| 徐卫峰,尹恒.LC-MS/MS法测定大鼠血浆中千层纸素的浓度[J].安徽医药,2016,20(7):. |
| LC-MS/MS法测定大鼠血浆中千层纸素的浓度 |
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| 投稿时间：2016-02-27 录用日期：2016-05-19 |
| DOI：同意录用 |
| 中文关键词: 千层纸素 LC-MS/MS 血药浓度 |
| 英文关键词: oroxylin A LC–MS/MS plasma-drug concentration |
| 基金项目: |
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| 中文摘要: |
| 目的 建立快速且灵敏的液相色谱-串联质谱法(LC-MS/MS)测定大鼠血浆中千层纸素的浓度。方法 色谱分离采用C18色谱柱，甲醇-10mmol/L醋酸铵（77:23,v/v）为流动相，流速1.05mL/min。大鼠血浆加入β-葡萄糖醛酸酶/硫酸酯酶，37℃孵化过夜，再加入内标染料木素及0.1%磷酸溶液，用乙酸乙酯提取，上清液40℃水浴中氮气流吹干，以流动相200?L溶解残渣，进行分析。检测器采用四极杆串联质谱仪，离子源采用电喷雾电离离子源(ESI)，检测方式采用选择反应检测扫描(SRM)，检测离子：千层纸素[M H] 284.9→269.9，内标[M H] 270.9→270.9。结果 千层纸素在5～1000ng/mL范围内，线性关系良好，回收率大于85%，日内和日间的相对标准偏差(RSD)小于15%。结论 建立的LC-MS/MS法符合生物样品分析的要求，可用于研究大鼠灌胃千层纸素后血浆中千层纸素的测定。 |
| 英文摘要: |
| Aim：To develop a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of oroxylin A in rat plasma. Methods: Plasma samples were partitioned with ethyl acetate and centrifuged for sample clean-up after genistin which was added as internal standard and 0.1% phosphoric acid were added. The supernatant was then evaporated to dryness, and the residue was dissolved in 200mL of mobile phase and centrifuged, an aliquot of 20mL was injected into HPLC column. Chromatographic separation was achieved on a C18 column and the mobile phase consisted of methanol and 10 mM ammonium acetate buffer (77:23, v/v) pumped at a flow rate of 1.05mL /min. The mass spectrometer was performed in the selected reaction monitoring (SRM) mode and the transitions selected for quantitation were [M+H]+ 284.9→269.9 for oroxylin A and [M+H]+ 270.9→270.9 for genistin (I.S.), respectively. Results:A liner calibration curve for assay of oroxylin A in rat plasma was obtained in the range of 5～1000ng/mL with the recoveries of at least 90%. Conclusion:The method can be used for the determination of oroxylin A in rat plasma after intragastric administration. |
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