Pashynska Vlada, Vermeylen Reinhilde, Vas Gyorgy, Maenhaut Willy, Claeys Magda
University of Antwerp (UIA), Department of Pharmaceutical Sciences, Universiteitsplein 1, B-2610 Antwerp, Belgium.
J Mass Spectrom. 2002 Dec;37(12):1249-57. doi: 10.1002/jms.391.
We developed and validated a gas chromatographic/ion trap mass spectrometric method for the determination of levoglucosan and the related monosaccharide anhydrides, mannosan, galactosan and 1,6-anhydro-beta-D-glucofuranose in urban atmospheric aerosols collected on quartz fiber filters. The method is based on extraction with dichloromethane-methanol (80 : 20, v/v), trimethylsilylation, multiple reaction monitoring in the tandem mass spectrometric mode using the ion at m/z 217, and the use of an internal standard calibration procedure with the structurally related compound methyl beta-L-arabinopyranoside. In addition, the method allows the quantification of other saccharidic compounds, arabitol, mannitol, glucose, fructose, inositol and sucrose, which were found to be important in summer aerosols. The recovery of levoglucosan was estimated by spiking blank filters and was better than 90%. The precision evaluated by analyzing parts of the same filters was about 2% for the monosaccharide anhydrides and 7% for the other saccharidic compounds in the case of a winter aerosol sample, and the corresponding values for a summer aerosol sample were 5% and 8%. The method was applied to urban PM(10) (particulate matter of <10 microm aerodynamic diameter) aerosols collected at Ghent, Belgium, during a 2000-2001 winter and a 2001 summer episode and revealed interesting seasonal variations. While monosaccharide anhydrides were relatively more important during the winter season owing to wood burning, the other saccharidic compounds were more prevalent during the summer season, with some of them, if not all, originating from the vegetation.
我们开发并验证了一种气相色谱/离子阱质谱法,用于测定在石英纤维滤膜上收集的城市大气气溶胶中的左旋葡聚糖及相关单糖酐、甘露聚糖、半乳聚糖和1,6 - 脱水 - β - D - 葡萄糖呋喃糖。该方法基于二氯甲烷 - 甲醇(80 : 20,v/v)萃取、三甲基硅烷化、在串联质谱模式下使用质荷比为217的离子进行多反应监测,以及使用与结构相关的化合物β - L - 阿拉伯吡喃糖苷甲基酯进行内标校准程序。此外,该方法还可对其他糖类化合物,如阿拉伯糖醇、甘露醇、葡萄糖、果糖、肌醇和蔗糖进行定量,这些化合物在夏季气溶胶中被发现具有重要意义。通过向空白滤膜加标来估算左旋葡聚糖的回收率,回收率优于90%。对于冬季气溶胶样品,通过分析同一滤膜的部分样品评估的精密度,单糖酐约为2%,其他糖类化合物约为7%;对于夏季气溶胶样品,相应的值分别为5%和8%。该方法应用于2000 - 2001年冬季和2001年夏季在比利时根特采集的城市PM(10)(空气动力学直径<10微米的颗粒物)气溶胶,揭示了有趣的季节变化。由于冬季木材燃烧,单糖酐在冬季相对更为重要,而其他糖类化合物在夏季更为普遍,其中一些(如果不是全部的话)源自植被。