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出 处:《药物分析杂志》2011年第6期1106-1110,共5页Chinese Journal of Pharmaceutical Analysis
基 金:山西省卫生厅科技攻关项目(200833)
摘 要: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HypersilODS2(4.6 mm×250 mm,5μm)色谱柱;流动相乙腈(A)-水(B)60∶40,梯度洗脱[0~30 min,40%B→10%B;30~40 min,10%B→10%B];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20.00~1000.00,3.00~150.00,4.00~120.00,0.20~40.00μg.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 andβ-elemene in volatile oil.
关 键 词:白术挥发油 苍术酮 Β-桉叶醇 白术内酯Ⅰ 白术内酯Ⅲ Β-榄香烯 HPLC
分 类 号:R917[医药卫生—药物分析学]
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