LC-MS／MS测定益智渗透泵片中有效成分Beagle犬血药浓度方法学研究  

Study on methodology of determination of Yizhi osmotic pump tablets active ingredient in Beagle dog plasma by LC-MS/MS

作　　者：王艳明[1,2] 杜守颖[3,1] 翟永松[4] 陆洋[3] 

机构地区：[1]天津中医药大学,天津300193 [2]哈尔滨医科大学大庆校区,黑龙江大庆163319 [3]北京中医药大学,北京100029 [4]首都医科大学,北京100069

出　　处：《中国中药杂志》2011年第14期1964-1968,共5页China Journal of Chinese Materia Medica

基　　金：国家“重大新药创制”科技重大专项(2009ZX09502-008,2009ZX09308-003)

摘　　要：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 develop a sensitive and specific LC-MS/MS method for determination of Yizhi osmotic pump tablets active ingredient in Beagle dog plasma. Method： Beagle dog plasma pre-treatment methods were established. Geniposide, notoginsenoside R1, ginsenoside Rg1 and Rb1 notoginsenoside molecular ions and fragment ions peaks were separated well and detected synchronously by LC-MS/MS with digoxin as internal standard. Result： Under the selected LC-MS/MS conditions, the characteristic fragment ions of the four components could be well separated and quantified, and the calibration curves showed good linearity within a certain concentration range of each component; extraction recoveries of those four compounds in plasma were higher than 75%, method recoveries were higher than 90%; day precision （RSD〈10%） and inter-day precision （RSD〈15%） were generally fine; freeze-thaw and room temperature experiments showed good stability （RSD〈15%）. Conclusion： The method is proved to be suitable for pharmacokinetic studies of Yizhi active ingredients in Beagle dog plasma.

关 键 词：LC—MS/MS 益智方 渗透泵片 血药浓度 方法学 

分 类 号：R96[医药卫生—药理学]