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柱前衍生-高效液相色谱法测定丙戊酸钠血药浓度
DETERMINATION OF SODIUM VALPROATE IN SERUM BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY AFTER PRE-COLUMN DERIVATIZATION
【摘要】 目的建立柱前衍生-高效液相色谱法测定血清样品中丙戊酸钠的含量。方法以Diamonsil C18(4.6×250mm 5μm)为色谱柱,流动相为甲醇-水(87:13,V/V),检测波长为245nm;流速为1.0mL/min;柱温25℃样品酸化提取后经α-溴代苯乙酮衍生化后分析,环己烷羧酸为内标。结果标准曲线线性相关系数(r)为0.999 3,线性范围15.0180.0μmL,平均回收率为103.2%,日内、日间相对标准差均小于10%,最低检出浓度为0.3μmL。结论该方法简便、准确,适合于临床血药浓度监测。
【Abstract】 Objective To establish a method for determining sodium valproate in serum by high performance liquid chromatography(HPLC) after pre-column derivatization.Methods The analytical column was Diamonsil C18 column(250mm ×4.6mm,5μm).The mobile phase consisted of methanolwater(87:13,V/V) at the flow rate of 1.OmL/min.The detection wave length was set at 245nm and the column temperature was set at 25℃.The samples were extracted after being acidified,then derived withα-bromoacetophenone before analysis.Cyclohexane carboxylic acid was used as the internal standard.Results The liner correlation of the standard curvilinear equation was r =0.999 3 with a linear range of15.0-180.00μg/mL.The mean relative recovery was 103.2%.The intra-day and the inter-day relative standard deviation were less than 10%.The lowest limit of detection of valproate was 0.3 μg/mL.Conclusion This method was convenient and accurate for the blood concentration monitoring of therapeutic drugs.
【Key words】 valproic acid; chromatography,high performance liquid; plasma concentration;
- 【文献出处】 河北医科大学学报 ,Journal of Hebei Medical University , 编辑部邮箱 ,2013年11期
- 【分类号】R96
- 【被引频次】1
- 【下载频次】2