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目的建立大鼠血浆中奥氮平和盐酸氟西汀的LC-MS/MS同时测定方法。方法血浆样品在碱性条件下用乙醚提取浓缩后,采用XDB-CN(2.1 mm′150 mm I.D.,5μm)柱进行分离,流动相为乙腈-10 mmol/L乙酸铵(p H=4.0)=55:45(v/v);ESI选择性反应正离子模式检测,氯雷他定作为内标。结果奥氮平在0.25~400 ng/m L范围内相关系数r=0.9979,最低检测限为0.10 ng/ml,日内、日间精密度分别为2.26%~8.38%及3.54%~7.37%;盐酸氟西汀在0.50~800ng/ml范围内相关系数r=0.9976,最低检测限为0.20 ng/ml,日内、日间精密度分别为1.03%~2.52%及3.26%~7.29%。结论本方法灵敏度高、专属性强、准确性好,符合生物样品的分析要求。
Objective To establish a method for the simultaneous determination of olanzapine and fluoxetine hydrochloride in rat plasma by LC-MS / MS. Methods The plasma samples were extracted with ethyl ether under basic condition, and then separated by XDB-CN (2.1 mm’150 mm ID, 5 μm). The mobile phase was acetonitrile-10 mmol / L ammonium acetate (p H = 4.0) 55:45 (v / v); ESI selective positive ion mode detection, loratadine as internal standard. Results The correlation coefficient of olanzapine in the range of 0.25-400 ng / m L was 0.9979 with the detection limit of 0.10 ng / ml. The intra-day and inter-day precision was 2.26% -8.88% and 3.54% -7.37%, respectively. The correlation coefficient of fluoxetine in the range of 0.50 ~ 800ng / ml was r = 0.9976, the lowest detection limit was 0.20 ng / ml, the intra-day and inter-day precision was 1.03% ~ 2.52% and 3.26% ~ 7.29%, respectively. Conclusion The method has high sensitivity, specificity and accuracy, and meets the requirements of biological samples analysis.