HPLC-MS/MS测定3类污水处理厂污泥及污水中的8种药物

HPLC-MS/MS determination of eight PPCPs in sewage and sludge from three types of sewage treatment plants

药物及个人护理品(pharmaceuticals and personal care products,PPCPs)是一类典型的新型痕量有机污染物,会对人类健康及生态系统带来风险.本文发展优化了以超声提取、固相萃取净化并结合高效液相色谱-串联质谱对污泥及污水中的8种药物,包括罗红霉素、美托洛尔、普萘洛尔、磺胺噻唑、磺胺甲恶唑、磺胺嘧啶、咖啡因、对乙酰氨基酚的分析检测方法.结果表明,在优化条件下,该方法对污泥回收率可达74.80%—127.96%,水样回收率除低浓度加标情况下对乙酰氨基酚回收率较低为39.45%外,其余物质回收率可达81.36%—120.18%,污水方法的检出限为0.020—5.155 ng·L^(-1),污泥方法检出限为0.004—1.031 ng·kg^(-1).应用所建立的方法,对天津市三个不同类型污水处理厂(医院、养猪场及城市污水处理厂)的脱水污泥及进出水进行检测分析.结果表明,污水中目标物浓度范围为(0.14—2157.03 ng·L^(-1)),污泥中目标物浓度范围为(0.12—9.84 ng·kg^(-1)).大多目标物在医院分布浓度较高,养猪场次之,城市污水厂相对较低.其中,美托洛尔、咖啡因、对乙酰氨基酚等3个物质的浓度较高,进出水浓度可达16.69—2157.03 ng·L^(-1),而其余5种物质浓度相对较低.

Pharmaceuticals and Personal Care Products（ PPCPs） is a class of typical trace emerging organic pollutants that are hazardous for human health and ecological systems. In this study,we developed and optimized a method for the extraction,purification and determination of eight PPCPs including roxithromycin, metoprolol, propranolol, sulfathiazol, sulfamethoxazole,sulfadiazine,caffeine and acetaminophen based on ultrasonic extraction,solid phase extraction（ SPE） and high-performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）.The results showed that under the optimized conditions,the spiked recoveries of the eight PPCPs inthe sludge samples ranged from 74. 80% to 127. 96%,and those in the wastewater ranged from 81.36% to 120. 18%,except that acetaminophen had a low recovery of 39. 45%. The method detection limits（ MDL） ranged from 0. 020 to 5. 155 ng·L^（-1） for the wastewater and from 0. 004 to 1.031 ng·kg^（-1） for the sludge. Using the established method,we investigated the PPCPs in the dewatered sludge and wastewater of three different types of sewage treatment plants（ hospital,pig farm and urban sewage treatment plants） in Tianjin. The results showed that the concentration of the target compounds ranged from 0. 14 to 2157. 03 ng·L^（-1） in the wastewater and from 0. 12 to9.84 ng·kg^（-1） in the sludge,and the detection rate was up to 100%. Generally,the concentrations of most PPCPs in sewage and sludge were relatively high in the hospital,followed by pig farm and municipal wastewater treatment plant. Among the PPCPs,the concentrations of metoprolol,caffeine and paracetamol ranged from 16.69 to 2157.03 ng·L^（-1）,and were higher than the others.