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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Headspace solid phase microextraction in-situ supercritical fluid extraction coupled to gas chromatography-tandem mass spectrometry for simultaneous determination of perfluorocarboxylic acids in sediments
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Headspace solid phase microextraction in-situ supercritical fluid extraction coupled to gas chromatography-tandem mass spectrometry for simultaneous determination of perfluorocarboxylic acids in sediments

机译:顶空固相微萃取原位超临界流体萃取-气相色谱-串联质谱联用同时测定沉积物中的全氟羧酸

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摘要

Headspace solid phase microextraction (HS-SPME) in-situ supercritical fluid extraction (SFE) was investigated for the determination of trace amounts of perfluorocarboxylic acids (PFCAs) in sediments. Quantitation was performed by using gas chromatography coupled to negative chemical ionization-tandem mass spectrometry (GC-NCI-MS/MS). The optimum conditions of HS-SPME following SFE were obtained using 500μL n-butanol as a derivatization reagent in supercritical carbon dioxide with static extraction for 10min, then dynamic extraction for 20min at 30MPa and 70°C and simultaneous collected with 100μm film thickness PDMS fiber. The linear range of proposed method was from 5 to 5000ngg~(-1), with limit of detection ranging from 0.39 to 0.54ngg~(-1) and limit of quantitation ranging from 1.30 to 1.80ngg~(-1). The developed method was successfully applied to analyze PFCAs in sediments from rivers and beach near industrial areas. The concentrations of PFCAs determined are from 282 to 4473ngg~(-1).
机译:研究了顶空固相微萃取(HS-SPME)原位超临界流体萃取(SFE),用于测定沉积物中痕量的全氟羧酸(PFCA)。使用与负化学电离串联质谱联用的气相色谱仪(GC-NCI-MS / MS)进行定量。在超临界二氧化碳中,使用500μL正丁醇作为衍生试剂,静态萃取10min,然后在30MPa和70°C下动态萃取20min,然后用100μm膜厚PDMS纤维同时收集,获得了SFE后HS-SPME的最佳条件。 。该方法的线性范围为5至5000ngg〜(-1),检测限为0.39至0.54ngg〜(-1),定量限为1.30至1.80ngg〜(-1)。该方法成功地用于分析工业区附近河流和海滩沉积物中的全氟辛烷磺酸。测定的全氟辛烷磺酸浓度为282至4473ngg〜(-1)。

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