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目的:建立犬血浆中冬凌草甲素浓度的LC-MS测定方法,为深入研究冬凌草甲素在犬体内的药代动力学特征提供有效、可靠的检测手段。方法:采用Shim-pack VP-ODS(150 mm×2.0 mm,5μm)色谱柱,以乙腈-水(50∶50)为流动相,HPLC/电喷雾离子源质谱检测(HPLC/ESI-MS),乙酸乙酯作为萃取剂,检测犬血浆中冬凌草甲素的含量,并评价方法的稳定性和重现性。结果:本方法在0.0125~6.4μg.mL-1浓度范围内线性关系良好(R2=0.9994),定量限为0.0125μg.mL-1,平均回收率为71.18%~76.99%,日内精密度为2.4%~5.0%,日间精密度为1.2%~6.3%。室温放置30 min,样品预处理后放置24 h、-24℃贮存14 d及反复冻融3次稳定性良好。其RSD均小于15%。结论:该分析方法可行性高,重现性好,可用于研究冬凌草甲素在犬体内药代动力学特征。
Objective: To establish an LC-MS method for determining the concentration of oridonin in canine plasma, and to provide an effective and reliable method for the further study of the pharmacokinetics of oridonin in dogs. METHODS: HPLC-ESI-MS / MS-MS was performed on a Shim-pack VP-ODS column (150 mm × 2.0 mm, 5 μm) using acetonitrile-water (50:50) Ethyl acetate as extractant, detection of dog plasma content of oridonin, and evaluate the stability and reproducibility of the method. Results: The method showed a good linearity (R2 = 0.9994) in the range of 0.0125-6.4μg.mL-1, the limit of quantification was 0.0125μg.mL-1, the average recovery was 71.18% -76.99%, and the intra-day precision was 2.4 % ~ 5.0%, day precision of 1.2% ~ 6.3%. After 30 min at room temperature, the samples were pretreated for 24 h, stored at -24 ° C for 14 days, and frozen and thawed repeatedly for 3 times. The RSD is less than 15%. Conclusion: This method is highly feasible and reproducible. It can be used to study the pharmacokinetics of oridonin in dogs.