Food and Environmental Safety Research Group (SAMA-UV), Desertification Research Centre (CIDE, UV-CSIC-GV) and, Faculty of Pharmacy, University of Valencia, Av. Vicent Andrés Estellés s/n, 46100 Burjassot, Valencia, Spain.
Desertification Research Centre-CIDE (CSIC-UV-GV), Carretera Moncada - Náquera, Km. 4.5, 46113 Moncada, Valencia, Spain.
J Pharm Biomed Anal. 2017 Nov 30;146:117-125. doi: 10.1016/j.jpba.2017.08.014. Epub 2017 Aug 24.
A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-NaEDTA buffer (pH=4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs<30%. Limits of Quantification for the target compounds were in the range of 10-50ng/g for soil, 2-40ng/g for sediment, 5-30ng/g for fish and 0.3-26ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean-up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effect<20% for 31 compounds against 21, and LOQs <25ngg for 38 compounds against 22) indicates that the proposed method is more efficient than QuEChERS, The method was applied to monitoring these compounds along the Turia River. In river waters, Paracetamol (175ngL), ibuprofen (153ngL) and bisphenol A (41ngL) were the compounds most frequently detected while in sediments were vildagliptin (7ngg) and metoprolol (31ngg) and in fish, bisphenol A (33ngg) or sulfamethoxazole (13ngg).
基于 McIlvaine-NaEDTA 缓冲液(pH=4.5)-甲醇的固相萃取(SPE)和固相萃取(SPE)前的超高效液相色谱-串联质谱法(UHPLC-MS/MS)的灵敏可靠方法,用于测定鱼肉、土壤和沉积物中的 47 种有机污染物。提取方法还用于测定水中这些化合物的 SPE 程序。所有基质的回收率均为 38-104%,相对标准偏差<30%。目标化合物的定量限范围为土壤 10-50ng/g、沉积物 2-40ng/g、鱼类 5-30ng/g 和水 0.3-26ng/L。此外,还将该方法与 QuEChERS(广泛用于环境基质)进行了比较,后者涉及缓冲乙腈(pH 5.5)提取和分散固相萃取净化。所得到的结果(36 种化合物的回收率>50%,9 种化合物的基质效应<20%,31 种化合物的回收率>21%,38 种化合物的 LOQs<25ng/g,22 种化合物)表明,该方法比 QuEChERS 更有效。该方法应用于监测图里亚河沿岸这些化合物的情况。在河水中,扑热息痛(175ng/L)、布洛芬(153ng/L)和双酚 A(41ng/L)是最常检测到的化合物,而在沉积物中则是维格列汀(7ng/g)和美托洛尔(31ng/g),在鱼类中则是双酚 A(33ng/g)或磺胺甲恶唑(13ng/g)。