Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, P. R. China.
Tianjin Key Laboratory of Phytochemistry and Pharmaceutical Analysis, Tianjin University of Traditional Chinese Medicine, Tianjin, P. R. China.
J Sep Sci. 2019 Jul;42(14):2426-2434. doi: 10.1002/jssc.201900227. Epub 2019 May 28.
An industrial MCM-41-miniaturized matrix solid-phase dispersion extraction coupled with response surface methodology was explored to determine L-epicatechin, typhaneoside, isorhamnetin-3-O-neohespeidoside, naringenin, kaempferol, and isorhamnetin in Pollen typhae by ultra-high performance liquid chromatography connected to a photodiode array detection. Several variables were optimized in detail, including mesh number of sieve, type of adsorbent, mass ratio of sample to adsorbent, grinding time, methanol concentration, and elution volume. Central composite design was applied to optimize the best conditions for the maximum yields of the total flavonoids. The results displayed a good linear relationship (R > 0.9992) and the recoveries ranged from 92.9 to 103% (RSD < 4.53%) of the six flavonoids. The optimal method with high efficiency and low consumption was obviously better than heating reflux and ultrasonic extraction. It was proven that the developed industrial MCM-41-miniaturized matrix solid-phase dispersion extraction coupled with simple ultra-high performance liquid chromatography method could be a rapid and efficient tool for extraction and determination of flavonoids in natural products.
采用工业 MCM-41-微型化基质固相分散萃取结合响应面法,通过超高效液相色谱与光电二极管阵列检测联用,对蒲黄中 L-表儿茶素、 typhaneoside、异鼠李素-3-O-新橙皮苷、柚皮苷、山柰酚和异鼠李素进行测定。详细优化了几个变量,包括筛目数、吸附剂类型、样品与吸附剂的质量比、研磨时间、甲醇浓度和洗脱体积。采用中心组合设计优化了最大产率的最佳条件。结果表明,六种黄酮类化合物的线性关系良好(R > 0.9992),回收率在 92.9%至 103%之间(RSD < 4.53%)。与加热回流和超声提取相比,高效、低耗的最佳方法明显更好。证明了开发的工业 MCM-41-微型化基质固相分散萃取结合简单的超高效液相色谱法可以成为提取和测定天然产物中黄酮类化合物的快速、有效的工具。