摘要
目的建立一种同时检测人体内奥氮平与帕罗西汀血清浓度的LC-MS/MS法。方法以乙酸乙酯为提取剂,奥氮平-D_3和帕罗西汀-D_4为内标,采用液-液萃取法处理血样,色谱柱:Agilent Eclipse plus C_(18)柱(100 mm×4.6 mm,5μm),流动相为甲醇-水体系(85∶15,含5 mmol·L^(-1)甲酸铵),流速为0.5 mL·min^(-1),采用电喷雾离子源(ESI),选择性正离子监测(MRM)分析,对方法进行验证,并应用于临床检测。结果奥氮平、帕罗西汀的线性范围分别为1~150μg·L^(-1)(R2=0.999 0),0.5~250μg·L^(-1)(R^2=0.998 1),4个不同质控浓度水平(定量下限,低、中、高浓度)的批内(n=6)和批间(n=3)精密度RSD值均≤12.68%,提取回收率均>67.63%。结论本方法血清用量少,灵敏度高,符合临床生物样本分析要求,可高效测定人体内奥氮平与帕罗西汀的血清浓度。
AIM To establish a method for the simultaneous determination of concentration of olanzapine and paroxetine in human serum by LC-MS/MS. METHODS Olanzapine-D3 and paroxetine-D4 were employed as the internal standard,and the mobile phase consisted of methanol and water（85： 15, 5 mmol· L^-1 ammonium format） at the flow rate of 0.5 mL· min^-1. The analytes were separated by Agilent Eclipse plus C18 column （100 mm × 4.6 mm,5 μm）after being treated with the liquid-liquid extraction method. The simultaneously detective method was performed with multiple reactions monitoring（MRM） using positive eletrospray ionization （ESI）. The method was validated, and to apply in clinical practice. RESULTS The calibration curves for olanzapine and paroxetine were 1 -150 μg· L^-1（R2 =0.999 0） （ n = 6） and intra-day （ n = 3 ） for four coveries were greater than 67.63%. 0.5 - 250 μg · L^-1 （R^2 = 0. 998 1 ） , respectively. The RSD of inter-day different concentration levels were less than 12.68% , and the extraction reCONCLUSION This method is consistent with requirements of clinical bio- logical sample analysis with high sensitivity and less serum use, which is suitable for clinical determination of olanzapine and paroxetine in human serum efficiently.
出处
《中国临床药学杂志》
CAS
2017年第3期168-172,共5页
Chinese Journal of Clinical Pharmacy
基金
广东省自然科学基金(编号2015A030313808)
韶关市卫生计生科研项目立项课题(编号Y16055)
