在线固相萃取LC-MS/MS法测定比格犬血浆中的知母皂苷B-Ⅱ  

Quantification of timosapanin B-Ⅱ in Beagle plasma by an on-line solid-phase extraction procedure combined with liquid chromatography/electrospray ionization tandem mass spectrometry

作　　者：陈方[1] 王清清[1] 戴舒佳[1] 赵阳[2] 马百平[2] 孙效[3] 欧伦[1] 宋海峰[1] 汤仲明[1] 

机构地区：[1]军事医学科学院放射与辐射医学研究所药理毒理研究室,北京100850 [2]军事医学科学院放射与辐射医学研究所植物化学研究室,北京100850 [3]解放军总后勤部丰台综合仓库药材供应站,北京100071

出　　处：《药物分析杂志》2012年第11期1908-1913,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：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 develop a simple, automatic and rapid quantification method for the determination of timosaponin B -Ⅱ in Beagle plasma. Methods： Raw plasma samples were directly loaded onto a home - packed stainless solid -phase extraction （SPE） column, followed with a timed valve - switching event and elution proce- dure. The analyte was eluted on -line to a reversed -phase high -performance liquid chromatography （RP - HPLC ） column and subsequently introduced into a linear ion trap mass spectrometer, LTQ - MS, via electrospray i- onization （ESI） interface. The negative charged compounds were specified and quantitatively analyzed using selec- tive reaction monitoring（SRM） mode. A single analysis run took about 4. 7 min. Results： The standard curves for timosaponin B -Ⅱ were linear over the concentration range of 0. 98 - 1000 ng mL-1. The lower limit of quantifi- cation （LLOQ） was 0. 98 ng mL- 1. The intra - and inter - batch precisions for timosaponin B -Ⅱ at three quality control levels were less than 7.9% and 14. 2% ,respectively. The accuracy ranged from - 1. 2% to 11.2%. Con- clusion： The method was successfully applied in the pharmacokinetic（PK） study on Beagles with oral administra- tion of a single dose of 5 mg kg-1 timosaponins B -Ⅱ.

关 键 词：甾体皂苷 液质联用法 药代动力学 在线固相萃取 定量分析 比格犬血浆 知母皂苷 

分 类 号：R917[医药卫生—药物分析学]