Fuke Chiaki, Arao Tomonori, Morinaga Yasumasa, Takaesu Hajime, Ameno Kiyoshi, Miyazaki Tetsuji
Department of Legal Medicine, School of Medicine, University of the Ryukyus, 207 Uehara, Nishihara, Okinawa, Japan.
Leg Med (Tokyo). 2002 Sep;4(3):156-63. doi: 10.1016/s1344-6223(02)00011-1.
The determination of paraquat, diquat and two metabolites of diquat in biological materials was developed using high-performance liquid chromatography combined with UV and fluorescence detectors. Paraquat, diquat and internal standards (ethyl viologen and o-acetamidophenol) were detected by the UV detector. Diquat-monopyridone and diquat-dipyridone were monitored by the fluorescence detector. Paraquat, diquat, diquat-monopyridone and ethyl viologen were effectively extracted from blood, liver and brain, using a Sep-Pak C(18) cartridge. Diquat-dipyridone and o-acetamidophenol were extracted with methanol. Paraquat and diquat at a concentration range of 0.1-10 microg/ml (or g), and diquat-monopyridone and diquat-dipyridone at a concentration range of 0.01-1 microg/ml (or g) in biological material were determined with high accuracy and precision. The detection limits of paraquat, diquat, diquat-monopyridone and diquat-dipyridone were 1, 1, 0.02 and 0.02 ng, respectively, as an injection amount. This method was applied for toxicological examination of a case of suspected paraquat and diquat intoxication. The analysis of the metabolites of diquat was helpful for the estimation of the elapsed time from ingestion to death.
采用高效液相色谱结合紫外和荧光检测器,建立了生物材料中百草枯、敌草快及其两种代谢物的测定方法。百草枯、敌草快和内标物(乙基紫精和邻乙酰氨基酚)通过紫外检测器进行检测。敌草快单吡啶酮和敌草快双吡啶酮通过荧光检测器进行监测。使用Sep-Pak C(18)柱从血液、肝脏和大脑中有效地提取百草枯、敌草快、敌草快单吡啶酮和乙基紫精。敌草快双吡啶酮和邻乙酰氨基酚用甲醇提取。生物材料中浓度范围为0.1 - 10微克/毫升(或克)的百草枯和敌草快,以及浓度范围为0.01 - 1微克/毫升(或克)的敌草快单吡啶酮和敌草快双吡啶酮,测定结果具有高准确度和精密度。以进样量计,百草枯、敌草快、敌草快单吡啶酮和敌草快双吡啶酮的检测限分别为1、1、0.02和0.02纳克。该方法应用于一例疑似百草枯和敌草快中毒病例的毒理学检查。对敌草快代谢物的分析有助于估计从摄入到死亡的时间间隔。