School of Pharmacy, Shanxi Medical University, Taiyuan, P. R. China.
J Sep Sci. 2018 Sep;41(18):3614-3621. doi: 10.1002/jssc.201800285. Epub 2018 Aug 20.
A sodium dodecyl sulfate sensitized switchable solvent liquid-phase microextraction method was developed and applied to the preconcentration of active alkaloids in Rhizoma coptidis followed by high performance liquid chromatography determination. Before extraction, nonionic triethylamine was converted to its cationic form in the presence of carbon dioxide. Then, the ionic solvent carrying target analytes was once more reverted to its nonionic form by adding sodium hydroxide, as well as phase separation and analytes enrichment were realized simultaneously. Several parameters affecting the approach, such as concentration of sodium dodecyl sulfate, extraction solvent volume, sodium hydroxide concentration, sample phase pH, injection solvent type, and extraction time, were investigated and optimized. The possible microextraction mechanism of double micelle supramolecular inclusion was explored. Under the optimum conditions, the enrichment factors of four protoberberine alkaloids were from 101.8 to 152.0. The linear ranges (with r ≥ 0.990) were 0.032-4.23, 0.031-4.33, 0.0026-10.04, and 0.0013-4.13 μg/mL for epiberberine, coptisine, palmatine, and berberine, respectively. The detection limits were in the range of 0.16-0.32 ng/mL. Satisfactory accuracies (recoveries 98.8-104.6%) and precisions (RSDs 1.9-10.9%) were also obtained. The results showed that the approach is rapid, effective, eco-friendly, and easy-to-handle for the enrichment and detection of active alkaloids in Rhizoma coptidis.
建立了一种十二烷基硫酸钠敏化的可切换溶剂液相微萃取方法,并将其应用于黄连中活性生物碱的预浓缩,然后进行高效液相色谱测定。在萃取之前,非离子三乙胺在二氧化碳的存在下转化为其阳离子形式。然后,通过加入氢氧化钠,将携带目标分析物的离子溶剂再次转化为非离子形式,同时实现了相分离和分析物的富集。研究并优化了影响该方法的几个参数,如十二烷基硫酸钠的浓度、萃取溶剂的体积、氢氧化钠的浓度、样品相的 pH 值、注入溶剂的类型和萃取时间。探讨了双胶束超分子包合的可能微萃取机制。在最佳条件下,四种原小檗碱类生物碱的富集因子为 101.8-152.0。四种原小檗碱类生物碱的线性范围(r≥0.990)分别为 0.032-4.23、0.031-4.33、0.0026-10.04 和 0.0013-4.13μg/mL;表小檗碱、黄连碱、巴马汀和小檗碱的检测限分别为 0.16-0.32ng/mL。还获得了令人满意的准确度(回收率 98.8-104.6%)和精密度(RSDs 1.9-10.9%)。结果表明,该方法快速、有效、环保、易于操作,可用于黄连中活性生物碱的富集和检测。