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目的:建立高效毛细管电泳(HPCE)测定白术中白术内酯Ⅰ(Atractylenolide-1)含量的方法。方法:运用高效毛细管电泳方法,熔融石英毛细管(75μm ID×50 cm),缓冲液为50 mmol·L-1硼砂缓冲液,检测波长:210 nm,分离电压:20 k V,柱温25℃,用0.45μm微孔滤膜过滤后进样,压力进样:50 mbar×5 sec。结果:方法最低检测浓度为0.5μg·ml-1,线性范围2~100μg·ml-1,r=0.996,线性关系良好。日内RSD为1.3%,日间RSD为2.5%,平均回收率分别为97.1%。结论:本法简单、灵敏经济,可作为白术中白术内酯Ⅰ的含量的测定。
Objective: To establish a method for the determination of Atractylenolide-1 in Atractylodes macrocephalae with high performance capillary electrophoresis (HPCE). Methods: High-performance capillary electrophoresis was used. The fused silica capillary tube (75 μm ID × 50 cm) was filled with 50 mmol·L-1 borax buffer at a detection wavelength of 210 nm. The separation voltage was 20 kV and the column temperature was 25 ℃. After filtering with 0.45μm microporous membrane, the sample was injected under pressure: 50 mbar × 5 sec. Results: The minimum detectable concentration was 0.5μg · ml-1 with a linear range of 2 ~ 100μg · ml-1 and r = 0.996. The linearity was good. The intraday RSD was 1.3% and the intraday RSD was 2.5%. The average recovery rates were 97.1%. Conclusion: This method is simple, sensitive and economical and can be used as the determination of the content of Atractylodes I in Atractylodes macrocephalae.