LC-MS/MS法测定Beagle犬血浆中右旋酮洛芬的浓度

LC-MS/MS determination of dexketoprofen in Beagle dog plasma

目的:建立LC-MS/MS法测定Beagle犬血浆中右旋酮洛芬的浓度。方法:血浆样品采用乙腈沉淀法处理,取上清液进样。以乙腈(每500 mL中加入甲酸10μL)-水(80∶20,v/v)为流动相;用Zorbax Eclipse SB-C18柱(5μm,150 mm×4.6 mm)色谱柱分离;以布洛芬为内标。流速0.5 mL·min-1;进样量25μL;柱温为室温。质谱检测采用ESI正离子模式,扫描方式为多反应监测,扫描离子对m/z右旋酮洛芬253.0/209.0,布洛芬204.8/160.8。结果:右旋酮洛芬的线性范围为1.0～1000 ng·mL-1,线性关系良好(r=0.9979),最低定量下限为1.0 ng·mL-1,绝对回收率在100.0%～104.3%之间,变异系数均小于6%。结论:该方法预处理快速简单,灵敏度高,所建立的LC-MS/MS法准确、可靠,可用于犬血浆中右旋酮洛芬的浓度测定及药代动力学研究。

Objective ：To establish an LC - MS/MS method for determination of dexketoprofen in beagle dog plasma. Methods：The plasma samples were deposited by acetonitrile before analysis. 25 uL supernatant was performed on a Zorbax Eclipse SB -C18 analytical column （5 um,150 mm ×4.6 mm） using acetonitrile （10 uL formic acid per 500 mL acetonitrile） -water （80： 20,v/v） as the mobile phase. The flow rate was 0.5 mL ·min-1. The mass spectrometer was operated under the positive ionmode and multiple reaction monitoring with the transitions of m/z 253.0/209.0 and m/z 204. 8/160. 8 was used to qualify dexketoprofen and ibuprofen （internalstandard）,respectively. Results：The linear calibration curve was obtained in the range of 1.0 - 1000 ng· mL-1. The lower limit of quantification was 1.0 ng · mL-1. Accuracy in the mesurement of quality control samples were in the range of 100.0% -104. 3%. Conclusion：This method is simple, rapid and sensitive and can be used for determination of dexketoprofen in Beagle dogs plasma and pharmacokinetical study.