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高效液相色谱-质谱-质谱联用法测定Beagle狗血浆中石杉碱甲
Determination of Huperzine A in Beagle Dog Plasma by HPLC/MS/MS Method
【摘要】 目的 :建立狗血浆中石杉碱甲的液质联用测定法。方法 :血浆样品经液液萃取 ,用高效液相色谱 质谱 质谱联用法检测。色谱柱为NucleocilODS柱 ,5 0× 2 0mmI D ,5 μm ,流动相为乙腈 甲醇 水 甲酸 (2 0∶4 0∶4 0∶0 1,v/v)。采用多反应监测 ,用于定量的离子为m/z 2 4 3→ 2 10 (石杉碱甲 )和m/z 2 5 7→ 2 2 6 (内标N 甲基石杉碱甲 )。结果 :线性范围为 0 1~ 12ng/ml,最低定量浓度为 0 1ng/ml,可以检测到Beagle狗静注和口服 10 0 μg石杉碱甲后 12h的血药浓度。结论 :该方法灵敏度高 ,简便快速 ,可用于药代动力学研究。
【Abstract】 AIM:To develop HPLC-MS-MS method for the quantification of huperzine A in beagle dog plasma. METHOD:Samples were extracted by liquid-liquid extraction and seperared on a Nucleocil ODS column.The mobile phase is MeOH-CH 3 CN-H2O-HCOOH(20∶40∶40∶0.1, v/v ).Flow rate was 0.2 ml/min.Quantitation was based on multiple reactin monitoring (MRM) using the precursor→product ion combinations of m/z 243→210 and m/z 257→226 for the huperzine A and N -methyl huperzine A respectively.RESULT:The assay range of this method is 0.1~12 ng/ml.The limit of quantification was 0.1 ng/ml.Huperzine A in beagle plasma at 12h after administration of 100 μg via the iv and po could be detected.CONCLUSION:The method is sensitive,simple and rapid.It can be applied to study the pharmacokinetics of huperzine A.
- 【文献出处】 中国药科大学学报 ,Journal of China Pharmaceutical University , 编辑部邮箱 ,2004年03期
- 【分类号】R96
- 【被引频次】16
- 【下载频次】336