固相萃取-超高效液相色谱法测定兵器工业生产废水中14种硝基酚类物质残留浓度  

Determination of 14 Nitrophenol Products by SPE-Ultra Performance Liquid Chromatography

作　　者：刘玉[1,2] 张同来[1] 杨利[1] 刘芮[1] 刘影[1] 

机构地区：[1]北京理工大学机电学院,北京100081 [2]潍坊市食品药品检验检测中心,山东潍坊262500

出　　处：《兵工学报》2015年第1期70-77,共8页Acta Armamentarii

基　　金：应用物理化学国防科技重点实验室科技基金项目(9140C3703051105;9140C370303120C37142);爆炸科学与技术国家重点实验室基金项目(QNKT12-02)

摘　　要：为了满足环境水样中痕量硝基酚类污染物检测的要求，在硝基酚快速检测中应用Bond Elut Plexa新型固相萃取柱，建立了快速同时测定兵器工业生产环境水样中三硝基苯酚（苦味酸PA）、三硝基间苯二酚（斯蒂酚酸TNR）和三硝基均苯三酚（TNPG）等14种硝基酚的超高效液相色谱分析方法。水样样品采用固相萃取柱净化，上样5．0mL，并最终用3．0mL四氢呋喃洗脱，洗脱液浓缩转溶剂后采用色谱分析。选择全氟苯基色谱柱，以乙腈和乙酸铵及0．1％甲酸作为流动相，梯度洗脱，检测波长为220nm，在优化的固相萃取前处理和液相色谱分离分析条件下，净化效果满足要求。14种硝基酚类化合物在22min内实现完全基线分离，在0．1～20mg／L范围内线性良好，相关系数为0．9973—0．9987；检出限为0．02～0．04mg／L，回收率为82．5％～104．8％，相对标准偏差3．2％-5．7％．本方法已成功应用于生产环境水中实际样品的分析。A simple ultra performance liquid chromatography （UPLC） method for the determination of fourteen nitrophenol residues in environmental waste water is proposed. A Bond Elut Plexa solid phase extraction （SPE） is used for the extraction and purification of the compounds in environmental waste wa- ter. The water sample with sampling amount of 5.0 mL is purified using a solid phase extraction column, and then eluted with 3.0 mL tetrahydrofuran. The elution is introduced into the instrument and deter- mined by HPLC with photodiode array detector with detection wavelength of 220 nm. A good base line separation of target compounds is achieved within 22 minutes under the optimal condition. The calibration curves of 3 amides are linear in the concentration range of 0.1 -20 mg/L with the correlation coefficients of 0. 997 3 - 0. 998 7. The recoveries are 82.5% 104.8% , and the relative standard deviations range from 3.2% to 5.7% for the target compounds. The minimum detectable concentrations are 0.02-0. 04 mg/L. This proposed method is convenient to use, sensitive and accurate, and is suitable for the routine detection of trace amide contaminants in environmental waste water .

关 键 词：环境工程学 超高效液相色谱法 硝基酚类 固相萃取方法 

分 类 号：O657[理学—分析化学]