Zhuo类药物 镇静催眠类药物 

分 类 号：D919[医药卫生—法医学]