College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, PR China.
Talanta. 2010 Mar 15;80(5):1873-80. doi: 10.1016/j.talanta.2009.10.037. Epub 2009 Oct 30.
In this paper, a solid-phase extraction (SPE) method based on mixed hemimicelles of cetyltrimethyl ammonium bromide (CTAB) on silica-coated magnetic nanoparticles (MNPs) is developed for extraction and preconcentration of compounds from the biological samples. We selected rhein and emodin which are the major active anthraquinones of rhubarb as model analytes. A high performance liquid chromatography-fluorescence detection (HPLC/FLD) method was developed for the determination of rhein and emodin in urine and serum samples. The main factors influencing the extraction efficiency including the amount of surfactant, the concentration of MNPs, the shaking time and the desorption ability of organic solvents were investigated and optimized. No interferences were caused by proteins or endogenous compounds in urine and serum samples. Good linearities (r(2)>0.9995) for all calibration curves were obtained, and the limits of detection (LODs) for rhein and emodin were 0.2 and 0.5 ng/mL in urine samples and 7 and 10 ng/mL in serum samples, respectively. Satisfactory recoveries (92.76-109.90% and 97.53-107.72% for rhein and emodin) in the biological matrices were achieved.
本文开发了一种基于 CTAB 在硅烷化磁性纳米粒子(MNP)上形成混合胶束的固相萃取(SPE)方法,用于从生物样品中提取和预浓缩化合物。我们选择大黄中的主要活性蒽醌化合物大黄酸和大黄素作为模型分析物。建立了高效液相色谱-荧光检测(HPLC/FLD)法测定尿液和血清样品中的大黄酸和大黄素。考察并优化了影响萃取效率的主要因素,包括表面活性剂的用量、MNP 的浓度、振荡时间和有机溶剂的解吸能力。尿液和血清样品中的蛋白质或内源性化合物不会造成干扰。所有校准曲线的线性关系良好(r(2)>0.9995),尿液中大黄酸和大黄素的检出限(LOD)分别为 0.2 和 0.5 ng/mL,血清中分别为 7 和 10 ng/mL。在生物基质中获得了令人满意的回收率(大黄酸和大黄素分别为 92.76-109.90%和 97.53-107.72%)。