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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 a LC-MS / MS method for the determination of dexketoprofen in Beagle dogs plasma. Methods: Plasma samples were treated with acetonitrile precipitation, the supernatant was injected. The separation was performed on a Zorbax Eclipse SB-C18 column (5 μm, 150 mm × 4.6 mm) column with acetonitrile (10 μL of formic acid per 500 mL) -water (80:20, v / v) As an internal standard. Flow rate 0.5 mL · min-1; injection volume 25μL; column temperature was room temperature. The ESI positive ion mode was adopted for the mass spectrometry detection, the multi-reaction monitoring was used for the scanning mode, and the m / z dexketoprofen 253.0 / 209.0 and the ibuprofen 204.8 / 160.8 were scans. Results: The linear range of dexketoprofen was 1.0-1000 ng · mL-1, the linearity was good (r = 0.9979), the lowest limit of quantification was 1.0 ng · mL-1, and the absolute recovery was 100.0% -104.3% The coefficients of variation were all less than 6%. Conclusion: The method is rapid, simple and sensitive. The established LC-MS / MS method is accurate and reliable and can be used to determine the concentration and pharmacokinetics of dexketoprofen in canine plasma.