Multi-residue determination of pharmaceuticals in sludge and sludge enriched soils using pressurized liquid extraction, solid phase extraction and liquid chromatography with tandem mass spectrometry
Multi-residue determination of pharmaceuticals in sludge and sludge enriched soils using pressurized liquid extraction, solid phase extraction and liquid chromatography with tandem mass spectrometry
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DOI：
10.1039/b717453e
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发表时间：
2008-01-01
影响因子：
--
通讯作者：
Paull, Brett
中科院分区：
文献类型：
--
作者：
Barron, Leon;Tobin, John;Paull, Brett
提出了一种分析方法，用于确定富含生物固体的土壤和消化污泥中 27 种常用处方和消耗药物的选择。将加压液体萃取、固相萃取和液相色谱与串联质谱相结合，可以检测每种样品类型中低亚ng g(-1) 水平的所有分析物。对 6 种不同吸附剂类型的固相萃取效率进行了比较，结果发现 Waters Oasis HLB 小柱对 20 种分析物具有增强的选择性，显示最终方法在土壤和消化污泥中的回收率 >= 60%。该方法在两个样品基质中的线性度、范围、精度和检测限均经过验证。然后在富含污泥的土壤以及初级废水处理厂生产的热干燥污泥肥料前体中测定所有分析物。消化污泥中抗菌剂三氯生的含量超过20μg g(-1)，热干燥污泥饼中的抗菌剂三氯生含量超过5μg g(-1)。上述样品中还检测到显着痕量的卡马西平和华法林。
An analytical method to determine a selection of 27 frequently prescribed and consumed pharmaceuticals in biosolid enriched soils and digested sludges is presented. Using a combination of pressurized liquid extraction, solid phase extraction and liquid chromatography with tandem mass spectrometry, it was possible to detect all analytes in each sample type at the low-sub ng g(-1) level. Solid phase extraction efficiencies were compared for 6 different sorbent types and it was found that Waters Oasis HLB cartridges offered enhanced selectivities with 20 analytes showing final method recoveries >= 60% in both soils and digested sludges. The method was validated for linearity, range, precision and limits of detection in both sample matrices. All analytes were then determined in sludge enriched soils as well as the precursor thermally dried sludge fertilizer produced from a primary wastewater treatment plant. Levels of the antibacterial agent triclosan were found to exceed 20 mu g g(-1) in digested sludge and 5 mu g g(-1) in thermally dried sludge cake. Significant traces of carbamazepine and warfarin were also detected in the above samples.