Feng Yanmei, Li Qian, Qiu Daiyu, Li Guichen
Gansu Provincial Key Laboratory of Aridland Crop Science, College of Agronomy, Gansu Agricultural University, Lanzhou 730070, China.
Molecules. 2021 Apr 21;26(9):2416. doi: 10.3390/molecules26092416.
The content of active components in traditional Chinese medicine is relatively small, and it is difficult to detect some trace components with modern analytical instruments, so good pretreatment and extraction are very important in the experiment. Graphene was introduced by a dispersive liquid-liquid microextraction method based on solidification of floating organic drop (DLLME-SFO) with graphene/1-dodecyl alcohol used as the extractant, and this method, combined with quantitative proton nuclear magnetic resonance spectroscopy (H-qNMR), was used to simultaneously qualitative and quantitative osthole, columbianadin and isoimperatorin in Angelicae Pubescentis Radix. In this experiment, a magnetic stirrer was used for extraction, all NMR spectra were recorded on a Bruker Advance III 600 MHz spectrometer with dimethyl sulfoxide-d (DMSO-d) as deuterated solvent and pyrazine as the internal standard. The influencing factors and NMR parameters in the extraction process were investigated and optimized. In addition, the methodology of the established method was also examined. The quantitative signals of osthole, columbianadin and isoimperatorin were at a chemical shift of δ6.25-δ6.26 ppm, δ6.83-δ6.85 ppm, and δ6.31-δ6.32 ppm. The linear ranges of osthole, columbianadin and isoimperatorin were all 0.0455-2.2727 mg/mL, and R were 0.9994, 0.9994 and 0.9995, respectively. The limits of detection of osthole, columbianadin and isoimperatorin were 0.0660, 0.0720, 0.0620 mg, and the limits of quantification of osthole, columbianadin and isoimperatorin were 0.2201, 0.2401, 0.2066 mg/mL. The solution had good stability and repeatability within 24 h. The recoveries of osthole, columbianadin and isoimperatorin were 102.26%, 99.89%, 103.28%, respectively. The established method is simple and easy to operate, which greatly reduces the cumbersome pretreatment of samples and has high extraction efficiency.
中药中活性成分的含量相对较少，使用现代分析仪器难以检测到一些痕量成分，因此良好的预处理和提取在实验中非常重要。采用基于漂浮有机滴固化的分散液液微萃取法（DLLME-SFO）引入石墨烯，以石墨烯/1-十二醇为萃取剂，将该方法与定量质子核磁共振波谱法（H-qNMR）相结合，用于同时定性和定量独活中的蛇床子素、哥伦比亚内酯和异欧前胡素。本实验采用磁力搅拌器进行萃取，所有核磁共振谱均在Bruker Advance III 600 MHz光谱仪上记录，以氘代二甲亚砜（DMSO-d）为氘代溶剂，吡嗪为内标。研究并优化了萃取过程中的影响因素和核磁共振参数。此外，还考察了所建立方法的方法学。蛇床子素、哥伦比亚内酯和异欧前胡素的定量信号化学位移分别为δ6.25-δ6.26 ppm、δ6.83-δ6.85 ppm和δ6.31-δ6.32 ppm。蛇床子素、哥伦比亚内酯和异欧前胡素的线性范围均为0.0455-2.2727 mg/mL，R分别为0.9994、0.9994和0.9995。蛇床子素、哥伦比亚内酯和异欧前胡素的检测限分别为0.0660、0.0720、0.0620 mg，定量限分别为0.2201、0.2401、0.2066 mg/mL。该溶液在24 h内具有良好的稳定性和重复性。蛇床子素、哥伦比亚内酯和异欧前胡素的回收率分别为102.26%、99.89%、103.28%。所建立的方法操作简便，大大减少了样品繁琐的预处理，萃取效率高。
