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

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5.0 m L,并最终用3.0 m L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220 nm,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22 min内实现完全基线分离,在0.1~20 mg/L范围内线性良好,相关系数为0.997 3~0.998 7;检出限为0.02~0.04 mg/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。

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

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 water. 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 determined 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.