超快速液相色谱-串联质谱法测定胎盘灌流液中的安替比林  

Determination of Antipyrine in Placental Perfusate by UFLC-MS /MS

作　　者：黄桦[1] 姚勤[1] 闫晨[2] 郑巧玲[1] 王晶晶[1] 张峻[1] 

机构地区：[1]昆明医科大学第一附属医院临床药学科,昆明650032 [2]昆明医科大学,昆明650032

出　　处：《中国药学杂志》2013年第15期1319-1322,共4页Chinese Pharmaceutical Journal

基　　金：云南省应用基础研究面上项目(2008ZC128M)

摘　　要：目的建立超快速液相色谱-串联质谱（UFLC-MS／MS）测定胎盘灌流液中安替比林浓度。方法以艾司唑仑为内标，胎盘灌流液样品用乙腈沉淀蛋白后进样分析。色谱柱为Shim-pack XR-ODS ⅡC18柱（2．0mm×75mm，2．2μm），以乙腈和0．1％（V／V）甲酸水溶液为流动相进行梯度洗脱，流速0．4mL·min^-1。质谱采用多反应监测（MRM）扫描模式，以电喷雾离子源（ESI）在正离子电离模式下进行测定，安替比林和艾司唑仑的定量分析离子分别为m／z189．2→56．2和m／z295．2→205．2。结果胎盘灌流液中安替比林在1．2-1200ng·mL^-1内线性关系良好（r=0．9993），日内及日间RSD均小于15％，稳定性考察结果良好。结论该方法快速、灵敏、专属性强，可用于胎盘灌流液中安替比林浓度的测定。OBJECTIVE To establish a UPLC-MS/MS method for the determination of antipyrine in placental perfusate. METHODS Sample was precipitated with acetonitrile. Analysis of antipyrine and estazolam（ internal standard） were carried out on a Shimpack XR-ODS Ⅱ C 18 column （2. 0 mm × 75 mm,2. 2 μm）. Gradient elution was adopted using acetonitrile and water（ containing 0. 1% formic acid, V/V） at a flow rate of 0.4 mL · min^-1. Detection was performed with multiple reactions monitoring（MRM） using positive electrospray ionization（ESI） at m/z 189. 2→56. 2 for antipyrine and m/z 295.2→205.2 for estazolam. RESULTS The calibration curve of antipyrine was linear over the range of 1.2 - 1 200 ng mL^- 1 （r = 0. 999 3 ）. Inter- and intra-day RSDs were less than 15% , and the analytes were proven to be stable. CONCLUSION This method is rapid, sensitive and specific,and can be applied to the determination of antipyrine in placental perfusate.

关 键 词：超快速液相色谱-串联质谱 安替比林 胎盘灌流液 

分 类 号：R917[医药卫生—药物分析学]