液相色谱-串联质谱法快速测定水及鱼肉中的苯胺  

Determination of aniline in water and fish byliquid chromatography-tandem mass spectrometry

作　　者：贺德春[1] 赵波[1] 唐才明[2] 许振成[1] 张素坤[1] 韩静磊[1] 

机构地区：[1]环境保护部华南环境科学研究所,广东广州510655 [2]中国科学院广州地球化学研究所,广东广州510540

出　　处：《色谱》2014年第9期926-929,共4页Chinese Journal of Chromatography

基　　金：环境保护部公益基金项目(201309001-04);全国重点地区环境与健康专项调查(21111011101)

摘　　要：为快速准确测定水及鱼肉中的苯胺,采用乙腈提取、高效液相色谱-串联质谱测定,建立了水及鱼肉中苯胺的快速测定方法。水样与乙腈以4∶1的体积比混合,1.00 g鱼肉中加入2.00 mL乙腈,涡旋提取1 min,水样和鱼肉样品的提取液离心5 min后取上清液测定。以C18柱为分离柱,乙腈-0.5%（v/v）甲酸水溶液（85∶15,v/v）为流动相,目标物质在3 min内分离。在0.5-500μg/L范围内,苯胺峰面积与内标峰面积之比与质量浓度的线性关系良好（R2〉0.999）。基质加标试验结果表明,苯胺在水中的回收率分别为93.7%（加标水平为40 ng）和86.7%（加标水平为400 ng）,苯胺在鱼肉中的回收率分别为96.8%、92.6%和81.8%（加标水平分别为5、50和500 ng）,相对标准偏差在1.5%-9.2%之间。水样和鱼肉样品中苯胺的检出限分别为0.50μg/L和1.00μg/kg,定量限分别为1.00μg/L和2.00μg/kg。应用该方法测定了从受苯胺污染的水库中采集的13份水样和12份鱼肉样品,结果表明,水和鱼肉中苯胺的最大含量分别为1 943.6μg/L和60.8μg/kg。本方法快速、准确,适用于水和鱼肉中苯胺的快速测定。A fast analytical method for the determination of aniline in water and fish meat by liquid chromatography-tandem mass spectrometry （LC-MS/MS） has been developed. The water sample was mixed with acetonitrile by 4：1 （v/v） and the fish sample was extracted by 2.00 mL acetonitrile for each gram of sample, and then the extracts of water and fish samples were centrifuged at 5 000 r/rain for 5 rain. The separation was performed on a reversed-phase C18 column using mobile phases of acetonitrile-0. 5% （v/v） formic acid aqueous solution （85：15, v/v）. Aniline was separated within 3 min. The calibration curve was linear in the range of 0.5-500 μg/L with R^2〉0. 999. The limits of detection （LODs） were 0.50 μg/L and 1.00 μg/kg and the limits of quantification （LOQs） were 1.00 μg/L and 2.00 μg/kg for aniline in water and fish meat, respectively. The average recoveries of aniline in water were 93.7% at the spiked level of 40 ng and 86.7% at the spiked level of 400 ng（ n = 5）. The average recoveries of aniline in fish were 96.8%, 92.6% and 81.8% at the spiked levels of 5, 50 and 500 ng respectively （ n = 5 ）. The relative standard deviations were 1. 5%- 9.2%. Thirteen water samples and twelve fish samples were collected from a reservoir polluted by aniline and the maximum contents found were 1943.6 μg/L in water and 60.8 μg/kg in fish. The method is suitable for the determination of aniline residues in water and fish with the characteristics of easy operation, high accuracy and precision.

关 键 词：液相色谱-串联质谱 苯胺 水 鱼 

分 类 号：O658[理学—分析化学]