College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, P. R. China.
Department of Traditional Chinese Medicine, Hangzhou Red Cross Hospital, Hangzhou, P. R. China.
Electrophoresis. 2020 Jan;41(1-2):123-130. doi: 10.1002/elps.201900244. Epub 2019 Nov 11.
A novel micro matrix solid phase dispersion method was successfully used for the extraction of quaternary alkaloids in Phellodendri chinensis cortex. The elution of target compounds was accomplished with sodium hexanesulfonate as the eluent solvent. A neutral ion pair was formed between ion-pairing reagent and positively charged alkaloids in this process, which was beneficial for selectively extraction of polar alkaloids. Several parameters were optimized and the optimal conditions were listed as follows: silica gel as the sorbent, silica to sample mass ratio of 1:1, the grinding time of 1 min. The exhaustive elution of targets was achieved by 200 µL methanol/water (9:1) containing 150 mM sodium hexane sulfonate at pH 4.5. The method validation covered linearity, recovery, precision of intraday and interday, limits of detection, limits of quantitation, and repeatability. This established method was rapid, simple, environmentally friendly, and highly sensitive.
一种新型的微矩阵固相分散法被成功地应用于提取黄柏中的季铵生物碱。目标化合物的洗脱是用正己烷磺酸钠作为洗脱溶剂来完成的。在这个过程中,离子对试剂与带正电荷的生物碱形成中性离子对,有利于极性生物碱的选择性提取。对几个参数进行了优化,列出了最佳条件如下:硅胶作为吸附剂,硅胶与样品的质量比为 1:1,研磨时间为 1 分钟。通过 200µL 甲醇/水(9:1)在 pH 4.5 下含 150mM 正己烷磺酸钠,可实现目标物的彻底洗脱。方法验证包括线性、回收率、日内和日间精密度、检测限、定量限和重复性。该方法快速、简单、环保、灵敏度高。