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目的:建立利用LC-MS/MS测定益智渗透泵片中有效成分Beagle犬血药浓度的方法。方法:建立Beagle犬血浆前处理方法;以地高辛为内标,LC-MS/MS同时测定有效成分栀子苷、三七皂苷R1、人参皂苷Rg1及三七皂苷Rb1分子离子峰及碎片离子峰,并建立各成分的血药浓度方法学。结果:在选定的LC-MS/MS条件下,4种成分的特征碎片离子可较好的分离并定量,在一定浓度范围内各成分线性良好;血浆中4种成分提取回收率均大于75%,方法回收率均大于90%;日内精密度RSD<10%,日间精密度RSD<15%;冻融及室温稳定性良好(RSD<15%)。结论:本方法灵敏、稳定、可靠,可用于研究益智方有效成分Beagle犬血药动力学过程。
OBJECTIVE: To establish a method for the determination of plasma concentration of Beagle dogs, an active ingredient in the puzzle osmotic pump by LC-MS / MS. Methods: The plasma pretreatment method was established in Beagle dogs. Using digoxigenin as internal standard, simultaneous determination of the ion peaks of geniposide, notoginsenoside Rg1, ginsenoside Rg1 and notoginsenoside Rb1 and fragment ions by LC-MS / MS Peaks and establishing a method of plasma concentration for each component. Results: Under the selected LC-MS / MS conditions, the characteristic fragment ions of the four components could be well separated and quantified. The linearity of the components was good in a certain range of concentration. The recoveries of the four components in plasma were all higher than 75 %, And the recovery rates were all above 90%. The intraday RSD was less than 10%, intraday RSD was less than 15%, and the freeze-thaw stability was good at room temperature (RSD <15%). Conclusion: The method is sensitive, stable and reliable and can be used to study the pharmacokinetics of Beagle dog, the active ingredient of Yizhi Fang.