同位素稀释气相色谱-三重四极杆质谱法测定环境空气中的多氯萘  

Determination of polychlorinated naphthalenes in ambient air by isotope dilution gas chromatography-triple quadrupole mass spectrometry

作　　者：刘洪媛 金静[2] 郭崔崔 陈吉平[2] 胡春[1] LIU Hongyuan;JIN Jing;GUO Cuicui;CHEN Jiping;HU Chun(Shenyang Pharmaceutical University, Shenyang 110000, China;CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;University of Chinese Academy of Sciences, Beijing 100012, China)

机构地区：[1]沈阳药科大学,辽宁沈阳110000 [2]中国科学院分离分析化学重点实验室,中国科学院大连化学物理研究所,辽宁大连116023 [3]中国科学院大学,北京100012

出　　处：《色谱》2022年第7期644-652,共9页Chinese Journal of Chromatography

基　　金：国家重点研发计划(2019YFC1804705).

摘　　要：环境空气中的多氯萘(PCNs)一般为痕量水平(pg/m^(3)),要实现其准确定量必然对分析方法的提取、净化和仪器分析提出较高要求。研究通过考察提取溶剂种类、净化流程和色谱-质谱参数,建立了加速溶剂萃取(ASE)-多层硅胶复合中性氧化铝柱的净化方法,并利用同位素稀释气相色谱-三重四极杆质谱(GC-MS/MS)对环境空气中的多氯萘进行测定。同时,通过在采样、提取和进样分析前分别添加同位素内标,开展质量控制和保证。结果表明,在2~100 ng/mL范围内3~8氯萘的平均相对响应因子(RRF)的相对标准偏差(RSD)均小于16%。PCNs同类物的方法检出限为1~3 pg/m^(3)(以样品体积为288 m^(3)计算)。采用基质加标法评价了方法对环境空气样品中PCNs测定的精密度和准确度,低、中、高加标水平下3~8氯萘的平均加标回收率分别为89.0%~119.4%、98.6%~122.5%和93.7%~124.5%,测定结果的平均相对标准偏差分别为1.9%~7.0%、1.6%~6.6%和1.0%~4.8%。整个分析过程中,采样内标和提取内标的平均回收率分别为136.2%~146.0%和42.4%~78.1%,RSD分别为5.6%~7.5%和2.7%~17.5%,满足痕量分析的要求且平行性较好。方法的灵敏度和准确度高,精密度良好,适用于环境空气中3~8氯萘的准确定量测定,可在一定程度上缓解多氯萘监测对高分辨气相色谱-高分辨质谱的依赖,为实现多氯萘的国际履约提供方法支持。Polychlorinated naphthalenes(PCNs)have a structure similar to that of polychlorinated biphenyls(PCBs)and represent a new type of persistent organic pollutants(POPs)that are widely present in the environment and biological communities.PCNs can migrate and transform via different environmental media,which severely affects the health of humans and organisms.Researchers have devoted considerable focus on ambient air pollution.Although the current ambient air quality has not yet limited the concentration of PCNs,the Stockholm Convention has required parties to prohibit and eliminate their production and use.As one of the contracting parties,China is obligated to improve its environmental monitoring.In other words,the development of a method for monitoring PCNs in ambient air is important for understanding ambient air quality and safeguarding human health.PCNs are generally present at trace levels(pg/m3)in ambient air.To achieve accurate quantification of PCNs,high demands are raised on the methods for extraction,purification,and instrumental analysis,which can directly affect the efficiency,accuracy,and sensitivity of a method.Considering the trace-level presence of PCNs in ambient air and the high efficiency and accuracy of the analytical method,accelerated solvent extraction(ASE),combined with column chromatography using a multilayer silica gel column and a neutral alumina column,was established for the extraction and purification of PCNs in ambient air.The important parameters involved in the aforementioned steps,such as the type of extraction and volume of elution solvent,were optimized.The results indicated that dichloromethane-hexane(1∶1,v/v)was the best extraction solvent for the recovery of PCNs.Hexane and dichloromethane-hexane(5∶95,v/v)were used as the elution solvents for the multi-silica gel column and neutral alumina column,respectively.Isotope dilution gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)was used to quantify the target compounds.Gas chromatographic parameters,such as tempe

关 键 词：气相色谱-三重四极杆质谱 同位素稀释 多氯萘 环境空气 

分 类 号：O658[理学—分析化学]