固相萃取-气相色谱质谱法同时测定环境水体中79种半挥发性有机污染物

Simultaneous Determination of 79 Semi-volatile Organic Pollutants in Environmental Water by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

建立了固相萃取-气相色谱质谱法(SPE-GC-MS)同时检测环境水体中不同极性范围的79种半挥发性有机污染物的分析方法。样品经膜片式固相萃取装置,以50 mL/min速率通过Empore C18膜片(47 mm)净化和富集后GC-MS检测,内标法定量。研究表明,79种半挥发性有机污染物在1~1000μg/L线性范围内相关系数R^(2)>0.99;检测限和定量限分别为0.009~0.077 ng/L和0.040~0.31 ng/L;在3个添加水平下(10、100、500 ng/L)79种半挥发性有机污染物在2种不同水体环境中的平均回收率为60.6%~137.3%,相对标准偏差(RSD)为0.8%~8.8%。该方法操作简便、前处理流程快、方法灵敏度和准确度高、环保和通用性强,适用于河流、水库和化工污水样品的检测,在环境监测工作中有很强的实际应用价值。

A solid-phase extraction gas chromatography mass spectrometry(SPE-GC-MS)method was developed for the simultaneous determination of 79 semi-volatile organic pollutants(SVOCs)with different polar ranges in environmental waters.The sample was first purified and enriched by Empore C18 membrane(47 mm)at rate of 50 mL/min.The sample was detected by GC-MS and quantified by internal standard method.The results showed that the correlation coefficient(R^(2))of 79 SVOCs pollutants was greater than 0.99 in the linear range of 1~1000μg/L.The MDL and LOQ were 0.009~0.077 ng/L and 0.040~0.31 ng/L,respectively.The average recoveries and relative standard deviations(RSDs)of the 79 SVOCs in two kinds of different environmental waters were 60.6%~137.3% and 0.8%~8.8% at 3 additive levels(10,100,and 500 ng/L).The method is easy to operate,fast in pretreatment process,high in sensitivity and accuracy,versatile in environmental protection.It is suitable for the detection of river,reservoir,and chemical wastewater samples,and has strong practical application values in monitoring environmental waters.