Yang Zhichao, Xu Xueyu, Sun Lingxia, Zhao Xue, Wang Hao, Fawcett John Paul, Yang Yan, Gu Jingkai
School of Life Sciences, Jilin University, Changchun 130012, PR China.
School of Pharmacy, University of Otago, Dunedin, PO Box 56, New Zealand.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 May 1;1020:36-42. doi: 10.1016/j.jchromb.2016.03.013. Epub 2016 Mar 15.
A rapid and sensitive assay based on supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS) has been developed and validated for the determination of oxcarbazepine (OXC) and its chiral metabolite licarbazine (Lic) in beagle dog plasma using carbamazepine as internal standard. Chiral analysis in a run time of only 3 min was performed on an ACQUITY UPC(2) ™ Trefoil™ CEL2 column (3.0 × 150 mm, 2.5 μm) at 50 °C by isocratic elution with a mobile phase of supercritical carbon dioxide (purity ≥ 99.99%) and methanol (60:40, v/v) at a flow rate of 2.3 mL/min. The assay was linear over the concentration ranges 5-1000 ng/mL for OXC and 0.5-100 ng/mL for the enantiomers of Lic with corresponding lower limits of quantitation of 5 ng/mL and 0.5 ng/mL. Intra- and inter-day precisions were in the range 0.78-14.14% with accuracies in the range -10.80% to 0.42%. The method was successfully applied to a pharmacokinetic study involving a single oral administration of 16 mg/kg OXC as Trileptal(@) tablets to beagle dogs.
已开发并验证了一种基于超临界流体色谱-串联质谱（SFC-MS/MS）的快速灵敏分析方法，以卡马西平为内标，用于测定比格犬血浆中的奥卡西平（OXC）及其手性代谢物利卡巴嗪（Lic）。在ACQUITY UPC(2) ™ Trefoil™ CEL2柱（3.0×150 mm，2.5μm）上，于50℃通过等度洗脱进行手性分析，流动相为超临界二氧化碳（纯度≥99.99%）和甲醇（60:40，v/v），流速为2.3 mL/min，运行时间仅为3分钟。该分析方法在OXC浓度范围为5 - 1000 ng/mL以及Lic对映体浓度范围为0.5 - 100 ng/mL时呈线性，相应的定量下限分别为5 ng/mL和0.5 ng/mL。日内和日间精密度范围为0.78 - 14.14%，准确度范围为 - 10.80%至0.42%。该方法成功应用于一项药代动力学研究，该研究涉及给比格犬单次口服16 mg/kg的OXC（商品名：曲莱(@)片）。
