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[摘要]
目的 建立梯度洗脱联合波长切换高效液相色谱(HPLC)法对参苓健体粉中去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ和白术内酯Ⅰ同时进行测定。方法 采用Venusil MP C18色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈-0.05%磷酸溶液,梯度洗脱;检测波长:210 nm(0~19 min,检测去氢土莫酸、去氢茯苓酸和茯苓酸)、220 nm(19~35 min,检测白术内酯Ⅲ和白术内酯Ⅰ);体积流量:0.8 mL/min;柱温:30℃;进样量为10 μL。结果 去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ、白术内酯I质量浓度分别在4.62~92.40 μg/mL(r=0.999 7)、3.80~76.00 μg/mL(r=0.999 9)、5.76~115.20 μg/mL(r=0.999 9)、3.95~79.00 μg/mL(r=0.999 8)、5.05~101.00 μg/mL(r=0.999 6)与峰面积关系良好;回收率分别为99.24%、97.75%、98.66%、98.49%、99.10%,RSD值分别为1.23%、1.79%、1.66%、0.80%、1.25%。结论 建立的方法操作简便、结果可靠,可用于参苓健体粉的质量控制。
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[Abstract]
Objective To develop an HPLC-wavelength switching method for simultaneous determination of dehydrotumulosic acid, dehydropachymic acid, pachymic acid, atracylenolide Ⅲ, and atracylenolide I in Shenling Jianti Powder. Method The Venusil MP C18 column (250 mm×4.6 mm, 5 μm) was adopted; the mobile phase was acetonitrile-0.05% phosphoric acid solution with gradient elution, with a flow rate of 0.8 mL/min. The column temperature was set at 30℃, and injection volume was 10 μL. Results Dehydrotumulosic acid, dehydropachymic acid, pachymic acid,atracylenolide Ⅲ and atracylenolide I had good linearity in the ranges of 4.62-92.40 μg/mL (r=0.999 7), 3.80-76.00 μg/mL (r=0.999 9), 5.76-115.20 μg/mL (r=0.999 9), 3.95-79.00 μg/mL (r=0.999 8), and 5.05-101.00 μg/mL (r=0.999 6), respectively. The average recoveries were 99.24%, 97.75%, 98.66%, 98.49%, and 99.10% with RSD of 1.23%, 1.79%, 1.66%, 0.80%, and 1.25%, respectively. Conclusion The method is rapid and with high accuracy which can be applied to the quality control of Shenling Jianti Powder.
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