目的 研究北苍术药材中苍术素、苍术酮和β-桉叶醇的GC测定及特征图谱研究方法,为科学评价其质量提供依据。方法 采用GC色谱法,以Agilent HP-5毛细管色谱柱,载气为氮气,FID检测器,程序升温,分流进样,进样口温度250 ℃,检测器温度250 ℃,柱温130 ℃;外标法,测定承德与其他市场采购的25批北苍术样品中苍术素、苍术酮和β-桉叶醇的量;建立特征图谱并利用中药色谱指纹图谱评价系统进行相似度分析。结果 建立了北苍术药材苍术素、苍术酮和β-桉叶醇量测定和GC特征图谱研究方法,指认了9个特征峰;β-桉叶醇线性范围20.00～406.10 μg/mL(r=0.999 9),平均加样回收率为100.75%,RSD为1.17%,最低检测限0.12 ng;苍术酮线性范围35.00～348.70 μg/mL(r=0.999 5),平均加样回收率为99.84%,RSD为1.29%,最低检测限0.04 ng;苍术素线性范围在16.46～329.30 μg/mL(r=0.999 6),平均加样回收率为100.12%,RSD为0.88%,最低检测限0.06 ng。结论 建立的苍术素、苍术酮、β-桉叶醇定量测定和特征图谱方法简便、灵敏、稳定性和重复性良好,测定结果准确可靠。

Objective To study the content determination of atractylodin, atractylon, and β-eudesmol in Atractylodis Rhizoma by GC and characteristic spectrum in order to provide a scientific basis for the quality control. Methods Using GC and Agilent HP-5 capillary column, taking nitrogen as carrier gas, FID as detector, temperature programming, split ratio, injection port temperature: 250 ℃, detector temperature: 250 ℃, column temperature: 130 ℃; The contents of atractylodin, atractylon and β-eudesmol of 25 samples between Chengde and purchased from other markets were determined by external standard method. The characteristic spectrum was set up and the similarity was analyzed by Estimating System of Similarity on the Chinese Medicine Fingerprint Chromatogram. Results The determination method and characteristic spectrum by GC for atractylodin, atractylon, and β-eudesmol in Atractylodis Rhizoma were established. Nine characteristic peaks were identified; The linear range of β-eudesmol was 20.00 - 406.10 μg/mL (r = 0.999 9), and the average recovery was 100.75%, RSD = 1.17% (n = 6), and the limit of detection was 0.12 ng. The linear range of atractylon was 35.00 - 348.70 μg/mL (r = 0.999 5), and the average recovery was 99.84%, RSD = 1.29% (n = 6), and the limit of detection was 0.04 ng; The linear range of atractylodin was 16.46 - 329.30 μg/mL (r = 0.999 6), and the average recovery was 100.12%, RSD = 0.88% (n = 6), and the limit of detection was 0.06 ng. Conclusion The concent determination and characteristic spectrum method of atractylodin, atractylon, and β-eudesmol established by this study are sensitive, simple, stability, which could make the determination result accurate and reliable.