Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
J Chromatogr A. 2012 Aug 31;1253:1-10. doi: 10.1016/j.chroma.2012.06.079. Epub 2012 Jul 2.
This paper presents a comparison of three extraction techniques--ultrasound-assisted extraction, microwave-assisted extraction and pressurized liquid extraction--in order to evaluate their efficiency in the determination of bisphenol A and its chlorinated derivatives in sewage sludge samples. Extraction parameters for each technique were accurately optimized to achieve the highest recoveries. The selected compounds were detected and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS), operating in negative atmospheric pressure chemical ionization (APCI) and in multiple reaction monitoring (MRM) mode. The analytes were separated in less than 6 min. BPA-d₁₆ was used as internal standard. Three selective, sensitive, robust and accurate analytical methods were developed. The limits of detection (LODs) of the methods ranged from 2 to 9 ng g⁻¹ and the limits of quantification (LOQs) from 8 to 26 ng g⁻¹, while inter- and intra-day variability was under 6% in all cases. Given the absence of certified reference materials (CRMs), the methods were validated separately by using matrix-matched calibration and recovery assays with spiked samples. Recovery rates ranged from 97.7% to 103.1%. The sewage sludge samples used for experiments were collected from two different wastewater treatments plants (WWTPs) located in the province of Granada (South-East Spain). The statistical comparison of the methods demonstrated no statistically significant differences between the extraction techniques for the determination of BPA and chlorinated derivatives in sludge samples.
本论文比较了三种提取技术——超声辅助提取、微波辅助提取和加压液体提取——以评估它们在测定污水污泥样品中双酚 A 及其氯化衍生物中的效率。为了获得最高的回收率，对每种技术的提取参数进行了精确优化。使用液相色谱-串联质谱（LC-MS/MS），在负大气压化学电离（APCI）和多重反应监测（MRM）模式下检测和定量选择的化合物。分析物在不到 6 分钟的时间内分离。使用 BPA-d₁₆ 作为内标。开发了三种选择性、灵敏、稳健和准确的分析方法。方法的检出限（LOD）范围为 2 至 9 ng g⁻¹，定量限（LOQ）范围为 8 至 26 ng g⁻¹，而所有情况下的日内和日间变异性均低于 6%。由于缺乏认证参考物质（CRMs），因此分别使用基质匹配校准和加标样品的回收率测定法对方法进行了验证。回收率范围为 97.7%至 103.1%。用于实验的污水污泥样品取自位于西班牙东南部格拉纳达省的两个不同废水处理厂（WWTP）。方法的统计比较表明，在污泥样品中测定 BPA 和氯化衍生物时，三种提取技术之间没有统计学上的显著差异。
