| 摘要: |
| 目的：建立液相色谱-串联质谱法测定家兔血浆中倍他米松含量。方法：血浆样品经乙醚-正己烷（41，V/V）液-液萃取，以乙腈-5 mmol/L醋酸铵-甲酸（80200.1，V/V/V）为流动相，Zorbax Eclipse XDB-C18柱分离；采用电喷雾电离源，以多反应监测（MRM）方式进行正离子检测，用于定量分析的离子反应分别为m/z 393m/z 373和m/z 393m/z 355 （倍他米松）和m/z 406m/z 247 （内标，A0）。结果：测定血浆中倍他米松方法的线性范围为15.0~1 000 pg/ml，定量下限为15.0 pg/ml，日内、日间精密度（RSD）均小于13.0%，准确度（RE）在-1.4%~-0.6%以内。应用本法对家兔经皮给予二丙酸倍他米松乳膏后的药动学进行研究，结果显示Tmax为(11.0±5.3) h，Cmax为(167±28) pg/ml，AUC0-t为(4.24±1.68) ng·h·ml-1。结论：该法选择性强、灵敏度高，适用于二丙酸倍他米松乳膏剂的药代动力学研究。 |
| 关键词: 二丙酸倍他米松 倍他米松 乳膏剂 液相色谱-串联质谱法 |
| DOI：10.3724/SP.J.1008.2008.00326 |
| 投稿时间：2007-11-05修订日期：2008-01-14 |
| 基金项目: |
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| Liquid chromatography/tandem mass spectrometry in determination of betamethasone concentration in rabbit plasma |
| DENG Pan1,CHEN Xiao-yan2,DAI Xiao-jian2,LI San-ming1* |
| (1.Department of Physics and Chemistry,Shenyang Pharmaceutical University,Shenyang 110016,China;2.Center of Drug Metabolism and Pharmacokinetics Research,Shanghai Institute of Materia Medica,Chinese Academy of Sciences,Shanghai 201203) |
| Abstract: |
| Objective：To set up a liquid chromatographic-tandem mass spectrometric (LC/MS/MS) method for determination of betamethasone in rabbit plasma.Methods: Betamethasone and the internal standard A0 were extracted from rabbit plasma by liquid-liquid extraction with diethyl ether-hexane (41,V/V). Chromatographic separation was performed on a Zorbax Eclipse XDB-C18 column with a mobile phase consisted of acetonitrile-5 mmol/L ammonium acetate-formic acid (80200.1,V/V/V) at a flow-rate of 0.60 ml/min. A tandem mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 393m/z 373 and m/z 393m/z 355 for betamethasone,and m/z 489m/z 357 for the internal standard. Results: The linear calibration curves were obtained within the concentration range of 15.0- 1 000 pg/ml. The lower limit of quantification was 15.0 pg/ml. The intra- and inter-day relative standard deviation over the entire concentration range was less than 13.0%. The accuracy was in the range of -1.4% to -0.6% in terms of relative error. The method was applied to a pharmacokinetic study of betamethasone dipropionate cream in rabbits. Maximal betamethasone plasma level was observed after (11.0±5.3) h and the Cmax was (167±28) pg/ml,AUC0-t was (4.24±1.68) ng·h·ml-1 after percutaneous administration of 0.5 g betamethasone dipropionate. Conclusion: This method is selective and sensitive,and can be used for the purpose of the pharmacokinetic study of betamethasone dipropionate cream. |
| Key words: betamethasone dipropionate betamethasone cream liquid chromatography-tandem mass spectrometry |
