Martínez K, Barceló D
Department of Environmental Chemistry, IIQAB-CSIC, Barcelona, Spain.
Fresenius J Anal Chem. 2001 Aug;370(7):940-5. doi: 10.1007/s002160100904.
A method has been developed for the simultaneous determination of antifouling pesticides and some of their degradation products, e.g. dichlofluanid, diuron, demethyldiuron, 1-(3,4-dichlorophenyl)urea, sea-nine, Irgarol 1051 and one of its metabolites (2-methylthio-4-tert-butylamino-s-triazine) in marine sediments. The determination of these compounds in sediment samples was performed by means of methanolic ultrasonic extraction then clean-up on an Isolute ENV+ solid phase extraction (SPE) cartridge. The resulting extract was then analyzed by reversed-phase high-performance liquid chromatography coupled with atmospheric-pressure chemical-ionization mass spectrometry in negative and positive ion modes (HPLC-APCI-MS). Recovery ranged from 54-109% for the antifouling agents and their degradation products. The determination limits for the different compounds varied between 0.2 and 1.6 microg kg(-1) dry sediment. The analytical procedure was successfully applied to the determination of these pesticides and their degradation products in marine sediment samples from different marinas of the Catalan coast. The compounds detected were: diuron, dichlofluanid, demethyldiuron, sea-nine, and Irgarol 1051. The highest concentrations were those of diuron and Irgarol 1051--136 and 88 microg kg(-1), respectively.
已开发出一种同时测定海洋沉积物中防污农药及其某些降解产物的方法，这些产物例如有二氯氟苯胺、敌草隆、去甲基敌草隆、1-(3,4-二氯苯基)脲、Sea-Nine、藻菌清1051及其一种代谢物（2-甲硫基-4-叔丁氨基-s-三嗪）。沉积物样品中这些化合物的测定是通过甲醇超声萃取，然后在Isolute ENV+固相萃取（SPE）柱上进行净化。所得提取物随后采用反相高效液相色谱结合大气压化学电离质谱在负离子和正离子模式下进行分析（HPLC-APCI-MS）。防污剂及其降解产物的回收率在54%至109%之间。不同化合物的测定限在0.2至1.6微克/千克干沉积物之间变化。该分析方法已成功应用于加泰罗尼亚海岸不同码头海洋沉积物样品中这些农药及其降解产物的测定。检测到的化合物有：敌草隆、二氯氟苯胺、去甲基敌草隆、Sea-Nine和藻菌清1051。最高浓度的是敌草隆和藻菌清1051，分别为136和88微克/千克。
