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
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篇名: 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
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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 μL。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RSD<2%(n=6或n=7);平均加样回收率分别为98.27%、99.98%,RSD分别为1.96%、1.84%(n=9)。结论:该方法操作简单、结果准确、稳定性和重复性好,适用于苗药了哥王中伞形花内酯和西瑞香素含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for content determination of umbelliferone and daphnoretin in ethanol extract of Miao medicine Wikstroemia indica simultaneously. METHODS: HPLC method was adopted. The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-0.2% phosphoric acid solution (gradient elution) at a flow rate of 1.0 mL/min. The detection wavelength was set at 324 nm during 0-15 min and 346 nm during >15-45 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.
期刊: 2018年第29卷第17期
作者: 冯果,李玮,何新,吴增光,郑传奇
AUTHORS: FENG Guo,LI Wei,HE Xin,WU Zengguang,ZHENG Chuanqi
关键字: 了哥王;苗药;高效液相色谱法;伞形花内酯;西瑞香素;含量测定
KEYWORDS: Wikstroemia indica; Miao medicine; HPLC; Umbelliferone; Daphnoretin; Content determination
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