Department of Environmental Analysis, Faculty of Chemistry, University of Gdańsk, ul. Sobieskiego 18, 80-952 Gdańsk, Poland.
J Chromatogr A. 2013 Aug 23;1304:138-46. doi: 10.1016/j.chroma.2013.07.018. Epub 2013 Jul 10.
Although the uncertainty estimate should be a necessary component of an analytical result, the presentation of measurements together with their uncertainties is still a serious problem, especially in the monitoring of the presence of pharmaceuticals in the environment. Here we discuss the estimation of expanded uncertainty in analytical procedures for determining residues of twelve pharmaceuticals in seawaters using solid-phase extraction (SPE) with H2O-Philic BAKERBOND speed disks and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Matrix effects, extraction efficiency and absolute recovery of the developed analytical method were determined. A validation was performed to obtain the method's linearity, precision, accuracy, limits of detection (LODs) and quantification (LOQs). The expanded uncertainty of the data obtained was estimated according to the Guide to the Expression of Uncertainty in Measurement and ISO 17025:2005 standard. We applied our method to the analysis of drugs in seawaters samples from the coastal area of the southern Baltic Sea. As a result, a new approach (concerning the uncertainty estimation as well as the development of analytical method) to the analysis of pharmaceutical residues in environmental samples is presented. The information given here should facilitate the introduction of uncertainty estimation in chromatographic measurements on a much greater scale than is currently the case.
虽然不确定度估计应该是分析结果的必要组成部分,但测量值及其不确定度的表示仍然是一个严重的问题,特别是在监测环境中药物的存在时。在这里,我们讨论了使用亲水 BAKERBOND 固相萃取(SPE)水盘和液相色谱-串联质谱(LC-MS/MS)测定海水中十二种药物残留的分析程序中扩展不确定度的估计。确定了开发的分析方法的基质效应、萃取效率和绝对回收率。进行了验证以获得方法的线性度、精密度、准确度、检测限(LOD)和定量限(LOQ)。根据《测量不确定度表示指南》和 ISO 17025:2005 标准,估算了所得数据的扩展不确定度。我们将我们的方法应用于波罗的海南部沿海地区海水中药物的分析。结果,提出了一种新的方法(关于不确定性估计以及分析方法的开发)来分析环境样品中的药物残留。这里提供的信息应该有助于在比目前更大的范围内引入色谱测量的不确定度估计。