摘要
短链氯化石蜡(SCCPs)是一种新型持久性环境污染物,准确分析水中SCCPs对研究和正确认识水环境中SCCPs的污染水平、环境行为等均具有重要意义。本研究建立了顶空-固相微萃取-全二维气相色谱-飞行时间质谱技术分析水中SCCPs的方法,确定了萃取探针、萃取温度、萃取时间、体系盐度、搅拌速率等最佳实验条件。本方法在0.2～20.0μg/L浓度范围内线性良好,相关系数大于0.999,检出限在0.06～0.13μg/L之间,平均加标回收率在80.9%～95.4%之间,日内和日间精密度(RSD)分别小于7.1%(n=5)和14.0%(n=5)。本方法灵敏、准确、环境友好、可自动化运行,已成功应用于皮革加工厂周围地下水和地表水中SCCPs的分析。
Short-chain chlorinated paraffins(SCCPs)are a new kind of persistent organic pollutant.Accurate analysis of SCCPs in water is important for good understanding of their pollution level,spatial distribution and environmental behavior in water environment.In this study,a simple,sensitive,and environmentally friendly method for the determination of trace SCCPs in water samples has been established based on headspace solid phase micro-extraction(HS-SPME)and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry(GC×GC-TOF-MS).The key parameters of HS-SPME were systematically optimized including fiber type,extraction temperature,extraction time,ionic strength,etc.Under the optimum extraction conditions,the calibration curves showed a good linearity(R 2≥0.999)in the concentration range of 0.2-20.0μg/L.The detection limits of this method were 0.06-0.13μg/L.The accuracy of the method was evaluated by calculating the recovery at 10μg/L,resulting in good recovery values between 80.9%and 95.4%.The method precision was also satisfactory,with the RSD values less than 7.1%and 14.0%for intra-day and inter-day tests,respectively.Finally,the proposed method was applied to detection of SCCPs in real water samples of leather processing area in Hebei Province.In conclusion,the main advantages of the proposed method are the small sample volume,solvent-free extraction,automated online operation,and meeting the requirement of quality detection on SCCPs in water as set by most environmental regulations,thus we believe that this method is a good choice for the detection of SCCPs in water samples.
作者
战楠
朱帅
郭峰
田芹
饶竹
ZHAN Nan;ZHU Shuai;GUO Feng;TIAN Qin;RAO Zhu(National Research Center for Geoanalysis,The Key Laboratory of Eco-geochemistry, Ministry of Nature Resources,Beijing 100037,China)
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2018年第12期2004-2010,共7页
Chinese Journal of Analytical Chemistry
基金
中国地质调查局地质调查项目(No.DD20189627)
中国地质科学院基本科研业务费项目(No.CSJ2017012)
国家自然科学基金项目(No.21607033)资助。
关键词
短链氯化石蜡
固相微萃取
全二维气相色谱-飞行时间质谱
水质分析
Short-chain chlorinated paraffins
Headspace solid phase micro-extraction
Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry
Water analysis
