Department of Physical and Analytical Chemistry, EPS of Linares, University of Jaén, 23700 Linares, Jaén, Spain.
Sci Total Environ. 2012 Mar 1;419:208-15. doi: 10.1016/j.scitotenv.2011.12.058. Epub 2012 Jan 28.
This paper reports a sensitive analytical method based on microwave-assisted extraction and continuous solid-phase extraction (SPE), followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous determination of residues of 18 pharmaceuticals (analgesics, antibacterials, anti-epileptics, β-blockers, lipid regulators and non-steroidal anti-inflammatories), one personal care product and 3 hormones in soils, sediments and sludge. The analytes are extracted with 3:2 methanol/water under the action of microwave energy and the resulting extract is passed through a SPE column to clean up the sample matrix and preconcentrate the analytes. Then, the analytes, trapped on Oasis-HLB sorbent, are eluted with ethyl acetate, silylated and determined by GC-MS. The proposed method provides a linear response over the concentration range 2.5-20,000 ng/kg with correlation coefficients higher than 0.994 in all cases. Also, it features low limits of detection (0.8-5.1 ng/kg), good precision (within- and between-day relative standard deviation less than 7%) and recoveries ranging from 91 to 101%. The method was successfully applied to agricultural soils, river and pond sediments, and sewage sludge. All samples contained some target analyte and sludge contained most -some at considerably high concentrations.
本论文报道了一种基于微波辅助提取和连续固相萃取（SPE），随后结合气相色谱-质谱（GC-MS）的灵敏分析方法，用于同时测定土壤、沉积物和污泥中 18 种药物（镇痛药、抗菌药、抗癫痫药、β-受体阻滞剂、血脂调节剂和非甾体抗炎药）、一种个人护理产品和 3 种激素的残留。在微波能量的作用下，用 3:2 的甲醇/水提取分析物，所得提取物通过 SPE 柱进行净化，以清除样品基质并浓缩分析物。然后，用乙酸乙酯洗脱被 Oasis-HLB 吸附剂捕获的分析物，进行硅烷化处理，再用 GC-MS 测定。该方法在 2.5-20000ng/kg 的浓度范围内呈现出线性响应，所有情况下的相关系数均高于 0.994。此外，该方法具有较低的检出限（0.8-5.1ng/kg）、良好的精密度（日内和日间相对标准偏差均小于 7%）以及回收率范围为 91-101%。该方法成功应用于农业土壤、河流和池塘沉积物以及污水污泥。所有样品均含有一些目标分析物，而污泥则含有大部分——有些浓度相当高。
