摘要
目的 :建立测定血清奥氮平浓度的高效液相色谱电化学检测法。方法 :以奥氮平的同系物LY170 2 2 2为内标 ,待测血清经碱化后 ,乙醚一步提取 ,氮气吹干 ,用定量流动相溶解后进样。采用InertsilODS - 3柱进行分离 ,BIO-RAD16 40型电化学检测器检测 ,检测电压 0 34V。流动相为甲醇与 5 0mmol·L-1KH2 PO4 -Na2 HPO4 缓冲液 (pH =5 98)的混合液 (6 0∶40 )。结果 :被测化合物奥氮平和内标LY170 2 2 2的色谱峰高均与检测电压呈“S”型曲线相关 ,检测电压应大于 0 30V才能得到稳定的峰高。奥氮平与内标峰高比和血清奥氮平浓度直线相关 ,r=0 9999,线性范围 0 5～ 32 μg·L-1。奥氮平的最低检测限 80pg ,最低检测浓度 0 2 5 μg·L-1,提取回收率在 80 %～ 97%之间 ,日内RSD 4 17%～ 5 76 % ,日间RSD 2 8%～ 12 2 1%。结论 :本法具有较高的灵敏度、精密度和特异性 。
Objective:To develop a method for the determination of olanzapine in serum utilizing high-performance liquid chromatography with electrochemical detection(HPLC-ECD).Method:HPLC-ECD amperometric detection was used with LY170222 as the internal standard.The serum samples were basified with Na 2CO 3 solution and extracted with distilled diethyl ether.The organic phase was evaporated to dryness with N 2 stream,and the residues were dissolved with mobile phase.The compounds were separated on an inertsil ODS-3 column.The mobile phase was composed of methanol and 0 05 mol·L -1 KH 2PO 4-Na 2HPO 4 buffer(60∶40).Results:The relationships between the peak heights of olanzapine and LY170222 and the detection voltages were two “S” shaped curve lines.To get stable peak heights,the detection voltage should be higher than 0 30 V.The peak height ratio of olanzapine and LY170222 with olanzapine serum concentration was linear within the range of 0 5～32 μg·L -1 , r =0 999 9.The lowest detection limit was 80 pg and the lowest concentration detected was 0 25 μg·L -1 .The extraction recovery of olanzapine and LY170222 were 80%～97%.The intra assay variance was less than 6%.The inter assay variance was 2 8%～12 21%。Conclusion:The method is sensitive,precise,reproducible and specific,and can be used in the pharmacological research and therapeutic monitoring of olanzapine.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2000年第5期304-307,共4页
Chinese Journal of Pharmaceutical Analysis
