College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding, China.
J Sep Sci. 2017 Dec;40(23):4591-4598. doi: 10.1002/jssc.201700602. Epub 2017 Oct 30.
A novel dispersive admicelle solid-phase extraction method based on sodium dodecyl sulfate-coated Fe O nanoparticles was developed for the selective adsorption of berberine, coptisine, and palmatine in Gegen-Qinlian oral liquid before high-performance liquid chromatography. Fe O nanoparticles were synthesized by a chemical coprecipitation method and characterized by using transmission electron microscopy. Under acidic conditions, the surface of Fe O nanoparticles was coated with sodium dodecyl sulfate to form a nano-sized admicelle magnetic sorbent. Owing to electrostatic interaction, the alkaloids were adsorbed onto the oppositely charged admicelle magnetic nanoparticles. The quick separation of the analyte-adsorbed nanoparticles from the sample solution was performed by using Nd-Fe-B magnet. Best extraction efficiency was achieved under the following conditions: 800 μL Fe O nanoparticles suspension (20 mg/mL), 150 μL sodium dodecyl sulfate solution (10 mg/mL), pH 2, and vortexing time 2 min for the extraction of alkaloids from 10 mL of diluted sample. Four hundred microliters of methanol was used to desorb the alkaloids by vortexing for 1 min. Satisfactory extraction recoveries were obtained in the range of 85.9-120.3%, relative standard deviations for intra- and interday precisions were less than 6.3 and 10.0%, respectively. Finally, the established method was successfully applied to analyze the alkaloids in two batches of Gegen-Qinlian oral liquids.
基于十二烷基硫酸钠包覆的 Fe3O4 纳米粒子的新型分散性混合胶束固相萃取方法，用于高效液相色谱法前对黄连解毒口服液中盐酸小檗碱、盐酸巴马汀和盐酸黄连碱的选择性吸附。Fe3O4 纳米粒子通过化学共沉淀法合成，并通过透射电子显微镜进行表征。在酸性条件下，Fe3O4 纳米粒子的表面包覆有十二烷基硫酸钠，形成纳米级混合胶束磁性吸附剂。由于静电相互作用，生物碱被吸附到带相反电荷的混合胶束磁性纳米粒子上。通过使用 Nd-Fe-B 磁铁，可快速将吸附有分析物的纳米粒子与样品溶液分离。在以下条件下可实现最佳萃取效率：800μL Fe3O4 纳米粒子悬浮液（20mg/mL）、150μL 十二烷基硫酸钠溶液（10mg/mL）、pH2 和涡旋时间 2min，用于从 10mL 稀释样品中萃取生物碱。通过涡旋 1min 用 400μL 甲醇洗脱生物碱。在 85.9-120.3%的范围内获得了令人满意的萃取回收率，日内和日间精密度的相对标准偏差分别小于 6.3%和 10.0%。最后，该方法成功应用于分析两批黄连解毒口服液中的生物碱。
