Key Laboratory of Mountain Ecological Restoration and Bioresource Utilization, Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu, PR China.
J Sep Sci. 2010 Dec;33(23-24):3675-82. doi: 10.1002/jssc.201000452.
A method that couples rapid, sensitive, reproducible and accurate ultra-performance LC (UPLC) with quadrupole-TOF-MS was established for the first simultaneous qualitative and quantitative analysis of phenolic compounds in Artemisia minor. Box-Behnken designs (BBDs) were applied as an effective tool to optimise major parameters that influence the resolution of UPLC, including three gradient steps and column temperature. Under optimal UPLC conditions, a total of 23 phenolic compounds in the crude methanol extracts of A. minor were well separated on a Waters Acquity UPLC BEH C(18) column (100×2.1 mm, 1.7 μm particle size) within 16.5 min, and the compounds were unequivocally or tentatively identified via comparisons with authentic standards and literature. In this study, a total of six major phenolic compounds were quantified in A. minor and the method was validated to be sensitive, precise and accurate within the LOD from 1.24 to 5.27 μg/mL, and the overall intra- and inter-day variations in detection were less than 3.76%. The recovery of the method ranged from 97.9 to 103.8% with RSDs that were less than 5.8%. These results demonstrate that this approach has the potential for quality control of A. minor and other Tibetan herbal medicines.
首次建立了一种将快速、灵敏、重现性好且准确的超高效液相色谱（UPLC）与四极杆飞行时间质谱（quadrupole-TOF-MS）相结合的方法，用于同时定性和定量分析小艾草中的酚类化合物。Box-Behnken 设计（BBD）被应用为一种有效的工具，以优化影响 UPLC 分辨率的主要参数，包括三个梯度步骤和柱温。在最优的 UPLC 条件下，在 Waters Acquity UPLC BEH C(18)柱（100×2.1mm，1.7μm 粒径）上，小艾草粗甲醇提取物中的 23 种酚类化合物在 16.5min 内得到了很好的分离，并通过与对照品和文献的比较，对这些化合物进行了明确或暂定的鉴定。在本研究中，小艾草中的 6 种主要酚类化合物进行了定量分析，该方法被证明具有较高的灵敏度、精密度和准确度，检测限从 1.24 到 5.27μg/mL，日内和日间的总变异系数小于 3.76%。该方法的回收率为 97.9%至 103.8%，RSD 小于 5.8%。这些结果表明，该方法有望用于小艾草和其他藏药的质量控制。
