超声萃取-高效液相色谱-串联质谱法测定土壤中三种硝基酚类化合物  

Determination of Three Nitrophenol Compounds in Soil by Ultrasonic Extraction-High Performance Liquid Chromatography-Mass Spectrometry

作　　者：乔淞汾 秦冲 刘爱琴 安彩秀 刘安 杨利娟 孙凯茜 冉卓 QIAO Songfen;QIN Chong;LIU Aiqin;AN Caixiu;LIU An;YANG Lijuan;SUN Kaixi;RAN Zhuo(Hebei Research Center for Geoanalysis,Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071052,China)

机构地区：[1]河北省地质实验测试中心,河北省矿产资源与生态环境监测重点实验室,河北保定071052

出　　处：《岩矿测试》2024年第3期501-508,共8页Rock and Mineral Analysis

基　　金：河北省地质矿产勘查开发局科技项目“土壤中酚类化合物分析方法研究”(13000023P0069B4101215)。

摘　　要：硝基酚类化合物作为一类有机化工原料,具有高毒性和致癌性,可通过空气、水传播进入土壤造成污染,危害人类健康。以往采用气相色谱法和气相色谱-质谱法直接测定硝基酚类化合物,存在色谱灵敏度低、峰形差等问题。为提高灵敏度,通常需要对硝基酚类化合物进行衍生化处理,但衍生化方法步骤繁琐耗时。为实现土壤中硝基酚类化合物的快速准确分析,本文建立了超声萃取-高效液相色谱-串联质谱法分析土壤中三种硝基酚类化合物的方法。用二氯甲烷-正己烷(2∶1,V/V)混合溶剂超声萃取土壤中硝基酚类化合物,在超声萃取液中加入强碱性水溶液(pH>12),将下层有机相除去。将水溶液调至酸性(pH<2)后,用二氯甲烷-乙酸乙酯(4∶1,V/V)混合溶剂萃取三种硝基酚类化合物。萃取液浓缩后用10%乙腈-水溶液定容至10.0mL,高效液相色谱-串联质谱仪测定,外标法定量。性能评价的结果表明方法精密度(RSD<10%,n=6)和准确度都可以满足测定要求,三种硝基酚类化合物的方法检出限为0.1~0.2μg/kg,加标回收率为61.7%~90.8%。本方法具有前处理简单、检出限低等优点,可应用于土壤中硝基酚类化合物的测定和评估。As important organic chemical raw materials,nitrophenol compounds have high toxicity and carcinogenicity,which can be transmitted into soil through air and water,causing pollution and endangering human health.In the past,nitrophenol compounds in soil were usually determined by gas chromatography and gas chromatography-mass spectrometry.The derivatization was usually required to improve the sensitivity,which was time-consuming and cumbersome.To achieve a rapid and accurate analysis of the three nitrophenol compounds in soil,a method of ultrasonic extraction-high performance liquid chromatography-mass spectrometry(HPLC-MS)was established.The nitrophenol compounds in soil were extracted by ultrasonic extraction with dichloromethane/n-hexane(2∶1,V/V),and a strong alkaline aqueous solution(pH>12)was added to the ultrasonic extraction solution to remove the underlying organic phase.After the aqueous solution was adjusted to acidity(pH<2),three nitrophenol compounds were extracted with dichloromethane-ethyl acetate(4∶1,V/V).The extraction solution was concentrated and diluted to 10.0mL with 10%acetonitrile aqueous solution,and then determined by HPLC-MS.The RSDs of three nitrophenol compounds were less than 10.0%,detection limits were 0.1−0.2μg/kg,and the recoveries were 61.7%−90.8%.This method has the advantages of simple pretreatment and low detection limit,and can be applied to the determination and evaluation of nitrophenol compounds in soil.

关 键 词：硝基酚类化合物 土壤 超声萃取 二氯甲烷-正己烷 高效液相色谱-串联质谱法 

分 类 号：O657.72[理学—分析化学] O657.63[理学—化学] S151.95[农业科学—土壤学]