UNSW Water Research Centre, School of Civil and Environmental Engineering, University of New South Wales, NSW 2052, Australia.
Talanta. 2012 Jan 30;89:407-16. doi: 10.1016/j.talanta.2011.12.053. Epub 2011 Dec 24.
A highly sensitive method for the analysis of six sulfonamide antibiotics (sulfadiazine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine and sulfamethoxazole), two sulfonamide metabolites (N(4)-acetyl sulfamethazine and N(4)-acetyl sulfamethoxazole) and the commonly co-applied antibiotic trimethoprim was developed for the analysis of complex wastewater samples. The method involves solid phase extraction of filtered wastewater samples followed by liquid chromatography-tandem mass spectral detection. Method detection limits were shown to be matrix-dependent but ranged between 0.2 and 0.4 ng/mL for ultrapure water, 0.4 and 0.7 ng/mL for tap water, 1.4 and 5.9 ng/mL for a laboratory-scale membrane bioreactor (MBR) mixed liquor, 0.7 and 1.7 ng/mL for biologically treated effluent and 0.5 and 1.5 ng/g dry weight for MBR activated sludge. An investigation of analytical matrix effects was undertaken, demonstrating the significant and largely unpredictable nature of signal suppression observed for variably complex matrices compared to an ultrapure water matrix. The results demonstrate the importance of accounting for such matrix effects for accurate quantitation, as done in the presented method by isotope dilution. Comprehensive validation of calibration linearity, reproducibility, extraction recovery, limits of detection and quantification are also presented. Finally, wastewater samples from a variety of treatment stages in a full-scale wastewater treatment plant were analysed to illustrate the effectiveness of the method.
一种用于分析六种磺胺类抗生素（磺胺嘧啶、磺胺噻唑、磺胺吡啶、磺胺甲噁唑、磺胺二甲嘧啶和磺胺甲恶唑）、两种磺胺类代谢物（N(4)-乙酰磺胺甲噁唑和 N(4)-乙酰磺胺嘧啶）和常用的抗生素甲氧苄啶的高灵敏度方法被开发用于分析复杂的废水样品。该方法包括过滤后的废水样品固相萃取，然后进行液相色谱-串联质谱检测。方法检测限显示出与基质有关，但在超纯水、自来水、实验室规模的膜生物反应器（MBR）混合液、生物处理后的废水和 MBR 活性污泥中的检测限分别为 0.2-0.4ng/mL、0.4-0.7ng/mL、1.4-5.9ng/mL、0.7-1.7ng/mL 和 0.5-1.5ng/g 干重。对分析基质效应进行了研究，结果表明与超纯水基质相比，各种复杂基质中观察到的信号抑制具有显著的、且在很大程度上不可预测的性质。结果表明，为了进行准确的定量，必须考虑到这种基质效应，就像本方法中通过同位素稀释来实现的那样。还全面验证了校准线性、重现性、提取回收率、检测限和定量限。最后，对来自一个全规模污水处理厂的各种处理阶段的废水样品进行了分析，以说明该方法的有效性。
