液相色谱-串联质谱法快速测定水及鱼肉中的苯胺

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0.5~500 μg/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0.50 μg/L和1.00 μg/kg，定量限分别为1.00 μg/L和2.00 μg/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1943.6 μg/L和60.8 μg/kg。本方法快速、准确，适用于水和鱼肉中苯胺的快速测定。

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

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 5000 r/min for 5 min. The separation was performed on a reversed-phase C_l8 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 R²>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.