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目的建立Beagle犬血浆中可待因质量浓度的液相色谱-串联质谱(LC-MS/MS)测定方法。方法色谱柱为Agela·C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-水-甲酸(体积比为15∶85∶0.5),血浆样品经甲醇沉淀蛋白处理,以多反应监测(multiple reaction monitoring,MRM)扫描方式检测,测定Beagle犬经口给予洛芬待因缓释片后血浆中可待因的质量浓度。结果血浆中可待因质量浓度在0.2~20μg·L-1内线性关系良好,日内和日间精密度RSD≤11.5%,平均提取回收率为104.1%~109.2%,基质效应为119.2%~128.3%。可待因在Beagle犬血浆中主要药动学参数t1/2为(2.9±0.5)h,ρmax为(8.7±3.4)μg·L-1,AUC0-∞为(28.5±7.3)μg·h·L-1。结论该方法适用于可待因在Beagle犬体内药动学的研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for determination of codeine in plasma of Beagle dogs. Methods The chromatographic column was an Agela C18 column (150 mm × 4.6 mm, 5 μm) with a mobile phase of methanol-water-formic acid (15:85:0.5 by volume). The plasma samples were treated with methanol precipitation and monitored by multi- multiple reaction monitoring (MRM) scanning method was used to determine the mass concentration of codeine in plasma after sustained release tablets of lupivibine in Beagle dogs. Results The linearity of codeine in plasma ranged from 0.2 to 20 μg · L-1. The intra-day and inter-day RSD was less than 11.5%, the average recovery was 104.1% -109.2% and the matrix effect was 119.2% -128.3 %. The major pharmacokinetic parameters of codeine in Beagle dogs were (2.9 ± 0.5) h, (8.7 ± 3.4) μg · L-1 and (28.5 ± 7.3) μg · h · L-1. Conclusion This method is suitable for studying the pharmacokinetics of codeine in Beagle dogs.