摘要
建立了液液萃取结合气相色谱-质谱法同时测定地表水中33种半挥发性有机物(SVOCs)的分析方法。样品以二氯甲烷为萃取剂在先酸性后中性条件下液液萃取2次,合并萃取液经无水硫酸钠脱水、浓缩并定容至1mL,采用气相色谱-质谱联用仪在电子电离源(EI)模式和选择离子监测(SIM)模式检测,内标法定量。对影响目标物萃取效率的关键因素,水样pH值、萃取剂种类与用量及萃取时间进行了优化与考察。在最优萃取条件下,33种SVOCs在5~500μg·L~(-1)范围内线性良好,平均相对响应因子的相对标准偏差(RRF RSD)小于15.5%,方法检出限为0.01~0.09μg·L~(-1),定量限为0.04~0.36μg·L~(-1),在2个空白添加高低质量浓度(0.05和0.25μg·L~(-1))水平下的平均回收率为67.1%~119.2%,相对标准偏差(n=6)为1.0%~9.3%。该方法具有较高的选择性、灵敏度和准确度,适合地表水中33种SVOCs快速分析检测。
The sample was extracted twice with dichloromethane as the extractant under acidic and then neutral conditions,the combined extract was dehydrated and concentrated with anhydrous sodium sulfate and the volume was fixed to 1 mL.The samples were detected by gas chromatography-mass spectrometry in electron ionization source(EI)mode and selective ion monitoring(SIM)mode,and quantified by internal standard method.The key factors affecting the extraction efficiency of the target substance,such as the pH value of the water sample,the type and amount of extractant,and the extraction time,were optimized and investigated.Under the optimal extraction conditions,the linearity of the 33 SVOCs was good in the range of 5 to 500μg·L-1 with the average relative standard deviation less than 15.5%,the limits of detection of the method were 0.01 to 0.09μg·L-1 and the limits of quantification were 0.04 to 0.36μg·L-1.The average recoveries were from 67.1%to 119.2%with the relative standard deviations(n=6)of 1.0%to 9.3%in two blank spiked levels(0.05 and 0.25μg·L-1).This method has high selectivity,sensitivity and accuracy.
作者
鲁瑞梅
李国文
Lu Ruimei;Li Guowen(Ecological and Environmental Monitoring Station of DEEY in Yuxi,Yuxi 653100,Yunan,China)
出处
《分析仪器》
CAS
2023年第4期36-42,共7页
Analytical Instrumentation
关键词
半挥发性有机物
同时测定
气相色谱-质谱法
地表水
内标法
Semi-volatile organic compounds
Simultaneous determination
Gas chromatography-mass spectrometry
Surface water
Internal labeling method
