高效液相色谱法测定白术中白术内酯Ⅰ、II、Ⅲ的含量

Determination of Atractylenolide Ⅰ,Ⅱ and Ⅲ in Rhizoma Atractylodis Macrocephalae by High Performance Liquid Chromatography

关键词:  白术  白术内酯Ⅰ  白术内酯Ⅱ  白术内酯Ⅲ  含量

Key words:  Rhizoma Atractylodis Macrocephalae  atractylenolideⅠ  atractylenolide Ⅱ  atractylenolide Ⅲ  content

摘要:

本实验建立了高效液相色谱技术(HPLC)测定白术中白术内酯Ⅰ、Ⅱ、Ⅲ的含量。采用Hypersil GOLD (250 mm×4.6 mm，5um)，以乙腈为流动相A、以0.1％磷酸溶液为流动相B进行梯度洗脱，流速1.0 mL/min，白术内酯Ⅰ检测波长为276 nm，白术内酯Ⅱ、白术内酯Ⅲ检测波长为220 nm，柱温为35 ℃，进样体积为20 μL。白术内酯Ⅰ在0.10～1.60 μg范围内线性关系良好，平均回收率为99.29%(RSD=2.25%)；白术内酯Ⅱ在0.10～1.60 μg范围内线性关系良好，平均回收率为100.07%(RSD=2.59%)；白术内酯Ⅲ在0.10～1.60 μg范围内线性关系良好，平均回收率为100.43%(RSD=2.20%)。结果表明该方法分离度好、准确度高、重现性好，可测定白术中白术内酯Ⅰ、Ⅱ、Ⅲ的含量。

Abstract:

This experiment established a high-performance liquid chromatography (HPLC) technique to determine the content of atractylenolide I, II, and III in Rhizoma Atractylodis Macrocephalae. Adopting Hypersil GOLD (250mm × 4.6mm, 5um), using acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B for gradient elution, with a flow rate of 1.0 mL/min. The detection wavelength of atractylenolide I was 276nm, atractylenolide II and III were 220nm, and the column temperature was 35℃. The injection volume was 20ul. The linear relationship of atractylenolide I within the range of 0.10 to 1.60ug is good, with an average recovery rate of 99.29% (RSD=2.25%); The linear relationship of atractylenolide II within the range of 0.10 to 1.60ug is good, with an average recovery rate of 100.07% (RSD=2.59%); The linear relationship of atractylenolide III within the range of 0.10 to 1.60ug is good, with an average recovery rate of 100.43% (RSD=2.20%). The results indicate that this method has good separation, high accuracy, and good reproducibility, and can be used to determine the content of atractylenolide I, II, and III in Rhizoma Atractylodis Macrocephalae.