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目的:建立简单、快速、自动化的在线固相萃取液质联用法定量测定比格犬血浆中的知母皂苷B-Ⅱ。方法:血浆样品直接进样,通过自灌的不锈钢固相萃取柱实现萃取富集过程。采用柱切换技术将被分析物在线洗脱至分析柱上实现色谱分离,最后经过电喷雾电离(ESI)源进入Finnigan线性离子肼质谱仪(LTQ),以选择离子反应(SRM)模式进行负离子检测。结果:知母皂苷B-Ⅱ的线性范围为0.98～1000 ng.mL-1,最低定量下限为0.98 ng.mL-1。日内、日间精密度(RSD)分别小于7.9%和14.2%,准确度(RE)在-1.2%～11.2%范围内。结论:该方法成功用于比格犬口服5 mg.kg-1知母皂苷B-Ⅱ后的药代动力学研究。
OBJECTIVE: To establish a simple, rapid and automated on-line solid phase extraction coupled with mass spectrometry for the quantitative determination of timosaponin B-Ⅱ in beagle dogs plasma. METHODS: Plasma samples were directly injected and the extraction and enrichment process was achieved by self-priming stainless steel SPE columns. The column was switched to elute the analyte to the analytical column for chromatographic separation. Finally, the electrospray ionization (ESI) source was used to enter the Finnigan linear ion-hydrazine mass spectrometer (LTQ) and negative ion detection (SRM) . Results: The linear range of timosaponin B-Ⅱ was 0.98-1000 ng.mL-1, and the lowest limit of quantitation was 0.98 ng.mL-1. The intra-day and inter-day precision (RSD) were less than 7.9% and 14.2%, respectively, and the accuracy (RE) ranged from -1.2% to 11.2%. Conclusion: This method was successfully used to study the pharmacokinetics of Beagle dogs treated with 5 mg.kg-1 timosaponin B-Ⅱ.