Baranowska Irena, Magiera Sylwia, Baranowski Jacek
Department of Analytical Chemistry, Silesian University of Technology, Gliwice, Poland.
J Chromatogr Sci. 2011 Nov-Dec;49(10):764-73. doi: 10.1093/chrsci/49.10.764.
A simple method using solid-phase extraction (SPE) and ultra high-performance liquid chromatography (UHPLC) for the simultaneous determination of β-blockers, isoflavones, and flavonoids in human urine is developed. A statistical central composite design and response surface analysis is used to optimize the separation of the analytes. These multivariate procedures are efficient in determining the optimal separation condition using resolutions and retention time as responses. A gradient elution using a mobile phase consisting of 0.05% trifluoroacetic acid in water and acetonitrile is applied on a Hypersil GOLD column within a short analysis time of 4.5 min. UV detection was used to monitor the analytes. The suggested method was linear in a concentration range from 0.04-20.00 μg/mL, depending on the compound. The limits of detection ranged from 8.9 to 66.2 ng/mL. The precision was lower than 2.74%, and the accuracy was between 0.01-3.65%. The Oasis HLB column, with the highest recoveries, is selected for the pre-concentration step. This present paper reports, for the first time, a method for the simultaneous determination of β-blockers, isoflavones, and flavonoids in human urine samples. Furthermore, the developed method can also be applied to the routine determination of examined compounds concentrations in human urine.
开发了一种使用固相萃取（SPE）和超高效液相色谱（UHPLC）同时测定人尿中β-受体阻滞剂、异黄酮和黄酮类化合物的简单方法。采用统计中心复合设计和响应面分析来优化分析物的分离。这些多变量程序在使用分离度和保留时间作为响应来确定最佳分离条件方面非常有效。在Hypersil GOLD柱上，使用由0.05%三氟乙酸水溶液和乙腈组成的流动相进行梯度洗脱，分析时间短至4.5分钟。采用紫外检测来监测分析物。根据化合物的不同，所建议的方法在0.04 - 20.00μg/mL的浓度范围内呈线性。检测限范围为8.9至66.2 ng/mL。精密度低于2.74%，准确度在0.01 - 3.65%之间。选择回收率最高的Oasis HLB柱用于预浓缩步骤。本文首次报道了一种同时测定人尿样中β-受体阻滞剂、异黄酮和黄酮类化合物的方法。此外，所开发的方法还可应用于人尿中被测化合物浓度的常规测定。
