| UPLC-MS/MS测定beagle犬内西罗莫司血药浓度 |
| 投稿时间：2010-10-10 修订日期：2011-03-31 点此下载全文 |
| 引用本文：陈咏,林晨,张晶,邱彬,周欣,宋洪涛.UPLC-MS/MS测定beagle犬内西罗莫司血药浓度[J].药学实践杂志,2011,29(5):353~355,375 |
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| 中文摘要:目的 建立测定beagle犬内西罗莫司(SRL)血药浓度的UPLC-MS/MS联用方法。 方法 色谱柱为Agilent C18柱(50 mm × 2.1 mm,1.7 μm,);预柱为C18柱(4.0 mm × 3.0 mm,5 μm);流动相为乙腈-水(90:10,v/v);流速为 0.30 ml/min;柱温为50℃;进样室温度为4 ℃。离子源为ESI源;正离子方式检测;扫描方式为多反应监测(MRM);用于定量分析的离子反应分别为m/z 936.6→m/z 409.7(西罗莫司)和m/z 826.6→m/z 415.4(内标他克莫司)。取全血样品经液-液萃取后进样20 μl。 结果 SRL在0.50~12.00 ng/ml浓度范围内呈良好的线性(r=0.999 7),定量下限0.5 ng/ml,日内、日间精密度(RSD)均小于15%,方法回收率均大于90%,萃取回收率大于76%。 结论 本方法具有样品处理简单,方法灵敏、快速、选择性强,满足西罗莫司在beagle犬体内药物检测的要求。 |
| 中文关键词:西罗莫司 超高效液相色谱-质谱联用 血药浓度 |
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| Determination of sirolimus in whole blood of beagle dog by UPLC-MS/MS |
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| Abstract:Objective To develop a UPLC-MS/MS method for the determination of sirolimus in whole blood of beagle dog. Methods Sirolimus and internal standard Tacrolimus were extracted from whole blood with liquid-liquid extraction,then separated on a Agilent C18 column (50 mm ×2.1 mm,1.7 μm) at the flow-rate of 0.30 ml/min. The mobile phase was Acetonitrile-water (90∶10) and the column temperature was 50 ℃. Electrospray ionization ( ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 936.6→409.7 and m/z 826.6→415.4 were used to quantify sirolimus and the internal standard,respectively. Results The calibration linea range of blood-Sirolimu concentrations was 0.50~12.00 ng/ml(r=0.999 7).The low limit of quantification was 0.50 ng/ml . The intra-and inter-day precisions (RSDs) were less than 15%. The method recoveries were more than 90% . The extraction recoveries were more than 76%. Conclusions The method was specific,sensitive,rapid and suitable for the pharmacokinetic study of sirolimus in whole blood of beagle dog. |
| keywords:sirolimus UPLC-MS/MS whole blood |
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