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Derivatization procedures and determination of levoglucosan and related monosaccharide anhydrides in atmospheric aerosols by gas chromatography-mass spectrometry

机译:气相色谱-质谱联用法测定大气气溶胶中左旋葡聚糖及相关单糖酐的含量

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This study evaluated the derivatization procedures for detecting the three most commonly monosaccharide anhydrides (MAs) (levoglucosan,mannosan and galactosan) in atmospheric aerosols using gas chromatography-mass spectrometry (GC-MS).Various silylating agents,mainly trimethylsilylating agents (TMS),were compared and the effects of various contents of trimethylchlorosilane (TMCS,as a stimulator) were evaluated to optimize the conditions for detecting these compounds in aerosol samples.Differences among the abundances of the derivatives were caused by the sterical hindrance of three hydroxyl groups in the structures of monosaccharide anhydrides.The effects of the reaction time and temperature were also examined.The optimal reaction time and temperature were 60 min and 80 °C with 1% TMCS plus 0.2% 1,4-dithioerythritol (DTE).Under these conditions,the percentages of formation of bis-O-TMS derivatives (as by-products) were 23,29 and 10% for galactosan,mannosan and levoglucosan,respectively.The concentrations of galactosan,mannosan and levoglucosan in particles of smoke samples ranged from 29 to 88,23 to 69 and 77 to 380 ng/m3,respectively;and in particles of atmospheric aerosols ranged from 0.06 to 0.75,n.d.to 0.49 and 1.6 to 132 ng/m3,respectively.Levoglucosan was the dominant MAs detected in both type of samples.Less than 10% quantitation difference was obtained when bis-O-TMS derivatives were included in the calculation.
机译:本研究评估了使用气相色谱-质谱(GC-MS)检测大气气溶胶中三种最常见的单糖酐(MAs)(左旋葡聚糖,甘露聚糖和半乳糖聚糖)的衍生程序。各种甲硅烷基化剂,主要是三甲基甲硅烷基化剂(TMS),比较了三甲基氯硅烷(TMCS,作为刺激剂)的各种含量的影响,以优化检测气溶胶样品中这些化合物的条件。衍生物的丰度差异是由三个羟基的空间位阻引起的。还研究了反应时间和温度的影响,最佳反应时间和温度为60分钟和80°C,1%TMCS加0.2%1,4-二硫赤藓糖醇(DTE)。 bis-O-TMS衍生物(作为副产物)的形成百分比分别为半乳糖,甘露聚糖和左旋葡聚糖的23,29和10%烟雾样品中半乳糖聚糖,甘露聚糖和左旋葡聚糖的浓度分别为29至88,23至69 ng和77至380 ng / m3;大气中的气溶胶颗粒浓度为0.06至0.75,ndto 0.49和1.6分别为132 ng / m3。左旋葡聚糖是两种类型样品中检测到的主要MAs。计算中包括bis-O-TMS衍生物时,定量差异小于10%。

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