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液相色谱法测定鱼类、小龙虾、贻贝和沉积物中的鱼藤酮。

Liquid chromatographic determination of rotenone in fish, crayfish, mussels, and sediments.

作者信息

Dawson V K, Allen J L

机构信息

U.S. Fish and Wildlife Service, National Fisheries Research Center, La Crosse, WI 54602-0818.

出版信息

J Assoc Off Anal Chem. 1988 Nov-Dec;71(6):1094-6.

PMID:3240959
Abstract

An analytical procedure is described for determining residues of rotenone in fish muscle, fish offal, crayfish, freshwater mussels, and bottom sediments. Tissue samples were extracted with ethyl ether and extracts were cleaned up by gel permeation chromatography and silica gel chromatography. Sediment samples were extracted with methanol, acidified, partitioned into hexane, and cleaned up on a silica gel column. Rotenone residues were quantitated by liquid chromatography, using ultraviolet (295 nm) detection. Recoveries from sediment samples fortified with rotenone at 0.3 microgram/g were 80.8%, whereas recoveries from tissue samples fortified with 0.1 microgram/g ranged from 87.7 to 96.8%. Samples fortified with 0.3 microgram/g and stored at -10 degrees C for 6 months before analysis had recoveries ranging from 83.2 to 90.5%. Limits of detection were 0.025 microgram/g for sediments and 0.005 microgram/g for tissue samples.

摘要

描述了一种用于测定鱼肉、鱼内脏、小龙虾、淡水贻贝和底部沉积物中鱼藤酮残留量的分析方法。组织样品用乙醚提取,提取物通过凝胶渗透色谱法和硅胶色谱法进行净化。沉积物样品用甲醇提取,酸化后,分配到己烷中,并在硅胶柱上进行净化。鱼藤酮残留量通过液相色谱法,使用紫外(295nm)检测进行定量。在沉积物样品中添加0.3微克/克鱼藤酮的回收率为80.8%,而在添加0.1微克/克的组织样品中的回收率为87.7%至96.8%。在分析前添加0.3微克/克并在-10℃下储存6个月的样品的回收率为83.2%至90.5%。沉积物的检测限为0.025微克/克,组织样品的检测限为0.005微克/克。

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