顶空单滴液相微萃取-气相色谱法测定水中苯胺类化合物
GC Determination of Anilines in Water with Head-Space Single Dropping Microextraction
摘 要
提出了气相色谱法测定水中苯胺、N,N-二甲基苯胺、邻甲苯胺、间甲苯胺等4种苯胺类化合物含量的方法。顶空单滴液相微萃取的优化条件如下:萃取剂为正己烷,萃取温度为25 ℃,液滴离萃取瓶内液面高度为2.0 cm,萃取时间为13 min,搅拌速率为400 r·min-1。4种苯胺类化合物的质量浓度在0.100~1.00 μg·L-1范围内与峰面积呈线性关系,检出限在0.006~0.014 μg·L-1之间。方法用于水样分析,加标回收率在90.0%~115%之间,测定值的的相对标准偏差(n=6)均小于10%。
气相色谱法
水样
苯胺类化合物
Head-space single dropping microextraction
GC
Water sample
Anilines
Abstract
GC with single dropping microextraction was applied to the determination of 4 anilines, i.e., aniline, N, N-dimethyl aniline, o-toluidine and m-toluidine in water. Analytical conditions were studied and the following optimized parameters were given: ① extractant: n-hexane; ② temperature of extraction: 25 ℃; ③ height of droplet from surface of liquid in extraction bottle: 2.0 cm; ④ time of extraction: 13 min; ⑤ rate of stirring: 400 r·min-1. Linear relationships between values of mass concentration and peak area of the 4 anilines were kept in the same range of 0.100-1.00 μg·L-1 with limits of detection in the range of 0.006-0.014 μg·L-1. The proposed method was used in the analysis of water sample, giving values of recovery obtained by standard addition method in the range of 90.0%-115% and values of RSD′s (n=6) less than 10%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 国家自然科学基金项目(41101456);国家级大学生创新创业训练计划项目(201211078008);广州市属高校科研计划项目(2012A069)
收稿日期 2013/2/15
修改稿日期
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备注耿新华(1974-),女,河南焦作人,副教授,博士,研究方向为有机地球化学。
引用该论文: GENG Xin-hua,LI Xiao,LIU Ru-feng,WEN Bi-hua,XIE Lian-xin. GC Determination of Anilines in Water with Head-Space Single Dropping Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(2): 202～205
耿新华,李晓,刘汝锋,温必花,谢连心. 顶空单滴液相微萃取-气相色谱法测定水中苯胺类化合物[J]. 理化检验－化学分册, 2014, 50(2): 202～205
被引情况:
【1】邱丰,费旭东,魏宇锋,赵波,王文青,张继东, "气相色谱-质谱法测定汽油中8种醚类和苯胺类添加剂",理化检验－化学分册 51, 790-794(2015)
【2】罗舒君,杜仁军, "顶空固相微萃取-气相色谱-质谱法测定水中的N,N-二甲基苯胺",理化检验－化学分册 52, 1187-1188(2016)
【3】朱 颖,刘 沛,秦迪岚,宋冰冰,罗岳平,毕军平,朱日龙, "液液萃取-高效液相色谱法测定水中的苯胺和联苯胺",理化检验－化学分册 52, 840-842(2016)
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参考文献
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【4】赵汝松,徐晓白,刘秀芬.液相微萃取技术的研究进展［J］.分析化学, 2004,32(9):1246-1251.
【5】WANG Xiao-wei, HE Ying-qian, LI Lin, et al. Application of fully automatic hollow fiber liquid phase microextraction to assess the distribution of organophosphate esters in the Pearl River Estuaries［J］. Science of the Total Environment, 2014,470(1):263-269.
【6】PEDERSEN-BJERGAARD S, RASMUSSEN K E. Bioanalys is of drugs by liquid-phase microextraction coupled to separation techniques［J］. J Chromatogr B, 2005,817:3-12.
【7】董杰,曹鹏,沈英,等.单滴液相微萃取-高效液相色谱法测定水中二甲戊乐灵农药残留［J］.分析化学, 2009,37(3):417-420.
【8】房贤文,谭培功,董新春,等.单滴液相微萃取气相色谱测定水中的酞酸酯类化合物［J］.分析试验室, 2007,26(7):100-103.
【9】王金玲,李义坤,赵京杨,等.单滴微萃取-气相色谱-质谱联用测定水中的硝基咪唑类药物［J］.分析试验室, 2010,29(1):107-110.
【10】SARAJI M, ESTEKI N. Analysis of carbamate pesticides in water samples using single-drop microextraction and gas chromatography-mass spectrometry［J］. Anal Bioanal Chem, 2008,391(3):1091-1100.
【11】GARBI A, SAKKAS V, FIAMEGOS Y C, et al. Sensitive determination of pesticides residues in wine samples with the aid of single-drop microextraction and response surface methodology［J］. Talanta, 2010,82(4):1286-1291.
【12】李刚,张占恩.中空纤维膜液相微萃取-气相色谱-质谱法测定水样中拟除虫菊酯类农药［J］.理化检验-化学分册, 2010,46(3):227-231.
【13】SANAGI M M, ABIDIN N A Z, IBREHIM W A W, et al. Application of double-phase liquid phase microextraction in the determination of partition coefficients and analysis of pesticides in water samples［J］. Chromatogaphia, 2010,71(5/6):461-467.
【14】BASHEER C, ALNEDHARY A A, RAO B S M, et al. Determination of organophosphorous pesticides in wastewater samples using binary-solvent liquid-phase microextraction and solid-phase microextraction: A comparative study［J］. Anal Chim Acta, 2007,605(2):147-152.
【15】WANG Li, WANG Lin-ling, CHEN Jing, et al. Ultrasonic-assisted water extraction and solvent bar microextraction followed by gas chromatography-ion trap mass spectrometry for determination of chlorobenzenes in soil samples［J］. Journal of Chromatography A, 2012,1256(21):9-14.
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