液相色谱-串联质谱测定尿液中奥普力农的浓度

Determination of Olprinone in Urine by HPLC-MS-MS Assay

目的建立尿液中奥普力农浓度的测定方法。方法采用LC-MS/MS法,以Agilent ZORBAX Eclipse Plus C1(84.6mm×150mm,5μm)为色谱柱;柱温:40℃;流动相为乙腈-40mmol/L甲酸铵(含0.04%甲酸)(体积比80∶20),流速:0.8ml/min,奥普力农尿样品经流动相稀释。样品经电喷雾离子源正离子化后,通过三重四级杆串联质谱仪,采用选择性反应监测对奥普力农(m/z251.0→155.0)和内标米力农(m/z212.1→140.0)进行测定。结果奥普力农在25～2000μg/L范围呈良好的线性关系,r=0.999(n=7),定量限浓度为25μg/L,相对回收率均>84.28%,日内RSD小于15%,色谱峰保留时间为1.746min。结论方法灵敏、准确、快速、特异性强,适用于奥普力农药动学研究。

Objective To establish an LC-MS/MS method for the determination of the olprinone content in the urine. Methods An LC-MS/MS method was adopted. Olprinone in urine was diluted with mobile phase and analyzed on a Agilent ZORBAX Eclipse Plus C18 [4.6 mm×150 mm, 5 um）column. The mobile phase was consisted of acetonitrile and 40 mmol/L of ammonium formate （including 0.04% formic acid） （80：20） with the flow rate of 0.8 ml/min and the column temperature of 40%. An Agilent 6410 triple quadrupole mass spectrometer system equipped with an electrospray ionization ion-trap source was used as the detector. The system was operated in the selected reaction monitoring mode transmitting m/z 251.0→155.0 transitions for both the olprinone and the internal standard. Results There was a good linearity over the concentration range of 25-2000 ug/L （r= 0.999, n=7）. The quantization limit of this method was 25 ug/L, and the relative recovery was more than 84.28%. The intra-day precision was less than 15%, and the chromatographic peak tR was 1.746 min. Conclusion The method is sensitive, accurate, rapid, and suitable for the determination of olprinone in human urine.