HPLC—双波长法同时测定苗药了哥王乙醇提取物中伞形花内酯和西瑞香素的含量
含量测定,高效液相色谱法
冯果 李玮 何新 吴增光 郑传奇中图分类号 R917;R284.1 文献标志码 A 文章编号 1001-0408(2018)17-2369-04
DOI 10.6039/j.issn.1001-0408.2018.17.15
摘 要 目的:建立同时测定苗药了哥王乙醇提取物中伞形花内酯和西瑞香素含量的方法。方法:采用高效液相色谱法。色谱柱为Diamonsil C18,流动相为乙腈-0.2%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为0~15 min,324 nm,>15~45 min,346 nm,柱温为30 ℃,进样量为20 ?L。结果:伞形花内酯和西瑞香素的检测进样量线性范围分别为0.33~6.60 μg(r=0.999 7)、0.21~4.20 μg(r=0.999 2);检测限分别为6.60、4.20 ng,定量限分别为18.90、12.60 ng;精密度、稳定性(48 h)、重复性试验的RSD15-45 min. The column temperature was 30 ℃, and injection volume was 20 μL. RESULTS: The linear range was 0.33-6.60 μg for umbelliferone (r=0.999 7) and 0.21-4.20 μg for daphnoretin (r=0.999 2). The detection limits were 6.60 and 4.20 ng, and the limits of quantification were 18.90 and 12.60 ng, respectively; RSDs of precision, stability (48 h) and reproducibility tests were lower than 2% (n=6 or n=7). The average recoveries were 98.27% (RSD=1.96%, n=9) and 99.98% (RSD=1.84%,n=9), respectively. CONCLUSIONS: The method is simple, accurate, stable and reproducible. It is suitable for content determination of umbelliferone and daphnoretin in Miao medicine W. indica simultaneously. ......
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