一测多评法定量分析薏苡仁药材质量

Quantitative analysis of quality of Coix seed based on one-measure multiple evaluation method

目的:建立薏苡仁药材中7种甘油酯类成分的一测多评分析方法,并结合聚类分析、主成分分析对不同产地、不同市场规格薏苡仁药材进行质量评价。方法:采用Waters Symmetry~?C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-二氯甲烷(6∶40),等度洗脱,流速为1.0 mL/min,柱温30℃,进样量10μL,蒸发光检测器检测;以甘油三油酸酯为内参物,计算甘油三亚油酸酯、1,2-二亚油酸-3-油酸甘油酯、1,2-二亚油酸-3-棕榈酸甘油酯、1,2-二油酸-3-亚油酸甘油酯、1-棕榈酸-2-油酸-3-亚油酸甘油酯、1,2-二油酸-3-棕榈酸甘油酯的相对校正因子,并利用一测多评法测定27批薏苡仁中7种甘油酯类成分的含量。结果:所测7个成分在测定范围内线性关系良好(r>0.999),加样回收率在96.05%~101.75%,相对校正因子的重现性良好,采用相对校正因子计算得到的7种甘油酯类成分的含量与外标法测得值无显著性差异;27批市售薏苡仁的甘油三油酸酯的含量在0.128~1.175 mg/g,不合格率达到了18.4%,反映出市售薏苡仁的质量参差不齐;市售薏苡仁质量与市售规格呈显著正相关。结论:本研究建立的一测多评法准确可靠,可用于薏苡仁药材的质量评价。

Objective:To establish a method of quantitative analysis of multi-components by single marker for the determination of seven kinds of glyceryl esters in Coix seed,and to evaluate the quality of Coix seed from different habitats and market specifications by cluster analysis and principal component analysis.Methods:Waters Symmetry®C18 chromatographic column(4.6 mm×250 mm,5μm)was used,the mobile phase was acetonitrile-dichloromethane(60∶40),the flow rate was 1.0 mL/min,the column temperature was 30℃,the injection volume was 10μL,and the evaporative light detector was used for detection.The relative correction factors of glycerol trioleate,1,2-dioleate-3-oleate glyceride,1,2-dioleate-3-palmitate glyceride,1,2-dioleate-3-linoleate glyceride,1-palmitate-2-oleate-3-linoleate glyceride and 1,2-dioleate-3-palmitate glyceride were calculated with glycerol trioleate as internal reference.The contents of seven glycerides in 27 batches of coix seed were determined by single-marker multi-criterion method.Results:The linearity within the measurement range of the seven components was good(r>0.999),the recovery rate was 96.05%~101.75%,and the reproducibility of the relative correction factor was good.There was no significant difference between the contents of seven glycerides calculated by the relative correction factor and those measured by external standard method.The content of glycerol trioleate in 27 batches of commercially available coix seeds ranged from 0.128~1.175 mg/g,and the unqualified rate reached 18.4%,reflecting the uneven quality of commercially available Coix seeds.There was a significant positive correlation between the quality of commercially available Coix seed and its specifications.Conclusion:The method established in this study is accurate and reliable,and can be used for the quality of Coix seed.