麸炒白术配方颗粒特征图谱及白术内酯Ⅲ含量测定研究

Study on HPLC Specific Chromatogram of Bran-processed Atractylodes Formula Granule and Determination of Atractylenolide Ⅲ

关键词:  麸炒白术配方颗粒  白术内酯Ⅲ  含量测定  特征图谱  质量研究

Key words:  bran-processed Atractylodes Formula granule  atractylenolide Ⅲ  content determination  specific chromatogram  quality study

摘要:

目的 建立麸炒白术饮片和麸炒白术配方颗粒中白术内酯Ⅲ的含量测定方法，并同时建立麸炒白术配方颗粒的HPLC特征图谱。方法 采用色谱柱为Welch Xtimate C₁₈柱（250 mm×4.6 mm，5 μm）；流动相为乙腈-水溶液，梯度洗脱；体积流量1.0 mL·min^-1；柱温30℃；检测波长224 nm；进样量10 μL。结果 建立了麸炒白术饮片及颗粒中白术内酯Ⅲ的含量测定方法，白术内酯Ⅲ在0.031 3~0.782 4 μg内与色谱峰面积呈良好的线性关系；麸炒白术饮片和麸炒白术配方颗粒平均加样回收率分别102.0%（RSD=1.88%），101.0%（RSD=1.02%）；建立了麸炒白术配方颗粒的HPLC特征图谱，确立了8个特征峰。结论 该方法准确、可靠，为麸炒白术配方颗粒的工艺研究及质量控制提供了参考依据。

Abstract:

OBJECTIVE To establish an HPLC method for the determination of atractylenolide Ⅲ in bran-processed atractylodes and bran-processed Atractylodes Formula granule, and to establish the specific chromatogram of bran-processed Atractylodes Formula granule. METHODS The chromatographic separation was performed on a Welch Xtimate C₁₈ column (250 mm×4.6 mm, 5 μm). The mobile phase was a mixture of acetonitrile-water in gradient elution at a flow rate of 1.0 mL·min^-1. The detection wavelength was 224 nm and the column temperature was set at 30℃. RESULTS The linear range of atractylenolide Ⅲ in bran-processed atractylodes and bran-processed Atractylodes Formula granule was 0.031 3-0.782 4 μg, with average recovery of 102.0%(RSD=1.88%) and 101.0%(1.02%). The HPLC specific chromatogram of bran-processed Atractylodes Formula granule showed 8 characteristic peaks. CONCLUSION The method is reliable and accurate, and can provide a reference for the technical study and quality control of bran-processed Atractylodes Formula granule.