超快速液相色谱-荧光可变波长测定纺织废水中酚类污染物

Determination of phenolic pollutants in textile wastewater by ultra-fast liquid chromatography coupled with fluorescence variable wavelength

建立了纺织废水中7种酚类化合物(苯酚、对苯二酚、双酚A、双酚F、双酚B、辛基酚、壬基酚)的固相萃取-超快速液相色谱-荧光检测(SPE-UFLC-FL)方法。样品酸化后经HLB-SPE小柱净化,采用Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d.,2.2μm)色谱柱,以甲醇-水为流动相进行梯度洗脱,荧光可变波长检测,以保留时间定性,外标法定量。结果表明,7种酚类化合物在0.1~5.0mg/L范围内呈良好的线性关系。取样量为50 mL,浓缩定容至0.5 mL时,方法的定量检测限为1.0μg/L。平均回收率为93.0%~108.0%,相对标准偏差(RSDs)为1.5%~6.5%。该方法快速、准确、灵敏,可用于纺织废水中酚类污染物的分析测定。

The determination method of 7 kinds of phenolic pollutants(phenol,hydroquinone,bisphenol A,bisphenol F,bisphenol B,octyl phenol,nonyl phenol)in textile wastewater was developed by solid phase extraction and ultra-fast liquid chromatography coupled with fluorescence variable wavelength(SPE-UFLC-FL).After acidification,the sample was purified on HLB-SPE cartridge.Chromatographic separa.tion was on Shim-pack XR-ODSⅡ(100 mm×2.0 mm i.d.,2.2μm)column.The analysis was determined by fluorescence variable wavelength in gradient elution with methanol/water.The qualitative and quantitative anal.ysis were based on the retention time and external standard method.The results showed that the 7 kinds of phenolic compounds showed a good linear relationship in the range of 0.1~5.0 mg/L.The limit of quantifica.tion(LOQ)was 1.0μg/L when 50 mL sample concentrated to 0.5 mL.The average recovery was in the range of 93.0%~108.0%,and the relative standard deviations was 1.5%~6.5%.This method was quick,accurate and sensitive,which was suitable for the analysis of phenolic pollutants in textile wastewater.