School of Pharmacy, Shanxi Medical University, Taiyuan, China.
J Sep Sci. 2018 Sep;41(18):3590-3597. doi: 10.1002/jssc.201701504. Epub 2018 Aug 5.
A fast, simple, and efficient salt-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography was developed and introduced for the simultaneous enrichment, extraction, and determination of the trace levels of matrine alkaloids (sophoridine, matrine, and sophocarpine) in Sophorae Flavescentis Radix and Composite Kushen injection. Compared with conventional dispersive liquid-liquid microextraction, the proposed method, with added salt but without dispersant and centrifuging, makes the operation simpler, greener, and leads to a higher enrichment factor. The crucial parameters affecting the enrichment factors of target analytes, such as type and volume of extraction solvent, pH of sample phase, salt concentration, volume of sample phase, and extraction time, were investigated and optimized, meanwhile, the extraction mechanism of the method was analyzed and described. Under the optimized conditions, the enrichment factors of the three matrine alkaloids were 150, 178, and 227, respectively. Good linearities (r ≥ 0.9992) for all analytes, low limits of detection (less than 0.08 ng/mL), satisfactory precisions (2.1-12.3%), and accuracies (recoveries, 99.3-103.9%) were achieved. The experimental results showed that the approach is a simple, fast, green, eco-friendly, and sensitive method and can be used for the preconcentration and determination of matrine alkaloids in traditional Chinese medicines and their preparations.
建立并提出了一种快速、简单、高效的盐辅助分散液液微萃取与高效液相色谱联用技术,用于同时富集、提取和测定苦参药材和复方苦参注射液中苦参碱类(槐定碱、苦参碱和氧化槐果碱)的痕量水平。与传统的分散液液微萃取相比,该方法在操作上更加简单、绿色,且富集因子更高,在萃取过程中添加盐但不使用分散剂和离心。研究并优化了影响目标分析物富集因子的关键参数,如萃取溶剂的类型和体积、样品相的 pH 值、盐浓度、样品相的体积和萃取时间,同时分析并描述了该方法的萃取机理。在优化条件下,三种苦参碱的富集因子分别为 150、178 和 227。所有分析物均具有良好的线性(r≥0.9992)、较低的检出限(均小于 0.08ng/mL)、令人满意的精密度(2.1-12.3%)和准确度(回收率为 99.3-103.9%)。实验结果表明,该方法简单、快速、绿色、环保且灵敏,可用于中药及其制剂中苦参碱类的预浓缩和测定。