Simultaneous determination of five nitroaniline and dinitroaniline isomers in wastewaters by solid-phase extraction and high-performance liquid chromatography with ultraviolet detection.
Simultaneous determination of five nitroaniline and dinitroaniline isomers in wastewaters by solid-phase extraction and high-performance liquid chromatography with ultraviolet detection.
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DOI：
10.1016/j.chemosphere.2010.06.066
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发表时间：
2010-09
期刊：
影响因子：
8.8
通讯作者：
C. Tong;Yun Guo;Wei-ping Liu
中科院分区：
文献类型：
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作者：
C. Tong;Yun Guo;Wei-ping Liu
建立了固相萃取-高效液相色谱-紫外检测法测定废水中2-硝基苯胺、3-硝基苯胺、4-硝基苯胺、2，4-二硝基苯胺和2，6-二硝基苯胺5种硝基苯胺和二硝基苯胺异构体的方法。五种异构体的提取用亲脂平衡柱Oasis HLB进行。用含有10%（v/v）乙腈和10%（v/v）乙酸乙酯的混合水溶液洗涤柱，然后用甲醇和乙酸的混合物洗脱5种异构体。采用Agilent TC-C18色谱柱，以乙腈/水（30/70）（v/v）为移动的流动相，流速为1.0mL/min，在30°C下分离，紫外检测器检测，检测波长为225 nm。5种异构体的回收率在84.6%~ 94.0%之间，相对标准偏差小于4.7%。在500 mL加标污水样品中测定的2-硝基苯胺、3-硝基苯胺和2，6-二硝基苯胺的定量限（LOQ）为2.0×10− 9 M，4-硝基苯胺和2，4-二硝基苯胺为4.5×10− 9 M。将该方法应用于酸性废水和印染废水真实的样品中5种异构体的测定。
A high-performance liquid chromatography (HPLC)-ultraviolet detection method, combined with solid-phase extraction (SPE), was developed for the determination of five nitroaniline and dinitroaniline isomers including 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 2,4-dinitroaniline and 2,6-dinitroaniline in wastewater samples. Extraction of the five isomers was carried out with a hydrophile–lipophile balance cartridge, the Oasis HLB. The cartridge was washed by a mixed aqueous solution containing 10% (v/v) acetonitrile and 10% (v/v) ethyl acetate before the five isomers were eluted by a mixture of methanol and acetic acid. Separation of the five isomers was achieved by using an Agilent TC-C18column at 30°C, and using a mixture of acetonitrile/water 30/70 (v/v) as mobile phase under an isocratic condition at a flow rate of 1.0mL/min. The analytes were detected by a UV detector at a wavelength of 225nm. Recoveries of the five isomers in the spiked sewage sample were between 84.6% and 94.0% with a relative standard deviation of less than 4.7%. The limits of quantification (LOQ) determined in a spiked sewage sample of 500mL were 2.0×10−9M for 2-nitroaniline, 3-nitroaniline and 2,6-dinitroaniline, and 4.5×10−9M for 4-nitroaniline and 2,4-dinitroaniline. The proposed method was applied to determine the five isomers in real samples of acidic wastewater and printing and dyeing wastewater.