顶空固相微萃取-气相色谱-三重四极杆质谱法测定水中14种酚类污染物

Determination of 14 Phenols Compounds in Water by Headspace Solid-phase Microextraction Coupled with Gas Chromatography-triple Quadrupole Mass Spectrometry

采用聚丙烯酸酯(PA,85μm)涂层萃取头,建立了顶空固相微萃取(HS-SPME)-气相色谱-三重四极杆质谱法(GC-MS/MS)测定水中14种酚类污染物的分析方法。主要对顶空温度、平衡时间、吸附时间等参数进行了实验优化,结果表明:在70℃下平衡40 min,吸附时间为15 min时,顶空固相微萃取过程基本达到平衡;在2.0~40.0μg/L质量浓度范围内,14种酚类化合物线性关系良好,相关系数均大于0.998,方法检出限在0.04~0.28μg/L范围内,实际水样的加标回收率平均值在83%~116%之间,6次平行测定的RSD范围在2.3%~12.3%之间。该方法操作简便、准确度和灵敏度高、重复性好,能够满足水中酚类污染物的检测要求。

A method based on headspace solid-phase microextraction(HS/SPME)coupled with Gas chromatography-triple quadrupole mass spectrometry was developed for the determination of 14 Phenols compounds in Water with the PA fiber(85μm).Parameters of the extraction conditions were optimized,such as equilibrium time,equilibrium temperature and adsorption time.The results showed that,the sampers balanced at 70℃for 40 min,and adsorbed for 15 min,could get the best results.The method showed a good linear relationship for 14 phenols in the range of 2.0~40.0μg/L,the correlation coefficient higher than 0.998,and the limits of detection were 0.04~0.28μg/L with average recovery rate of 83%~116%and relative standard deviations(RSD)of 2.3%~12.3%(n=6).The method is simple,accurate,sensitive and repeatable,and can meet the requirements for the detection of phenolic pollutants in water.