Yao Xiunan, Wang Ninglian, Zheng Xingwang, Li Quanlian, Santos Ewerton, Maharjan Linda, Wang Junjie, Guo Zhihui, Guo Jiahua, Zhang Huan, Zheng Kui, Wu Jingquan, Li Yao
Shaanxi Key Laboratory of Earth Surface System and Environmental Carrying Capacity Xi'an 710127 China
College of Urban and Environmental Sciences, Northwest University Xi'an 710127 China.
RSC Adv. 2023 Mar 1;13(10):7030-7036. doi: 10.1039/d2ra07419b. eCollection 2023 Feb 21.
The sensitive determination of levoglucosan in aqueous samples has great significance for the study of biomass burning. Although some sensitive high-performance liquid chromatography/mass spectrometry (HPLC/MS) detection methods have been developed for levoglucosan, there are still plenty of shortcomings, such as complicated sample pre-treatment procedures, large-amount sample requirements, and poor reproducibility. Herein, a new method for the determination of levoglucosan in the aqueous sample was developed using ultra-performance liquid chromatography with triple quadrupole mass spectrometry (UPLC-MS/MS). In this method, we firstly found that compared with H, Na could effectively enhance the ionization efficiency of levoglucosan, even though the content of H is higher in the environment. Moreover, the precursor ion / 185.1 [M + Na] could be used as a quantitative ion to sensitively detect levoglucosan in aqueous samples. Only 2 μL of un-pretreated sample is required for one injection in this method, and great linearity was obtained ( = 0.9992) using the external standard method when the concentration of levoglucosan was 0.5-50 ng mL. The limit of detection (LOD) and quantification (LOQ) were 0.1 ng mL (0.2 pg absolute mass injected) and 0.3 ng mL, respectively. Acceptable repeatability, reproducibility, and recovery were achieved. This method has the advantages of high sensitivity, good stability, good reproducibility, and simple operation, which could be widely used for the detection of different concentrations of levoglucosan in various water samples, especially for the detection of samples with low content such as ice core or snow samples.
对水样中左旋葡聚糖进行灵敏测定对于生物质燃烧研究具有重要意义。尽管已经开发了一些用于左旋葡聚糖的灵敏高效液相色谱/质谱(HPLC/MS)检测方法,但仍存在许多缺点,如样品前处理程序复杂、样品需求量大以及重现性差等。在此,开发了一种使用超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)测定水样中左旋葡聚糖的新方法。在该方法中,我们首先发现,与H相比,Na能有效提高左旋葡聚糖的电离效率,尽管环境中H的含量更高。此外,前体离子/185.1 [M + Na]可作为定量离子来灵敏检测水样中的左旋葡聚糖。该方法一次进样仅需2 μL未经预处理的样品,当左旋葡聚糖浓度为0.5 - 50 ng/mL时,采用外标法获得了良好的线性关系( = 0.9992)。检测限(LOD)和定量限(LOQ)分别为0.1 ng/mL(绝对进样质量0.2 pg)和0.3 ng/mL。实现了可接受的重复性、重现性和回收率。该方法具有灵敏度高、稳定性好、重现性好和操作简单等优点,可广泛用于检测各种水样中不同浓度的左旋葡聚糖,尤其适用于检测冰芯或雪样等低含量样品。