目的 建立测定附桂骨痛胶囊中新乌头碱、乌头碱和次乌头碱的HPLC-MS分析方法。方法 采用HPLC-MS，色谱柱为Polaris C₁₈-A柱（50 mm×2.0 mm，5 μm），流动相为甲醇-水（90∶10），体积流量0.2 mL/min，质谱检测采用电喷雾电离源，正离子方式检测。结果 新乌头碱、乌头碱和次乌头碱分别在0.464～3.944 μg/mL（r＝0.999 6）、81.6～816 ng/mL（r＝0.999 4）、0.482～6.748 μg/mL（r＝0.999 7）线性关系良好，平均回收率分别为98.8%（RSD 3.1%）、98.1%（RSD 3.3%）、98.4%（RSD 3.3%）（n＝6）。结论 该方法是一种快速、灵敏、准确的分析方法，可以为附桂骨痛胶囊的质量控制提供科学依据。

Objective To establish an HPLC-MS method for determining mesaconitine, aconitine, and hypaconitine in Fugui Gutong Capsula. Methods The separation was performed using HPLC-MS mothod with Polaris C₁₈-A column (50 mm × 2.0 mm, 5 μm) with the mobile phase of CH₃OH-H₂O (90:10) at flow rate of 0.2 mL/min. The detection was done by positive-ion electrospray ionization mass spectrometry. Results The linear ranges were 0.464—3.944 μg/mL (r = 0.999 6) for mesaconitine, 81.6—816 ng/mL (r = 0.999 4) for aconitine, and 0.482—6.748 μg/mL (r = 0.999 7) for hypaconitine, respectively. The average recoveries were 98.8% (RSD = 3.1%) for mesaconitine, 98.1% (RSD = 3.3%) for aconitine, and 98.4% (RSD = 3.3%) for hypaconitine, respectively (n = 6). Conclusion A rapid, sensitive, and accurate method for the determination of mesaconitine, aconitine, and hypaconitine in Fugui Gutong Capsula is set up. The study may provide a scientific basis for the quality control of Fugui Gutong Capsula.

国家“十一五”科技支撑计划重大专项课题（2006BAE01A01-12）；西南科技大学博士研究基金项目（08zx7110）；西南科技大学青年基金项目（09zx3129）