Chen Xuan, Wang Jin, Hu Shuang, Bai Xiaohong
School of Pharmacy, Shanxi Medical University, Taiyuan, China.
J Sep Sci. 2016 Mar;39(5):827-34. doi: 10.1002/jssc.201501160. Epub 2016 Feb 19.
A new hollow-fiber double-solvent synergistic microextraction method was proposed for the extraction and concentration of trace active compounds in traditional Chinese medicine. The main variables affecting the method were investigated and optimized. Under the optimized conditions, linearities were 0.01-10 μg/mL, detection limits were lower than 0.8 ng/mL, and interday, and intraday relative standard deviations were <9.20%. Furthermore, average recoveries ranged from 102.8 to 104.1%, and enrichment factors were 6-70 for the four alkaloids tested. The antitumor alkaloid group in Coptis chinensis was screened and identified by hollow-fiber cell fishing with high-performance liquid chromatography. The four alkaloids were then enriched and quantified by hollow-fiber double-solvent synergistic microextraction with high-performance liquid chromatography. The mechanism of the proposed microextraction method was described, and results demonstrated that the approach was a simple and reliable sample-preparation procedure. This method, as well as hollow-fiber cell fishing combined with high-performance liquid chromatography can be adopted to study the different characteristic effects of the multiple components and multiple targets of traditional Chinese medicine. The approach can also be used to conduct tailored quality control of the active compounds associated with therapeutic efficacy.
提出了一种新的中空纤维双溶剂协同微萃取方法，用于中药中痕量活性成分的萃取和富集。对影响该方法的主要变量进行了研究和优化。在优化条件下，线性范围为0.01 - 10μg/mL，检测限低于0.8ng/mL，日间和日内相对标准偏差均<9.20%。此外，四种被测生物碱的平均回收率在102.8%至104.1%之间，富集因子为6 - 70。采用中空纤维细胞垂钓-高效液相色谱法对黄连中的抗肿瘤生物碱组进行了筛选和鉴定。然后通过中空纤维双溶剂协同微萃取-高效液相色谱法对这四种生物碱进行富集和定量。阐述了所提出的微萃取方法的机理，结果表明该方法是一种简单可靠的样品制备方法。该方法以及中空纤维细胞垂钓结合高效液相色谱法可用于研究中药多成分、多靶点的不同特征效应。该方法还可用于对与治疗效果相关的活性成分进行定制质量控制。
