Quantitative and qualitative comparison of marine dissolved organic nitrogen recovery using solid phase extraction

Quantitative and qualitative comparison of marine dissolved organic nitrogen recovery using solid phase extraction
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固相萃取回收海洋溶解有机氮的定量和定性比较

DOI:
10.1002/lom3.10558
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发表时间:
2023
期刊:
Limnology and Oceanography: Methods
影响因子:
--
通讯作者:
Knapp, Angela N.
Knapp, Angela N.
中科院分区:
--
文献类型:
--
作者:
Miranda, Carlos;Boiteau, Rene M.;McKenna, Amy M.;Knapp, Angela N.

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海洋溶解有机碳和氮(DOC和DON)是全球主要的碳和营养库,其表征依赖于提取方法的预浓缩和除盐。现有的方法优化捕获和描述DOC。在这里,我们报告了一个优化的分析策略,以恢复海洋DON随后的分子表征。据报道,7种固相萃取(SPE)吸附剂的保留效率在5%和95%之间,与C18回收的95%相比,PPL回收了23%的海洋DON。使用C18和PPL吸附剂研究了不同样品体积和洗脱速度的影响以及所得DON提取物的分子组成的额外比较。样品体积> 200 mL会降低DON的保留效率,与SPE吸附剂无关,重力洗脱回收的DON是真空洗脱的1.7 - 4.2倍。通过负离子电喷雾电离傅立叶变换离子回旋共振质谱法(FT-ICR MS)对提取的DON进行表征,突出了通过每种方法回收的DON物质之间的组成差异。用优化的方法分离的DON包括具有低O:C比(0.2至0.5)的低分子量(< 600 Da)肽样化合物,其不能被其他SPE吸附剂检测到(例如,PPL)。用这种方法分离的大多数额外DON通过直接输注阴性模式FT‐ICR MS分析是检测不到的。
Marine dissolved organic carbon and nitrogen (DOC and DON) are major global carbon and nutrient reservoirs, and their characterization relies on extraction methods for preconcentration and salt removal. Existing methods optimize for capturing and describing DOC. Here, we report an optimized analytical strategy to recover marine DON for subsequent molecular characterization. Retention efficiencies between 5% and 95% are reported for seven solid phase extraction (SPE) sorbents, with PPL recovering 23% of marine DON compared to 95% recovered with C18. Additional comparisons of the effect of varying sample volumes and elution speed, and the resulting molecular composition of DON extracts, were investigated using C18and PPL sorbents. Sample volumes > 200 mL decreased DON retention efficiency independent of SPE sorbent, and gravity elution recovered 1.7‐ to 4.2‐fold more DON compared to vacuum elution. Characterization of extracted DON by negative‐ion electrospray ionization Fourier transform‐ion cyclotron resonance mass spectrometry (FT‐ICR MS) highlights compositional differences between DON species recovered by each method. DON isolated with optimized methods includes low molecular weight (< 600 Da) peptide‐like compounds with low O:C ratios (0.2 to 0.5) that are not detected by other SPE sorbents (e.g., PPL). The majority of additional DON isolated with this approach was undetectable by direct infusion negative mode FT‐ICR MS analysis.
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