Agricultural Bio-pharmaceutical Laboratory, College of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China; Key Laboratory of Bee Products for Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Institute of Apicultural Research, Chinese Academy of Agricultural Sciences, Beijing 100093, China.
Agricultural Bio-pharmaceutical Laboratory, College of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Sep 1;1125:121710. doi: 10.1016/j.jchromb.2019.06.037. Epub 2019 Jul 2.
We developed an online solid phase extraction procedure using a hydrophilic-lipophilic balance sorbent, with reversed-phase liquid chromatography-high-resolution mass spectroscopy for the determination of oxcarbazepine and its active metabolite licarbazepine in plasma samples. The analytes were detected using a high-resolution Q Orbitrap mass spectrometer with targeted-selected ion monitoring (t-SIM) in positive scan mode. Under the optimized conditions, the method was linear with R values >0.99. The method was linear from 0.008 to 2.000 μg mL and the lower limit of quantification was 0.008 μg mL for both oxcarbazepine and licarbazepine. Recoveries ranged from 92.34 to 104.27% and from matrix-matched samples from 94.26 to 104.19%. The intraday and interday precision RSD values were <9.13% with an associated accuracy of 92.71 to 104.06%. The total time for the one step online procedure was only 8 min. This method provides a direct and accurate measurement for therapeutic drug monitoring of oxcarbazepine and its active metabolite licarbazepine.
我们开发了一种在线固相萃取程序，使用亲水-疏水平衡吸附剂，结合反相液相色谱-高分辨率质谱法，用于测定血浆样品中的奥卡西平和其活性代谢物拉卡巴西。使用高分辨率 Q Orbitrap 质谱仪，在正扫描模式下采用靶向选择离子监测（t-SIM）进行检测。在优化条件下，该方法的线性相关系数（R 值）大于 0.99。奥卡西平和拉卡巴西的线性范围分别为 0.008 至 2.000 μg/mL，定量下限均为 0.008 μg/mL。回收率范围为 92.34%至 104.27%，基质匹配样品的回收率范围为 94.26%至 104.19%。日内和日间精密度的相对标准偏差（RSD）值均小于 9.13%，准确度为 92.71%至 104.06%。一步在线程序的总时间仅为 8 分钟。该方法为奥卡西平和其活性代谢物拉卡巴西的治疗药物监测提供了直接、准确的测量方法。
