混合型固相萃取/超高压液相色谱法测定废水中苯胺类化合物  

Determination of Aniline Derivatives in Waste Water by Ultra High Pressure Liquid Chromatography with Mixed-mode Solid Phase Extraction

作　　者：王超[1] 彭涛 高愈霄[1] 吕怡兵[1] 滕恩江[1] 

机构地区：[1]中国环境监测总站,北京100012 [2]扬州市环境监测中心站,江苏扬州225007

出　　处：《分析测试学报》2013年第12期1415-1420,共6页Journal of Instrumental Analysis

基　　金：国家高技术研究发展计划(863计划)(2013AA06A308)

摘　　要：通过对色谱分析、固相萃取和氮吹浓缩条件的优化研究,建立了混合型固相萃取/超高压液相色谱法测定废水中7种苯胺类化合物的方法。200 mL水样以5 mL/min通过MCX混合型固相萃取小柱,经4 mL2%甲酸水溶液锁定,4 mL 25%甲醇水溶液净化,8 mL 2%氨水甲醇溶液洗脱后,洗脱液经50℃氮吹浓缩至1 mL,微孔滤膜（0.22μm,尼龙）过滤后,采用BEH C18色谱柱（2.1 mm×50 mm,1.7μm）进行分离,以甲醇-乙酸铵溶液梯度洗脱,250 nm检测。7种苯胺类化合物可在6.5 min内实现基线分离,在0.1~5.0 mg/L范围内线性关系良好,相关系数均大于0.999,方法检出限（S/N=3）为0.10~0.50μg/L,定量下限（S/N=10）为0.33~1.67μg/L。在0.2μg和1.0μg加标水平下,回收率分别为52%~101%和54%~96%,RSDs分别为2.2%~11.3%和2.5%~9.0%。方法抗干扰能力强、分析速度快、灵敏度高,适用于废水中苯胺类化合物的测定。A mixed-mode solid phase extraction（SPE） coupled with ultra high pressure liquid chromatography（ UPLC） was developed for the determination of seven aniline derivatives（ ADs） in waste water by optimizing chromatographic analysis,SPE and nitrogen-blowing concentration. 200 mL water sample was loaded onto MCX SPE cartridges with a flow rate of 5 mL / min,and ADs were immobilized on SPE column with 4 mL 2% formic acid. Before eluted with 4 mL methanol containing 2% ammonia,the column was cleaned up with 4 mL 25% methanol. The elute was concentrated to 1 mL by nitrogen blowing at 50 ℃,and filtered through a microfiltration membrane（ 0. 22 μm,nylon）. The separation of ADs was performed on a BEH C 18 column（ 2. 1 mm × 50 mm,1. 7 μm） by gradient elution using methanol- 50 mmol / L ammonium acetate. The UV detector was set at 250 nm. Under the optimal conditions,seven ADs were separated by baseline within 6. 5 min. The calibration curves for seven ADs were linear in the range of 0. 1- 5. 0 mg / L with correlation coefficients more than 0. 999. The method limits of detection（ S / N = 3） and limits of quantitation（ S / N = 10） were 0. 10- 0. 50 μg / L and 0. 33- 1. 67 μg / L,respectively. The recoveries of seven ADs at spiked levels of 0. 2 μg and 1. 0 μg were 52%- 101% and 54%- 96%,with RSDs of 2. 2%- 11. 3% and 2. 5%- 9. 0%,respectively. With the advantages of good anti-interference ability,rapidness and sensitivity,the method was suitable for the detection of ADs in waste water.

关 键 词：苯胺类化合物 混合型固相萃取 超高压液相色谱 废水 

分 类 号：O657.72[理学—分析化学] O623.731[理学—化学]