Levoglucosan is a thermal decomposition product of cellulose in particulate matter. δ¹³C value of levoglucosan could be used in studying the combustion mechanisms and chemical pathways. In order to introduce a minimum number of carbon atoms, based on the stereostructure of levoglucosan, a two-step derivatization method with methylboronic acid and MSTFA was developed and carefully optimized. The recommended reaction temperature is 70°C; the reaction time is 60 min for MBA and 120 min for MSTFA derivatization; and the molar ratio of levoglucosan : MBA : MSTFA is 1 : 1: 100 and 1 : 1: 120 and the reagent volume ratio of MSTFA : pyridine is between 1 : 3 and 1 : 4. The developed method achieved excellent reproducibility and high accuracy. The differences in the carbon isotopic compositions of the target boronate trimethysilylated derivative between the measured and calculated ranged from 0.09 to 0.36‰. The standard deviation of measured δ¹³C value of levoglucosan was between 0.22 and 0.48‰. The method was applied to particle samples collected from the combustion of cellulose at four different temperatures. δ¹³C values of levoglucosan in particle samples generated from a self-made combustion setup suggesting that combustion temperature play a little role on isotope fractionation of levoglucosan, although ¹³C enriched in levoglucosan during the combustion process.

中文翻译：

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左旋葡聚糖的衍生化，通过气相色谱/燃烧/同位素比质谱法对化合物进行特定的δ13C分析。

左旋葡聚糖是纤维素在颗粒物质中的热分解产物。δ ¹³左旋葡聚糖的C值可用于研究燃烧机理和化学途径。为了引入最小数目的碳原子，基于左旋葡聚糖的立体结构，开发并仔细优化了使用甲基硼酸和MSTFA的两步衍生化方法。推荐的反应温度为70°C；MBA反应时间为60分钟，MSTFA衍生反应时间为120分钟。左旋葡聚糖∶MBA∶MSTFA的摩尔比为1∶1∶100和1∶1∶120，MSTFA∶吡啶的试剂体积比为1∶3至1∶4。该方法具有良好的重现性和高精度。 。测定和计算出的目标硼酸酯三甲基甲硅烷基化衍生物的碳同位素组成之间的差异为0.09至0.36‰。实测标准偏差δ ¹³左旋葡聚糖的C值是0.22和0.48之间‰。该方法应用于从纤维素在四个不同温度下燃烧收集的颗粒样品。δ ^13个从自制燃烧设置表明燃烧温度发挥上左旋葡聚糖的同位素分馏一点作用产生的颗粒样品在左旋葡聚糖的C值，虽然¹³下，在左旋葡聚糖在燃烧过程中富集。