液相色谱-质谱法同时测定吴茱萸水提物中吴茱萸碱和吴茱萸次碱的含量

Simultaneous Determination of Evodiamine and Rutaecarpine in Water extracts of Evodia rutaecarpa by LC-MS

目的：建立同时测定吴茱萸水提物中吴茱萸碱（Evodiamine，EVO）和吴茱萸次碱（Rutaecarpine，RUT）的LC/MS方法。方法：液相色谱采用Welch Materials Xtimate-C18色谱柱（2.1 mm ＆#215;150 mm，3μm），以甲醇-10 mmol/L乙酸铵水溶液（85∶15）为流动相，流速0.2 mL/min，柱温30℃。质谱采用正离子全扫描模式，m/z：0～1000，电喷雾离子化源（ESI）。雾化气为氮气，雾化压力为40 psi；喷雾电压4000 V，源温度为100℃；去溶剂气为氮气，温度350℃，流速为10 L/min。结果：吴茱萸碱在2.02～504 ng/mL（r＝0.9992），吴茱萸次碱在1.97～493.33 ng/mL（r＝0.9999）线性关系良好，回收率分别为87.8％～97.04％和86.35％～98.22％，日内、日间精密度均＜10％。结论：该方法简便、可靠、灵敏度高，可用于同时测定吴茱萸水提物中吴茱萸碱和吴茱萸次碱的含量及药代动力学研究。

Objective：To establish a LC-MS method for the simultaneous determination of evodiamine and tutaecarpine in water extracts of Evodia rutaecarpa Methods：A Welch Materials Xtimate-C18 （2.1 mm ＆#215;150 mm,3 μm） was used .The mobile phase consisting of a mixture of methanol and 10 mmol/L ammonium acetate （85：15） was delivered at a flow-rate of 0.2 mL/min.The column temperature was maintained at 30℃.The mass spectrometer was operated under the positive ion mode .Atomization pressure（N2） was 40 psi, volt-age was 4000v and temperature was 100℃.The drying gas （ N2） flow was 10 L/min, the drying gas temperature was 350℃.Results：The linear ranges were 2.02~504 ng/mL （r=0.9992） and 1.97~493.33 ng/mL （r=0.9999） for evodiamine and rutaecarpine .The method extraction recoveries of evodiamine and rutaecarpine were 87.8%~97.04%and 86.35%~98.22%respectively.The intra-and inter -day RSD were also lower than 10%.Conclusion：The method is simple , reliable and sensitive .It can be used for the phar-macokinetics research of water extracts of Evodia rutaecarpa .