液相色谱-三重四极杆质谱法测定土壤中苯胺和3,3'-二氯联苯胺的研究
Determination of Aniline and 3,3'-dichlorobenzidine in Soil-Liquid Chromatography-triple Quadrupole Mass Spectrometry
潘丽敏 1黄娟 1王飞逸 1何妙茵1
作者信息
- 1. 广东省绿色产品认证检测中心有限公司,广东 广州 510000
- 折叠
摘要
从土壤样品的前处理改进研究、方法检出限、方法精密度和准确度等方面分析,建立了土壤中苯胺和 3,3'-二氯联苯胺的液相色谱-三重四极杆质谱法的检测方法.实验结果表明,样品前处理过程中加入适量氨水对目标物的稳定性和提取效果有明显的作用;质量浓度范围内(0.5～100.0 μg/L)目标物的曲线相关系数≥0.999 8,苯胺和3,3'-二氯联苯胺方法检出限(MDL)分别为 0.2 μg/kg和 0.9 μg/kg,精密度相对标准偏差分别为 0.7%～2.0%和1.8%～7.2%,准确度加标回收率分别为92.4%～97.8%和 99.1%～120%.该方法具有较高灵敏性及良好的精密度,回收效果好,可应用于实际的监测工作中.
Abstract
A liquid chromatography-triple quadrupole mass spectrometry method for the detection of aniline and 3,3'-dichlorobenzidine in soil was established based on the analysis of the improvement of soil sample pretreatment,detection limit,precision,and accuracy of the method.The experimental results indicate that adding an appropriate amount of ammonia water during the sample pre-treatment process has a significant effect on the stability and extraction efficiency of the target substance;The correlation coefficient of the target substance curve within the mass concentration range(0.5～100.0 μg/L)is≥0.9998,and the detection limits(MDL)for aniline and 3,3'-dichlorobenzidine methods are 0.2 μg/kg and 0.9 μg/kg respectively,the method has high sensitivity and good precision,with relative standard deviations of 0.7%～2.0%and 1.8%～7.2%,and accuracy spiked recoveries of 92.4%～97.8%and 99.1%～120%.The recovery effect is good,and it can be applied to practical monitoring work.
关键词
土壤/苯胺和3,3'-二氯联苯胺/超声萃取/液相色谱-三重四极杆质谱法Key words
soil/aniline and 3,3'-dichlorobenzidine/ultrasonic extraction/liquid chromatography-triple quadrupole mass spectrometry引用本文复制引用
出版年
2024
NETL
NSTL
万方数据