Department of Chemistry, Virginia Commonwealth University, Richmond, VA 23284-2006, USA.
J Sep Sci. 2012 Jul;35(14):1837-43. doi: 10.1002/jssc.201200053.
A variety of pharmaceuticals have been found in various water systems, including wastewater treatment effluent. Due to the possible environmental and human health implications, it is important to be able to quickly and reliably quantify the amount of pharmaceuticals and personal care products that may be present in such samples. To this end, a new chromatographic analysis technique involving three dimensions of liquid chromatography, including selective comprehensive separations in the second and third dimensions, was applied to the analysis of a wastewater treatment plant effluent (WWTPE) sample using both standard addition and external calibrations. Iterative key set factor analysis alternating least squares with the application of both sample and spectral selectivity constraints was used to resolve the phenytoin peak at a concentration corresponding to about 40 parts-per-trillion using UV absorbance detection. Both the precision and accuracy of the method are investigated. We determined that the concentration of phenytoin in WWTPE using selective three dimensional liquid chromatography with diode array detection was 42 ± 1 ng/L, after resolution from an unknown interferent. The estimated concentration was not significantly different from that obtained by the reference 2DLC/MS/MS method, but was four and a half times more precise.
各种药品已在各种水体中被发现，包括废水处理厂的出水。由于可能对环境和人类健康造成影响，因此能够快速可靠地定量检测此类样品中存在的药品和个人护理产品的含量非常重要。为此，采用了一种新的色谱分析技术，涉及三维液相色谱，包括第二维和第三维的选择性综合分离，使用标准添加和外部校准对污水处理厂出水（WWTPE）样品进行了分析。迭代关键集因子分析交替最小二乘法，同时应用样品和光谱选择性约束，用于使用紫外吸收检测解析浓度约为 40ppt 的苯妥英峰。该方法的精密度和准确度均进行了考察。我们使用具有二极管阵列检测的选择性三维液相色谱法从未知干扰物中解析出，确定 WWTPE 中的苯妥英浓度为 42±1ng/L。从估计浓度与参考 2DLC/MS/MS 方法得到的浓度没有显著差异，但精度高四倍半。
