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目的:建立灵敏、准确的测定Beagle犬血浆中豆腐果苷浓度的液相色谱-电喷雾离子化-质谱联用(HPLC-ESI-MS)的分析方法,并将其应用于Beagle犬的药动学研究。方法:应用正丁醇作为提取剂的液-液萃取方法。色谱柱为Luna C_(18)(150mm×2.00mm,3.5μm),流动相为乙腈和500μmol·L_1的氯化铵,梯度洗脱程序。四极杆质谱,负离子选择性离子检测方式,检测离子豆腐果苷和内标岩白菜素[M+Cl]~-m/z分别为319.00和363.05。结果:豆腐果苷的最低定量限为5ng·mL_1,本方法在5～2500ng·mL_1浓度范围内线性关系良好。被分析物的批内及批间变异在10.0%以内。豆腐果苷血浆样品在存储、制备和分析过程中稳定性良好。结论:本方法可以准确用来进行豆腐果苷临床前药动学的定性、定量研究,并已经成功地应用于Beagle犬的药动学研究。
Objective: To establish a sensitive and accurate method for the determination of tofuin in plasma of Beagle dogs by liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and apply it to the pharmacokinetics of Beagle dogs Study. Methods: Liquid-liquid extraction using n-butanol as extractant. The chromatographic column was Luna C 18 (150 mm × 2.00 mm, 3.5 μm) with acetonitrile and 500 μmol·L -1 ammonium chloride gradient elution program. Quadrupole mass spectrometry, negative ion selective ion detection, detection of ionic tofuin and endogenous bergenin [M + Cl] ~ -m / z were 319.00 and 363.05, respectively. Results: The lowest limit of quantification for tofuin was 5 ng · mL -1. The method showed good linearity in the range of 5-2500 ng · mL -1. Intra-assay and intra-assay variability of analytes was within 10.0%. Taupiin plasma samples are stable during storage, preparation and analysis. Conclusion: This method can be used accurately and qualitatively in the preclinical pharmacokinetics of tofuin and has been successfully applied to the pharmacokinetics of Beagle dogs.