| 摘要: |
| 目的:建立高效液相色谱-质谱联用测定全血中环孢霉素A含量的方法.方法:色谱柱为Hypersil C8 (4.6 mm×150 mm,5 μm),流动相为乙腈-醋酸溶液(Ph 4.5)7030,流速为1.0 ml·min-1,柱后分流比82,柱温为65℃,进样量10 μl;质谱条件为电喷雾电离源(ESI),正离子选择离子监测,毛细管电压为4 000 V,干燥气流速为8.0 L·min-1,干燥气温度为350℃,雾化器压力为30 psi,裂解器电压为140 V.结果:环孢霉素A在26.68 ～1 067 μg·L-1范围内线性方程为y=0.001 1x-0.004 6(r=0.999 3),最低检测浓度为4.35 μg·L-1,低、中、高3种浓度的相对回收率分别为(89.81±4.91)﹪、(104.5±3.73)﹪、(95.17±2.33)﹪,绝对回收率分别为(77.64±4.38)﹪、(78.01±3.79)﹪、(83.02±1.59)﹪,日内、日间RSD均＜6﹪,150 d内稳定性试验结果,RSD均＜5﹪.结论:该法操作快速、简便、灵敏度高、专属性强,适用于环孢霉素A临床血药浓度监测. |
| 关键词: 环孢霉素A、色谱法,高效液相、光谱分析,质量 |
| DOI：10.3724/SP.J.1008.2006.00899 |
| 投稿时间：2005-12-25修订日期：2006-06-23 |
| 基金项目:第二军医大学青年启动基金(05QN42). |
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| High-performance liquid chromatography/tandem mass spectrometry for determination of cyclosporin A level in whole blood |
| WANG Bin,LI Xiang,CHAI Yi-feng,ZHANG Guo-qing |
| (第二军医大学药学院药物分析学教研室,上海,200433;第二军医大学东方肝胆外科医院药材科,上海,200438) |
| Abstract: |
| Objective： To establish a high performance liquid chromatography/tandem mass spectrometry （HPLC-MS） method for determination of cyclosporin A level in the whole blood. Methods： A Hypersil C8 column （65 ℃, 4.6 mm × 150 mm, 5 μm） was used with a mobile phase of acetonitrile-acetic acid （pH 4.50） 70 ： 30 at a flow rate of 1.0 ml · min^-1. Atomospheric pressure electronic spray ionization was used to quantify cyclosporin A, with the capillary voltage being 4 000 V, the flow of drying gas being 8.0 L · min^-1 , nebulizer pressure being 30 psi, and fragment voltage being 140 V. Results： The calibration curve of cyclosporin A was linear in a range of 26.68 -1 067 μg · L^-1 ： y=0. 001 1x-0. 004 6（r=0. 999 3）. The lowest limit of detection was 4. 35 μg · L^-1. The method recoveries of low, medium and high concentrations cyclosporin A were （89.81±4.91）%, （104.5±3.73）%, and （95. 17±2.33）%, respectively; the extraction recoveries of 3 concentrations were （77.64 ± 4.38）%, （78.01 ±3.79）%, and （83.02±1.59）%, respectively. The intra-day and inter-day RSD was less than 6%, and the RSD was less than 5% in 150 days. Conclusion： The present method is fast, sensitive and selective. It is suitable for clinical monitoring of cycolsporin A. |
| Key words: cycolsporin A chromatography, high pressure liquid spectrum analysis , mass |
