论文部分内容阅读
提出了一种反相高效液相色谱法同时测定4种苯二氮卓艹类药物的分析方法.考察了4种苯二氮卓艹类药物的保留值与流动相组成、流速、pH及柱温等色谱条件的关系,优化了色谱条件.确定了以ODSHypersil为色谱柱,甲醇-水(51∶49;V/V,用氨水调pH7.8)为流动相,流速为0.8mL/min,柱温为45℃,检测波长为220nm的最佳色谱条件.甲苯作为内标物,以内标法峰面积定量.硝西泮,地西泮,三唑仑和艾司唑仑线性范围分别是0.1mg/L～320mg/L,0.2mg/L～320mg/L,0.1mg/L～320mg/L和0.08mg/L～320mg/L;检测限分别为0.1mg/L,0.2mg/L,0.1mg/L和0.08mg/L.该方法用于尿液中的苯二氮卓艹类药物的测定.其回收率为97.0%～108.7%,标准偏差为1.7%～3.0%(n=7).该方法简单、快速、精确、灵敏、重复性好.
A method for the simultaneous determination of 4 benzodiazepines by reversed-phase high performance liquid chromatography (RP-HPLC) was proposed.The retention values of the four benzodiazepines were investigated with the mobile phase composition, flow rate, pH and column Temperature and other chromatographic conditions to optimize the chromatographic conditions.ODSHypersil column, methanol-water (51:49; V / V, pH7.8 with ammonia water) was used as the mobile phase, the flow rate was 0.8mL / min, The column temperature was 45 ℃ and the detection wavelength was at 220 nm.The best chromatographic conditions were toluene as internal standard and internal standard peak area.The linear ranges of nitrazepam, diazepam, triazolam and estazolam were 0.1 The detection limits were 0.1mg / L, 0.2mg / L, 0.1mg / L ~ 320mg / L, 0.1mg / L ~ 320mg / L and 0.08mg / L ~ mg / L and 0.08 mg / L. The method was applied to the determination of benzodiazepines in urine with recovery of 97.0% -108.7% and standard deviation of 1.7% -3.0% (n = 7) The method is simple, rapid, accurate, sensitive and reproducible.