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自动液液萃取-固相萃取净化-气相色谱质谱联用法测定地下水中14种酚类化合物

Determination of 14 Phenolic Compounds in Groundwater by Automatic Liquid-Liquid Extraction Solid-Phase Extraction Purification Gas Chromatography-Mass Spectrometry
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摘要 水样调节至酸性(pH<2)的条件下,采用自动液液萃取方式,用二氯甲烷/乙酸乙酯(体积比1∶1)萃取水样中的酚类化合物,萃取液经过无水硫酸钠除水、硅胶柱净化、氮吹浓缩定容后,经气相色谱质谱联用仪进行分离检测,根据保留时间和目标化合物的特征离子进行定性,采用内标法定量,建立一种快速、准确测定地下水中14种酚类化合物的方法。结果表明,酚类化合物的线性范围为1~20 mg/L,相关系数良好,为0.995~0.999,方法回收率为60%~86%,相对标准偏差为2.5%~14.4%,方法检出限为0.1~0.4μg/L。 Under the condition of adjusting the water sample to acidity(pH<2),automatic liquid-liquid extraction is used to extract phenolic compounds from the water sample by using dichloromethane/ethyl acetate(volume ratio 1∶1),and the extraction solution is dehydrated with anhydrous sodium sulfate,purified with a silica gel column,and concentrated to volume with nitrogen blowing before being separated and detected by gas chromatography-mass spectrometry,and qualitation is conducted based on retention time and characteristic ions of the target compound,the internal standard method is used for quantification,thus establishing a rapid and accurate method for the determination of 14 phenolic compounds in groundwater.The results show that the linear range of phenolic compounds is 1~20 mg/L,and the correlation coefficient is good,which is 0.995~0.999,and the recovery rate of the method is 60%~86%,the relative standard deviation is 2.5%~14.4%,and the detection limit of the method is 0.1~0.4μg/L.
作者 顾桔 鞠华 GU Ju;JU Hua(Qingshan Lvshui(Jiangsu)Inspection and Testing Co.,Ltd.,Changzhou 213000,China)
出处 《中国资源综合利用》 2023年第11期4-6,共3页 China Resources Comprehensive Utilization
关键词 液液萃取 气相色谱质谱联用法 地下水 酚类化合物 liquid-liquid extraction gas chromatography-mass spectrometry groundwater phenolic compounds
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