HPLC法同时测定白术挥发油中5种抗肿瘤成分含量

目的: 建立HPLC法同时测定白术挥发油中苍术酮、β-桉叶醇、白术内酯Ⅰ、Ⅲ、β-榄香烯含量。 方法: 采用Hypersil ODS2(4.6 mm×250 mm,5 μm)色谱柱;流动相乙腈(A)-水(B)60∶ 40,梯度洗脱 ;流速为1.0 mL·min^-1,柱温30 ℃;检测波长:0~9 min时200 nm(白术内酯Ⅲ、 β-桉叶醇),9.1~20 min时220 nm(白术内酯Ⅰ),20.1~45 min时200 nm(苍术酮、 β-榄香烯)。 结果: 苍术酮浓度在0.10~1.00 mg·mL^-1;β-桉叶醇、白术内酯Ⅰ、Ⅲ、 β-榄香烯浓度分别在20.00~1000.00,3.00~150.00,4.00~120.00,0.20~40.00 μg·mL^-1范围内呈良好线性关系(r≥0.9998);各组分低、中、高浓度平均加样回收率在98.5%~102.0%之间,RSD(n=3)≤2.3%;重复性良好,RSD(n=6)≤1.6%。 结论: 本法简便、准确可靠,可用于同时测定挥发油中苍术酮、β-桉叶醇、白术内酯Ⅰ、Ⅲ、β-榄香烯的含量。

Objective: To develop an HPLC method to determine atractylon,β-eudesmol,atractylenolidⅠ,atractylenolidⅢ and β-elemene in Atractylodes macrocephala Koidz volatile oil. Method: The method was carried out by Hypersil ODS2 column(250 mm×4.6 nm,5 μm),using acetonitrile(A)-water(B) 60∶ 40 as mobile phase with gradient elution(0-30 min,40%B→10%B;30-40 min,10%B→10%B),at a flow rate of 1.0 mL·min^-1.The detection wavelength was set at 200 nm(β-eudesmol,atractylenolidⅢ)(0-9 min),220 nm(atractylenolidⅠ)(9.1-20 min) and 200 nm(atractylon,β-elemene)(20.1-45 min).The column temperature was 30 ℃. Results: The linear relationship was good for atractylon in the range of 0.100-1.000 mg·mL^-1,and for β-eudesmol,atractylenolid Ⅰ,atractylenolid Ⅲ and β-elemene in the range of 20.00-1000.00,3.00-150.00,4.00-120.00 and 0.20-40.00 μg·mL^-1 (r≥0.9998).The average recoveries(n=3)of the five investigated compounds at low,medium and high concentration levels were in the range of 98.5%-102.0%(RSD≤2.3%).The repeatability(n=6)were good(RSD≤1.6%). Conclusion: The method was simple,accurate and reliable.It could be used to determinate the contents of atractylon,β-eudesmol,atractylenolidⅠ,atractylenolid Ⅲ and β-elemene in volatile oil.