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目的通过优化固相微萃取(SPME)条件,确定最优实验条件,建立一种固相微萃取与气相色谱-质谱(GC-MS)联用法测定饮用水中32种挥发性有机物的方法。方法采用固相微萃取-气相色谱-质谱联用法对饮用水中的32种挥发性有机物进行测定,确定各化合物的定性定量参数,并优化固相微萃取条件,如萃取头类型、加盐量、平衡时间、萃取时间、萃取温度等,获得最优的测定条件。结果确定的最优条件为:萃取头:CAR/PDMS萃取头;加盐量:10%;平衡时间:20 min;萃取时间:30 min;萃取温度:60℃。本方法的检出限为0.005~5μg/L,在所测浓度范围内回归曲线的线性相关性良好,加标回收率为74.5%~129.5%,RSD均不大于15%(n=6)。结论该方法的前处理操作简单,具有较好的精密度和准确度,且检出限远低于国家限定标准,可对饮用水中多种挥发性有机物同时进行分析。
OBJECTIVE To establish a method for the determination of 32 volatile organic compounds in drinking water by solid phase microextraction coupled with gas chromatography-mass spectrometry (GC-MS) by optimizing SPME conditions and determining the optimal experimental conditions. Methods The 32 volatile organic compounds in drinking water were determined by solid-phase microextraction-gas chromatography-mass spectrometry. The qualitative and quantitative parameters of each compound were determined and the conditions of solid-phase microextraction, such as the type of extraction head, , Equilibration time, extraction time, extraction temperature, etc., to obtain the optimal determination conditions. The optimum conditions were as follows: extraction head: CAR / PDMS extraction head; salt content: 10%; equilibrium time: 20 min; extraction time: 30 min; extraction temperature: 60 ℃. The detection limit of this method was 0.005 ~ 5μg / L. The linearity of the regression curve was good within the range of concentration tested. The recoveries were 74.5% ~ 129.5%, and the RSD was no more than 15% (n = 6). Conclusion The pretreatment of this method is simple, has good precision and accuracy, and the detection limit is much lower than the national limit standard, which can simultaneously analyze a variety of volatile organic compounds in drinking water.