典型药物污染物的SPE-UPLC-MS-MS检测方法

Study of Typical Pharmaceutical Contaminants in Natural Water Using Solid-phase Extraction and High Performance Liquid Chromatography with Tandem Mass Spectrometry

采用固相萃取-高效液相色谱-串联质谱法（SPE-UPLC-MS-MS）测定自然水体中的10种典型药物污染。比较了2种萃取柱HLB和C18的富集效果,并对水样pH、萃取柱的淋洗溶剂及水样体积进行了优化。结果表明,采用HLB小柱进行富集净化,水样体积为500 mL,调节pH=3.0,95%甲醇洗脱,在0-200μg/L范围内10种药物的标准曲线线性关系良好（r≥0.999）,方法检出限0.5-2.0 ng/L,精密度高（RSD〈10%）,加标回收率为64.3%-100.7%。经过对太湖和某污水厂排水口水样的测试,表明该方法适用于自然水体药物的快速检测,同时大部分药物被检出,说明选择的10种目标药物及建立的检测方法对研究中国水体药物污染具有一定的参考价值。

Solid-phase extraction,high performance liquid chromatography with tandem mass spectrometry were used for determination of ten typical pharmaceuticals in natural water. The extraction efficiencies of HLB and C18 cartridges were compared,and the sample pH value,elution solvent and sample volume were optimized. HLB cartridge was selected for sorption and kept the water sample volume at 500 mL. The water sample was acidified to pH 3. 0,and 95% methanol was used as elution solvent. The calibration curve was linear in the range of 0-200 μg /L with correlation coefficients up to 0. 999. The recovery of standard addition for the method was 64. 3%-100. 7% with a high precision（ RSD 10%） and a low detection limit（ LOD 2 ng /L）. The testing results of natural samples showed that the method was suitable for quick determination of pharmaceuticals in natural water body. Most select pharmaceuticals were detected,so the selected 10 compounds and its detection method could be referred in the study of pharmaceuticals pollution in natural water.