QuEChERS-GC-MS法快速同时测定水质中12种硝基酚类化合物  

Rapid determination simultaneously of twelve kinds of nitrophenolic compounds in water by modified QuEChERS-GC-MS

作　　者：武建强 赵中敬 洪霞 何海宁 袁彩霞 WU Jian-qiang;ZHAO Zhong-jing;HONG Xia;HE Hai-ning;YUAN Cai-xia(Gansu Zhongshang Food Quality Test and Detection Co.,Ltd.,Lanzhou,Gansu 730010,China;Gansu Business Science and Techology Institute Co.,Ltd.,Lanzhou,Gansu 730010,China)

机构地区：[1]甘肃中商食品质量检验检测有限公司,甘肃兰州730010 [2]甘肃省商业科技研究所有限公司,甘肃兰州730010

出　　处：《食品与机械》2021年第8期70-76,共7页Food and Machinery

基　　金：甘肃省青年科技计划项目(编号:20JR5RA076);中国-塔吉克斯坦食品安全检测科技创新合作(编号:KY201801003);甘肃省中央引导地方科技发展专项项目;甘肃省青年科技人才托举工程项目;甘肃省动物源制品安全分析与检测技术重点实验室(编号:18JR2RA024)。

摘　　要：目的:建立一种简单、高效、快速、准确且同时测定水质中12种硝基酚类化合物的方法。方法:通过共沉淀法、水热法合成磁性四氧化三铁纳米粒子负载具有双官能团十八烷胺功能化碳纳米管复合材料作为混合净化剂,优化了QuEChERS样品前处理方法,并将其与气相色谱-质谱联用仪结合建立了同时检测水质中12种硝基酚类化合物的方法。结果:优化后QuEChERS样品前处理方法赋予了磁性纳米粒子和碳纳米材料两者的优势,该条件下对水质中12种硝基酚类具有净化效果好,而且缩短前处理时间,消除基质干扰能力,省去了过滤和离心等复杂的操作步骤。建立的基于QuEChERS样品前处理方法在0.05~0.20μg/mL质量浓度范围具有很好线性关系,最低检出质量浓度为0.009~0.010μg/mL,平均回收率为82.2%~94.6%,相对标准偏差<10%。结论:与传统技术相比,优化QuEChERS技术应用于水质中12种硝基酚类化合物快速检测具有操作简单,吸附能力强,成本低,有机试剂用量小,实现了富集分离一体化。Objective:A simple,efficient,rapid,sensitive,reproducible,accurate and rapid method was established for the simultaneous determination of 12 nitrophenols in water.Methods:Magnetic Fe 3 O 4 nanoparticles loaded with bifunctional octadecylamine functionalized carbon nanotube composites were synthesized by coprecipitation and hydrothermal methods.The sample pretreatment method of QuEChERS was optimized and combined with gas chromatography-mass spectrometry to establish a method for the simultaneous determination of 12 kinds of nitrophenols in water quality.Results:The optimized QuEChERS sample pretreatment method gave the advantages of magnetic nanoparticles and carbon nano materials.Under the control of these conditions,high efficiency of purification of the 12 kinds of nitrophenols in water was found,with shortening the pretreatment time,eliminating matrix interference,and omitting complex operation steps of filtration and centrifugation.The established sample pretreatment method was based on QuEChERS,and the concentration range of 0.05~0.20μg/mL has a good linear relationship,with the minimum detection concentration of 0.009~0.010μg/mL,the average recovery ranging from 82.2%to 94.6%,and the relative standard deviation less than 10%.Conclusion:Compared with the traditional technology,the optimized QuEChERS technology has the advantages of simple operation,strong adsorption capacity,low cost and small amount of organic reagent,and can realize the integration of enrichment and separation.

关 键 词：QUECHERS 硝基酚类 气相色谱-质谱法 磁性纳米复合物 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]