Wang Caiyun, Chen Xuan, Hu Shuang, Bai Xiaohong
School of Pharmacy, Shanxi Medical University, Taiyuan, China.
J Sep Sci. 2016 Nov;39(22):4290-4298. doi: 10.1002/jssc.201600605. Epub 2016 Oct 24.
A novel stirrer-liquid/solid microextraction method was developed for the separation and enrichment of trace levels of curcumin, bisdemethoxycurcumin, and demethoxycurcumin in Rhizoma Curcumae Longae, Radix Curcumae, and Rhizoma Curcumae before their analysis by high-performance liquid chromatography with ultraviolet detection. In the proposed approach, a magnetic stirrer was immersed in decanol to coat its surface completely with decanol, which was used as an extraction platform. The stirrer coated with decanol is not only a power to agitate the sample solution to constantly update the sample on the stirrer surface but also it can adsorb and extract the target analytes. Some effective parameters, including suitable superficial area of stirrer, extraction solvent, sample phase pH, NaCl concentration, stirring rate, extraction time, sample phase volume, were analyzed and selected. Under the optimal conditions, the linearities are 0.0044-2.20 μg/mL, detection limits are 0.3-0.6 ng/mL, and the extraction content per unit length and enrichment factors of the target analytes are 6.24-9.71/mm and 589-917, respectively. Also, the stirrer-liquid/solid microextraction mechanism for the extraction and enrichment of the target analytes was analyzed and expounded. The results showed that stirrer-liquid/solid microextraction is a simple, rapid sample pretreatment approach with a high enrichment factor.
开发了一种新型搅拌器-液/固微萃取方法,用于在采用高效液相色谱-紫外检测法分析之前,对姜黄、郁金和莪术中痕量姜黄素、双去甲氧基姜黄素和去甲氧基姜黄素进行分离和富集。在所提出的方法中,将磁力搅拌器浸入癸醇中,使其表面完全被癸醇覆盖,癸醇用作萃取平台。涂有癸醇的搅拌器不仅是搅拌样品溶液以不断更新搅拌器表面样品的动力,而且还能吸附和萃取目标分析物。分析并选择了一些有效参数,包括合适的搅拌器表面积、萃取溶剂、样品相pH值、NaCl浓度、搅拌速率、萃取时间、样品相体积。在最佳条件下,线性范围为0.0044 - 2.20μg/mL,检测限为0.3 - 0.6ng/mL,目标分析物的单位长度萃取量和富集因子分别为6.24 - 9.71/mm和589 - 917。此外,还对目标分析物萃取和富集的搅拌器-液/固微萃取机理进行了分析和阐述。结果表明,搅拌器-液/固微萃取是一种简单、快速且富集因子高的样品前处理方法。