超声辅助萃取快速分析土壤及沉积物中常见季铵盐类化合物  

Rapid Analysis of Commonly Used Quaternary Ammonium Compounds in Soil and Sediment by Ultrasonic-assited Extraction

作　　者：宋谦 肖时宇[1,2,3] 张彪 曾祥英 梁医[1,2] 于志强[1,2] SONG Qian;XIAO Shi-Yu;ZHANG Biao;ZENG Xiang-Ying;LIANG Yi;YU Zhi-Qiang(State Key Laboratory of Organic Geochemistry,Guangzhou Institute of Geochemistry,Chinese Academy of Sciences,Guangzhou 510640,China;Center for Excellence and Innovation in Deep Earth Sciences,Chinese Academy of Sciences,Guangzhou 510640,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院广州地球化学研究所,有机地球化学国家重点实验室,广州510640 [2]中国科学院深地科学卓越创新中心,广州510640 [3]中国科学院大学,北京100049

出　　处：《分析化学》2024年第11期1651-1658,共8页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划项目(No.2019YFC1805501);国家自然科学基金项目(No.42277251);广东省省级科技计划项目(No.2023B1212060049)资助。

摘　　要：季铵盐类化合物(Quaternary ammonium compounds,QACs)作为杀菌剂和表面活性剂在日化产品、日常消毒产品以及工业领域被广泛使用,长期使用和持续排放导致其在土壤和水体环境富集和累积。本研究基于超声辅助萃取-液相色谱-串联质谱(UAE-LC-MS/MS)技术,建立了土壤和沉积物中3类11种常见QACs的快速提取分析方法,包含4种苄基烷基二甲基铵盐(Benzylalkyldimethylammonium compounds)、4种三甲基烷基铵盐(Alkyltrimethylammonium compounds)和3种双甲基双烷基铵盐(Dialkyldimethylammonium compounds)。考察了萃取溶剂种类、pH值、萃取温度以及净化次数对QACs回收率的影响。研究结果表明,在60℃条件下,使用5%HCL-乙腈可有效萃取土壤和沉积物中的QACs,水洗3次可有效降低土壤沉积物基质的干扰。采用三元洗脱体系(0.1%甲酸-水、0.1%甲酸-甲醇和0.1%甲酸-乙腈),11种目标QACs在ZORBAX SB-C_(18)色谱柱上可实现基线分离,线性检测范围为0.001~0.5μg/mL(R^(2)>0.9776),方法检出限为0.01~0.31 ng/g(S/N=3)。土壤中QACs的加标回收率为78.7%~99.3%,相对标准偏差(RSD)<12.9%。本方法前处理操作简便,仅需4 h即可完成1个批次的土壤和沉积物样品中QACs的萃取、分离和净化。本方法耗材成本低,回收率和重现性良好,适用于土壤和沉积物中QACs的快速分析测定。Quaternary ammonium compounds(QACs)are widely used as fungicides and surfactants in daily products and disinfection products,and as additives in industrial process.The QACs can be deposited and accumulated in soil after long-term discharge.In the present study,based on ultrasonic-assisted extraction-liquid chromatography-tandem mass spectrometry(UAE-LC-MS/MS)technique,a sensitive analytical method was developed for rapid analysis of 11 kinds of QACs,including 4 kinds of benzylalkyldimethylammonium compounds,4 kinds of alkyltrimethylammonium compounds,and 3 kinds of dialkyldimethylammonium compounds.The results showed that QACs in soil and sediment could be effectively extracted with 5%acetonitrile at 60 C.The 11 kinds of QACs were baseline-separated on a ZORBAX SB-C_(18) column coupled with ternary mobile phases(O.1%formic-water,0.1%formic-methanol and 0.1%formic-acetonitrile),showing excellent linear relationship in the range of 0.001-0.5μg/mL(R^(2)>0.9776).The limits of detection were 0.01-0.31 ng/g(S/N=3).The recoveries of 11 kinds of QACs in soil samples were 78.7%-99.3%with relative standard deviations(RSDs)<12.9%,showing acceptable recoveries and repeatability.The results indicated that QACs could be extracted and cleaned-up within 4 h using this analytical method,with small volume of organic solvent consumed and less consumables materials.

关 键 词：土壤 沉积物 季铵盐 超声萃取 液相色谱-质谱联用 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]