Cao Wan, Cao Jun, Ye Li-Hong, Xu Jing-Jing, Hu Shuai-Shuai, Peng Li-Qing
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. 2015 Dec;36(23):2951-60. doi: 10.1002/elps.201500330. Epub 2015 Oct 7.
This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained.
本文介绍了介孔分子筛KIT-6作为吸附剂,与超高效液相色谱联用,用于微型化基质固相分散(MSPD)法测定牙膏、黄芩和唾液中的生物活性黄酮类化合物。在本研究中,首次将KIT-6用作这种萃取模式的吸附材料。与普通的硅基吸附剂(C18和硅胶)相比,所提出的具有三维立方Ia3d结构和高度有序介孔通道阵列的KIT-6分散剂对被测化合物表现出优异的吸附能力。此外,对几个实验变量,如样品与分散剂的质量比、研磨时间和洗脱溶剂进行了优化,以最大限度地提高萃取效率。所提出的分析方法简单、快速,且样品、分散剂和洗脱溶剂的消耗量低,从而满足“绿色化学”要求。在优化条件下,通过分析加标样品获得的三种生物活性黄酮类化合物的回收率为89.22%至101.17%。此外,测定分析物的检测限和定量限分别在0.02-0.04μg/mL和0.07-0.13μg/mL范围内。最后,微型化基质固相分散法成功应用于实际样品中目标溶质的分析,并获得了满意的结果。