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分散液液微萃取气相色谱-质谱法测定水中15种硝基苯类化合物
Determination of 15 Kinds of Nitrobenzene in Water Using Dispersive Liquid-Liquid Microextraction and Gas Chromatography-Mass Spectrometry
投稿时间:2019-08-29  修订日期:2020-06-18
DOI:10.19316/j.issn.1002-6002.2020.06.19
中文关键词:  硝基苯类化合物  气相色谱串联质谱  中心组合设计(CCD)  超声辅助分散液液微萃取
英文关键词:nitrobenzenes  gas chromatography-mass spectrometry (GC-MS)  central composite design (CCD)  ultrasonic assisted dispersive liquid-liquid microextraction (UA-DLLME)
基金项目:
作者单位
崔君 国土资源部上海资源环境监督检测中心, 上海 200072
上海市地质勘查技术研究院, 上海 200072
上海市地质调查研究院, 上海 200072 
张强 国土资源部上海资源环境监督检测中心, 上海 200072
上海市地质勘查技术研究院, 上海 200072
上海市地质调查研究院, 上海 200072 
顾华 国土资源部上海资源环境监督检测中心, 上海 200072
上海市地质调查研究院, 上海 200072 
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中文摘要:
      建立了超声辅助基质分散液液微萃取(UA-DLLME)作为前处理联合气相色谱串联质谱(GC-MS)同时测定地下水和地表水中15种硝基苯类化合物的分析方法。萃取剂、分散剂、萃取温度、萃取时间和离子强度等影响因素采用Plackett-Burman设计,快速筛选出最显著影响因素,利用中心组合设计(CCD)简化实验步骤优化显著因素,结合响应曲面图最终确定最佳的萃取条件:5 mL水样在3%氯化钠条件下迅速加入40 μL四氯化碳(萃取剂)和0.5 mL乙腈(分散剂),50 ℃下超声4 min,混合液4 000 r/min离心3 min。结果表明:15种硝基苯类化合物在50.0~1 000.0 μg/L的浓度范围内线性相关系数均大于0.995;采用超声辅助基质分散液液微萃取时,方法检出限(MDL)为0.018~0.039 μg/L;15种目标物的加标平均回收率为83.31%~99.08%,相对标准偏差均不高于5.0%(n=6)。
英文摘要:
      A method was developed for the simultaneous determination of 15 nitrobenzenes in ground and surface water samples by ultrasonic assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry detector (GC-MS).A Plackett-Burman design was performed for screening of significant variables that affecting the extraction efficiency such as extraction and disperser solvent volumes,extraction temperature and time,ionic strength.Then,the significant factors were optimized by using a central composite design (CCD) model and the response surface equations were derived.The optimum experimental conditions included:A 5 mL aqueous sample solution with the ionic strength of 3% NaCl,0.5 mL methanol (disperser solvent),containing 40 μL carbon tetrachloride CCl4 (extraction solvent) was injected rapidly into the sample solution.Ultrasonic extraction for 4 min at 50 ℃.A Cloudy mixture was obtained and centrifuged for 3 min at 4000 r/min.The results showed the linear correlation coefficients of 15 nitrobenzenes in the concentration ranges of 50.0-1000.0 μg/L were more than 0.995.The limits of detection (MDL) were 0.018-0.039 μg/L,the average recoveries for 15 targets at spiked water ranged from 83.31% to 99.08% with the relative standard deviations (RSD) were below 5.0% (n=6).
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