枳术颗粒多指标成分含量测定及化学计量学分析

Content determination and chemometric analysis of multi-index components in Zhizhu granules

目的:建立高效液相色谱法同时测定枳术颗粒中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、柚皮素、川陈皮素、白术内酯Ⅲ7个指标性成分的含量,同时结合化学计量学分析为其质量评价提供参考依据。方法:采用Waters Symmetry C18色谱柱(250 mm×4.6 mm, 5μm),流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱,流速1.0 mL·min^(-1),检测波长220 nm(白术内酯Ⅲ)、280 nm(芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、柚皮素)和332 nm(川陈皮素),柱温30℃,进样体积10μL。采用统计分析软件对含量测定结果进行聚类分析、主成分分析与正交偏最小二乘法判别。结果:24批枳术颗粒中各成分分离度较好,在考察的线性范围内浓度与峰面积呈良好的线性关系(r>0.999 9),平均回收率在87.6%~114.3%。24批枳术颗粒存在一定差异,筛选出4个差异性成分柚皮苷、橙皮苷、新橙皮苷和柚皮素。24批枳术颗粒供试样品中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、柚皮素、川陈皮素、白术内酯Ⅲ的含量依次为0.378 4~1.380 1、5.125 8~18.137 6、0.283 9~1.195 8、4.490 3~22.585 0、0.022 5~0.349 8、0.063 3~0.211 4和0.054 7~0.137 5 mg·g^(-1)。结论:所建立的方法准确可靠,重复性强,可为枳术颗粒的质量控制提供参考依据。

Objective:To establish an HPLC method for simultaneous determination of seven components(nariru⁃tin,naringin,hesperidin,neohesperidin,naringenin,nobiletin and atractylenolideⅢ)in Zhizhu granules.And to provide reference for its quality evaluation by using chemometric analysis.Methods:The chromatographic col⁃umn Waters Symmetry C_(18)(250 mm×4.6 mm,5μm)was adopted using HPLC-DAD.The mobile phase consis⁃ted of acetonitrile(A)-0.1%phosphoric acid(B)in gradient elution with flow rate of 1.0 mL·min^(-1),the detection wavelength were 220 nm(atractylenolideⅢ),280 nm(narirutin,naringin,hesperidin,neohesperidin and naringenin)and 332 nm(nobiletin).The column temperature was set at 30℃and the injection volume was 10μL.Cluster analysis,principal component analysis and orthogonal partial least squares-discrimination analy⁃sis were used to distinguish the content determination results.Results:The resolution of each component in 24 batches of Zhizhu granules was good,and the linear relationship between concentration and peak area was good(r>0.9999).The average recoveries were within 87.6%-114.3%.There were some differences in 24 batches of Zhizhu granules,and 4 different components were screened out,which were naringin,hesperidin,neohesperidin and naringin.The contents of narirutin,naringin,hesperidin,neohesperidin,naringenin,nobiletin and atractylenolideⅢin 24 batches of Zhizhu granules samples were 0.3784-1.3801 mg·g^(-1),5.1258-18.1376 mg·g^(-1),0.2839-1.1958 mg·g^(-1),4.4903-22.5850 mg·g^(-1),0.0225-0.3498 mg·g^(-1),0.0633-0.2114 mg·g^(-1) and 0.0547-0.1375 mg·g^(-1),respectively.Conclusion:The established method is accurate,reliable and reproducible,which can provide reference for the quality control of Zhizhu granules.