论文部分内容阅读
目的建立优化的HPLC方法同时测定不同产地罗布麻药材中芦丁、金丝桃苷、异槲皮苷以及槲皮素含量。方法采用Shiseido C18(3.0μm,3.0 mm×100 mm)色谱柱;以乙腈:甲醇=10:1作为A相-0.1%甲酸水溶液作为B相,梯度洗脱(0~4 min,5%→16%A;4~15 min,16%→23%A;15~20 min,23%→35%A;20~22 min,35%→55%A),流速0.6 ml.min-1;二极管阵列检测器检测波长:360 nm;柱温:30℃;进样量:5μl。结果芦丁、金丝桃苷、异槲皮苷、槲皮素在22 min内基线分离,线性范围分别为0.308 4~30.84μg.ml-1(r=0.999 9),0.877 6~87.76μg.ml-1(r=0.999 9),0.902 0~90.20μg.ml-1(r=0.999 9),0.249 8~24.98μg.ml-1(r=0.999 9)。方法学考察表明,日内和日间精密度、最低检测限和定量限的范围均符合相关标准,加样回收率(n=3)分别为:芦丁102.0%、96.40%、103.8%;金丝桃苷98.50%、101.0%、102.9%;异槲皮苷98.40%、100.4%、101.4%;槲皮素104.4%、103.1%、103.5%。测定了9个产地的罗布麻中4个黄酮类成分的含量。结论本法快速,准确、简便,具有良好的重复性,可以为罗布麻药材质量控制提供依据。
Objective To establish an optimized HPLC method for simultaneous determination of rutin, hyperoside, quercetin and quercetin in Apocynum venetum L. from different areas. Methods The chromatographic column was Shiseido C18 (3.0 μm, 3.0 mm × 100 mm). The column was eluted with gradient elution (0-4 min, 5% → 16 % A; 4-15 min, 16% → 23% A; 15-20 min, 23% → 35% A; 20-22 min, 35% → 55% Detector detection wavelength: 360 nm; column temperature: 30 ℃; injection volume: 5μl. Results Rutin, hyperoside, isoquercetin and quercetin were separated within 22 min. The linear range was 0.308 4 ~ 30.84 μg.ml-1 (r = 0.999 9) and 0.877 6 ~ 87.76 μg respectively. ml-1 (r = 0.999 9), 0.902 0-90.20 μg.ml-1 (r = 0.999 9), 0.249 8-24.98 μg.ml-1 (r = 0.999 9). The methodological study showed that the precision, the minimum detectable limit and the limit of quantification within the range of day, day and day were in accordance with relevant standards. The recoveries (n = 3) were: rutin 102.0%, 96.40%, 103.8% Peach glycosides 98.50%, 101.0%, 102.9%; isoquercitrin 98.40%, 100.4%, 101.4%; quercetin 104.4%, 103.1%, 103.5%. The content of 4 flavonoids in Apocynum was determined. Conclusion The method is rapid, accurate, simple and reproducible, which can provide the basis for the quality control of Apocynum venetum.