液相色谱-串联质谱法测定大鼠血浆中的灯盏乙素  

LC-MS/MS determination of scutellarin in rat plasma

作　　者：王莹[1] 杭太俊[1] 庄莹[1] 李丹[1] 吴晓鸾[1] 江丽[1] 邱娟[1] 宋敏[1] 吕文莉[2] 平其能[2] 

机构地区：[1]中国药科大学药物分析室,南京210009 [2]中国药科大学药剂学教研室,南京210009

出　　处：《药物分析杂志》2006年第6期737-740,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家863计划重大科技专项(2004AA2Z3230);江苏省自然科学基金重点项目(BK2001210)

摘　　要：目的:建立大鼠血浆中灯盏乙素的液相色谱-串联质谱测定法,研究大鼠尾静脉注射灯盏花素注射液的药代动力学。方法:血浆样品经含5%甲酸的甲醇溶液提取富集,液相色谱分离[Inertsil ODS-3(250mm×4.6mm,5μm)柱,甲醇-水-甲酸(60:40:0.2)流动相,流速1.0mL·min^(-1)],电喷雾离子化三重四极杆串联质谱负离子选择反应检测(SRM),离子反应分别为 m/z 461.1→m/z 285.1(灯盏乙素)和 m/z 445.1→m/z 269.1(黄芩苷,内标)。碰撞气(Ar)压力为0.186 Pa,碰撞能量25eV。结果:线性范围为0.005～40.0μg·mL^(-1)(r=0.9996),最低定量浓度为5ng·mL^(-1)。灯盏乙素的回收率>80%,日内、日间 RSD 皆小于15%(n=5)。结论:建立的大鼠血浆中灯盏乙素的液相色谱-串联质谱测定法灵敏、准确,可用于大鼠血浆中灯盏乙素浓度测定及临床前药代动力学研究。Objective ：To develop a sensitive and accurate liquid chromatography -tandem mass spectrometry （LC -MS/MS） method for the determination of scutellarin in rat plasma after intravenous administration. Method： Scutellarin and baicalin （ internal standard） were enriched by anhydrous methanol containing 5 % formic acid from freeze - dried plasma samples and separated on an Inertsil - ODS column （250 mm × 4. 6 mm, 5μm） with a mobile phase of methanol - water - formic acid （60： 40： 0. 2） at a flow rate of 1.0 mL · min^-1. LC - MS/MS detection was made with an electrospray negative ionization （ESI） and selected reaction monitoring （SRM）. The transitions selected for quantitation were m/z 461.1→m/z 285. 1 for scutellarin and m/z 445. 1→m/z 269. 1 for baicalin both with Ar CID at 0. 186 Pa and 25 eV. Results：The calibration curve was linear over the concentration rang of 0. 005 to 40. 0 μg·mL^-1. The limit of quantitation was 5 ng · mL^-1. The recovery was over 80% and within - day and between- day RSD less than 15% （n = 5 ）. Condusion：The established LC -MS/MS method is validated to be specific, accurate and sensitive for the pharmacokinetic study of breviscapine in rats after intravenous administration of 7.5 mg·kg^- 1 breviscapine injection.

关 键 词：灯盏乙素 灯盏花素注射液 大鼠血浆药代动力学 液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]