首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Development of an analytical methodology for the determination of organochlorine pesticides by ethylene-vinyl acetate passive samplers in marine surface waters based on ultrasound-assisted solvent extraction followed with headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry
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Development of an analytical methodology for the determination of organochlorine pesticides by ethylene-vinyl acetate passive samplers in marine surface waters based on ultrasound-assisted solvent extraction followed with headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry

机译:基于超声辅助溶剂萃取的海洋表面水中乙烯 - 乙酸乙烯酯的无源取样器测定用于测定有机氯杀虫剂的分析方法的开发方法用顶空固相微萃取和气相色谱 - 串联质谱法

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摘要

A novel strategy for the analysis of 20 organochlorine pesticides (OCPs) monitoring in marine surface waters through ethylenevinyl acetate (EVA) passive samplers was developed and validated. The approach is based on the coupled of ultrasound-assisted solvent extraction (UASE) and headspace solid phase microextraction (HS-SPME) as extraction method for OCPs from EVA samplers. The UASE-HS-SPME method was optimized with a 27-4 Plackett-Burman design, while the significant factors (salting out, temperature and extraction time) were optimized using a central composite design (CCD) combined with desirability function (DF). The OCPs detection was performed using multiple reaction monitoring (MRM) by gas chromatography-tandem mass spectrometry (GC-MS/MS). The optimum experimental conditions comprised: salting out: 23% wv-1 NaCl, temperature: 75 degrees C and extraction time: 55 min. The optimized method was validated in terms of linearity (R2>0.9946), recovery (>61%) and inter-day and intra-day reproducibility (<19%) for 20 OCPs studied. The limits of detection (LODs) were ranging from 0.01 ng for ct-hexachlorocyclohexane and 0.27 ng for endrin aldehyde. Finally, the methodology was tested in marine surface seawater of Southern Chile using EVA samplers, where twelve OCPs were detected at ultra-trace levels (ngL(-1)). (C) 2019 Elsevier B.V. All rights reserved.
机译:通过乙酸乙酯(EVA)被动采样器分析了20种有机氯农药(OCP)监测的新策略(EVA)被动采样器进行了乙酰乙烯乙烯乙烯乙烯乙烯(EVA)被动采样器。该方法基于超声辅助溶剂萃取(uase)和顶空固相微萃取(HS-SPME)作为来自EVA采样器的OCP的提取方法。通过27-4个Plackett-Burman设计进行了优化了Uase-HS-SPME方法,而使用中央复合设计(CCD)与期望功能(DF)相结合进行了显着因素(盐洗,温度和提取时间)。使用多反应监测(MRM)通过气相色谱 - 串联质谱(GC-MS / MS)进行OCPS检测。最佳的实验条件包括:盐氮:23%WV-1 NaCl,温度:75℃和提取时间:55分钟。在线性度(R2> 0.9946)方面验证了优化的方法,研究了20个OCP的恢复(> 61%)和日内的日期和日期的再现性(<19%)。检测极限(LOD)为CT-六氯环己烷的0.01ng和0.27ng用于浸润醛醛。最后,使用EVA采样器在智利南部海洋表面海水中进行了测试,其中在超痕量水平下检测到12个OCP(NGL(-1))。 (c)2019 Elsevier B.v.保留所有权利。

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