INRS-ETE, Université du Québec 490, Rue de la Couronne, Québec, Canada G1K 9A9.
Talanta. 2012 Sep 15;99:247-55. doi: 10.1016/j.talanta.2012.05.047. Epub 2012 May 29.
In this study, the distribution of the anti-epileptic drug carbamazepine (CBZ) in wastewater (WW) and aqueous and solid phases of wastewater sludge (WWS) was carried out. A rapid and reliable method enabling high-throughput sample analysis for quicker data generation, detection, and monitoring of CBZ in WW and WWS was developed and validated. The ultrafast method (15s per sample) is based on the laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). The optimization of instrumental parameters and method application for environmental analysis are presented. The performance of the novel method was evaluated by estimation of extraction recovery, linearity, precision and detection limit. The method detection limits was 12 ng L(-1) in WW and 3.4 ng g(-1) in WWS. The intra- and inter-day precisions were 8% and 11% in WW and 6% and 9% in WWS, respectively. Furthermore, three extraction methods, ultrasonic extraction (USE), microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) with three different solvent condition such as methanol, acetone and acetonitrile:ethyle acetate (5:1, v/v) were compared on the basis of procedural blank and method recovery. Overall, ASE showed the best extraction efficiency with methanol as compared to USE and MAE. Furthermore, the quantification of CBZ in WW and WWS samples showed the presence of contaminant in all stages of the treatment plant.
本研究对废水(WW)和废水污泥(WWS)的水相和固相中抗癫痫药物卡马西平(CBZ)的分布情况进行了研究。建立并验证了一种快速、可靠的高通量样品分析方法,以便更快速地生成、检测和监测 WW 和 WWS 中的 CBZ。该超快方法(每个样品 15 秒)基于激光二极管热解吸-大气压化学电离(LDTD-APCI)与串联质谱(MS/MS)联用。本研究介绍了仪器参数的优化和环境分析方法的应用。通过对提取回收率、线性度、精密度和检测限的评估,对新方法的性能进行了评价。该方法在 WW 中的检测限为 12ng/L,在 WWS 中的检测限为 3.4ng/g。WW 中的日内和日间精密度分别为 8%和 11%,WWS 中的分别为 6%和 9%。此外,在基于程序空白和方法回收率的基础上,对超声提取(USE)、微波辅助提取(MAE)和加速溶剂提取(ASE)三种不同提取方法,以及甲醇、丙酮和乙腈-乙酸乙酯(5:1,v/v)三种不同溶剂条件进行了比较。总体而言,与 USE 和 MAE 相比,ASE 用甲醇作为提取溶剂的提取效率最佳。此外,对 WW 和 WWS 样品中 CBZ 的定量分析表明,在处理厂的各个阶段都存在污染物。