液相色谱-质谱联用测定人血浆中罗哌卡因的浓度

Determination of concentration of ropivacaine in human plasma with LC-MS/MS

目的建立测定人血浆中罗哌卡因浓度的液相色谱质谱联用(LCMS/MS)法。方法血浆样品加入布比卡因内标,经沉淀液(甲醇∶0.1%甲酸水溶液=9∶1)处理后,以甲醇-0.1%甲酸水溶液(70∶30,V/V)为流动相,在0.2mL·min-1的流速下,用ZorbaxC18柱(5cm×2.1mm,5μm)分离。样品经电喷雾离子源(ESI)正离子化后,通过三级四极杆串联质谱仪,以N2为碰撞气,采用多反应离子检测方式测定罗哌卡因(m/z275.2→126.1)和内标布比卡因(m/z289.2→140.3)浓度。结果线性范围为50～2000μg·L-1,最低定量浓度为50μg·L-1,方法的相对回收率在85%～115%之间,日内、日间RSD均<15%。结论该方法快速、简便,特异性强。

AIM To develop an LC-MS/MS method for determination of ropivacaine in human plasma. METHODS Plasma samples were treated by addition of bupivacaine as internal standard and precipitation with methanol-01%formic acid solution(9∶1,V/V),then separated on a Zorbax C 18(5 cm×21 cm,5 μm)column with methanol-0.1% formic acid solutio(70∶30,V/V)as mobile phase,at a flow rate of 02 mL·min -1.A triple quadruple tandem mass spectrometer was used as the detector.Electrospray ionization source was applied and operated in positive ion mode.With N2 as collision gas and multiple reaction monitoring as scan type,ropivacaine and the internal standard bupivacaine were quantitated by monitoring the ion transition of m/z 2752→1261 and m/z 2892→1403 respectively.RESULTS The linear calibration curve was obtained over the concentration range of 50-2 000 μg·L -1 and the lowest limit of quantiation was 50 μg·L -1.The relative recovery was within 85%-115%,and the relative standard deviation of within-day and between-day was less than 15%. CONCLUSION The method proved to be rapid,simple and specific.