Department of Chemistry, Université de Montréal, C.P. 6128, Succursale Centre-Ville, Montreal, QC, Canada H3C 3J7.
Anal Chim Acta. 2012 Nov 19;754:75-82. doi: 10.1016/j.aca.2012.09.046. Epub 2012 Oct 17.
A new solid phase extraction (SPE) method coupled to a high throughput sample analysis technique was developed for the simultaneous determination of nine selected emerging contaminants in wastewater (atrazine, desethylatrazine, 17β-estradiol, ethynylestradiol, norethindrone, caffeine, carbamazepine, diclofenac and sulfamethoxazole). We specifically included pharmaceutical compounds from multiple therapeutic classes, as well as pesticides. Sample pre-concentration and clean-up was performed using a mixed-mode SPE cartridge (Strata ABW) having both cation and anion exchange properties, followed by analysis by laser diode thermal desorption atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). The LDTD interface is a new high-throughput sample introduction method, which reduces total analysis time to less than 15s per sample as compared to minutes with traditional liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS). Several SPE parameters were evaluated in order to optimize recovery efficiencies when extracting analytes from wastewater, such as the nature of the stationary phase, the loading flow rate, the extraction pH, the volume and composition of the washing solution and the initial sample volume. The method was successfully applied to real wastewater samples from the primary sedimentation tank of a municipal wastewater treatment plant. Recoveries of target compounds from wastewater ranged from 78% to 106%, the limit of detection ranged from 30 to 122ng L(-1) while the limit of quantification ranged from 90 to 370ng L(-1). Calibration curves in the wastewater matrix showed good linearity (R(2)≥0.991) for all target analytes and the intraday and interday coefficient of variation was below 15%, reflecting a good precision.
一种新的固相萃取(SPE)方法与高通量样品分析技术相结合,用于同时测定废水中的九种选定的新兴污染物(莠去津、去乙基莠去津、17β-雌二醇、炔雌醇、炔诺酮、咖啡因、卡马西平、双氯芬酸和磺胺甲恶唑)。我们特别包括了来自多个治疗类别的药物化合物,以及农药。样品预浓缩和净化使用具有阳离子和阴离子交换性能的混合模式 SPE 小柱(Strata ABW)进行,然后通过激光二极管热解吸大气压化学电离串联质谱法(LDTD-APCI-MS/MS)进行分析。LDTD 接口是一种新的高通量样品引入方法,与传统的液相色谱串联质谱法(LC-MS/MS)相比,可将每个样品的总分析时间缩短至 15 秒以内。为了优化从废水中提取分析物时的回收率效率,评估了几个 SPE 参数,例如固定相的性质、加载流速、萃取 pH 值、洗涤溶液的体积和组成以及初始样品体积。该方法成功应用于城市污水处理厂初沉池的实际废水样品。目标化合物从废水中的回收率范围为 78%至 106%,检测限范围为 30 至 122ng L(-1),定量限范围为 90 至 370ng L(-1)。在废水基质中,校准曲线对所有目标分析物均具有良好的线性(R(2)≥0.991),日内和日间变异系数均低于 15%,表明精密度良好。