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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 ,适用于药代动力学和治疗药物监测的研究
Objective: To establish a method for the determination of serum olanzapine by high performance liquid chromatography electrochemical detection. Methods: The olanzapine homologue LY170222 was used as internal standard. After the serum was alkalified, it was extracted with diethyl ether in one step and then dried in nitrogen. The sample was dissolved with a mobile phase of quantitation. Using InertsilODS - 3 column separation, BIO-RAD16 40 electrochemical detector detection, detection voltage 0 34V. The mobile phase was a mixture of methanol and 50 mmol·L -1 KH 2 PO 4 -Na 2 HPO 4 buffer (pH = 5 98) (60:40). Results: The chromatographic peaks of olanzapine and internal standard LY170 2 2 2 of the test compound were correlated with the “S” curve of the test voltage. The test voltage should be greater than 0 30V to obtain a stable peak height. Olanzapine and internal standard peak height ratio and serum olanzapine concentration linearly correlated, r = 0 9999, linear range 0 5 ~ 32 μg · L-1. The detection limit of olanzapine was 80 pg, the lowest detection concentration was 0 2 5 μg · L-1, the recoveries were between 80% and 97%, RSD 4 17% ~ 5 76% and day RSD 28% 12 2 1%. Conclusion: This method has high sensitivity, precision and specificity, suitable for pharmacokinetic and therapeutic drug monitoring research