首页|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

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

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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-C18色谱柱上可实现基线分离,线性检测范围为0.001~0.5μg/mL(R2>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.
Rapid Analysis of Commonly Used Quaternary Ammonium Compounds in Soil and Sediment by Ultrasonic-assited Extraction
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℃. The 11 kinds of QACs were baseline-separated on a ZORBAX SB-C18 column coupled with ternary mobile phases (0.1%formic-water,0.1%formic-methanol and 0.1%formic-acetonitrile),showing excellent linear relationship in the range of 0.001-0.5μg/mL (R2>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.

SoilSedimentQuaternary ammonium compoundsUltrasonic extractionLiquid chromatography-mass spectrometry

宋谦、肖时宇、张彪、曾祥英、梁医、于志强

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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

中国科学院深地科学卓越创新中心,广州510640

中国科学院大学,北京100049

土壤 沉积物 季铵盐 超声萃取 液相色谱-质谱联用

2024

分析化学
中国化学会 中国科学院长春应用化学研究所

分析化学

CSTPCD北大核心
影响因子:1.423
ISSN:0253-3820
年,卷(期):2024.52(11)