Determination of lignin in marine sediment using alkaline cupric oxide oxidation-solid phase extraction-on-column derivatization-gas chromatography
Determination of lignin in marine sediment using alkaline cupric oxide oxidation-solid phase extraction-on-column derivatization-gas chromatography
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碱性氧化铜-固相萃取-柱衍生-气相色谱法测定海洋沉积物中的木质素
DOI：
10.1007/s11802-011-1936-z
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发表时间：
2013-01
影响因子：
1.6
通讯作者：
Wang Min
中科院分区：
文献类型：
--
作者：
Sun Shuwen;Lan Haiqing;Du Peirui;Wang Min
木质素是研究海洋环境中陆源有机物的重要分子化石之一。木质素氧化产物（LOPs）的提取和衍生化是海洋沉积物中木质素准确定量的关键。在这里，我们报告了传统的碱性氧化铜（CuO）氧化方法的修改，修改组成的固相萃取（SPE）和一种新的柱上衍生化被采用更好的效率和重现性。在空白加标中，固相萃取法的回收率为77.84%~ 99.57%，相对标准偏差（RSD）为0.57%~ 8.04%（n=3），而传统液-液萃取法的回收率为44.52%~ 86.16%（n=3），相对标准偏差（RSD）为0.53%~ 13.14%（n=3）。此外，SPE大大提高了重现性，溶剂消耗量更少，处理时间更短。LOPs的柱上衍生化平均效率为100.8% ± 0.68%，显著高于瓶内或注射器内衍生化，从而导致更少的衍生试剂消耗。利用建立的方法对长江口南部表层沉积物中的木质素进行了测定。回收率为72.66%~ 85.99%，标准偏差小于0.01mg/10 g干重，对羟基苯甲醛除外。研究区木质素含量Σ8（10 g干沉积物产生）在0.231 ~ 0.587 mg之间。S/V和C/V比值（分别为1.028 ± 0.433和0.192 ± 0.066）表明，该地区的托姆植物起源于木本和非木本被子植物的混合体，高的（Ad/Al）v值表明托姆植物已经高度退化。
Lignin serves as one of the most important molecular fossils for tracing Terrestrial Organic Matters (TOMs) in marine environment. Extraction and derivatization of lignin oxidation products (LOPs) are crucial for accurate quantification of lignin in marine sediment. Here we report a modification of the conventional alkaline cupric oxide (CuO) oxidation method, the modification consisting in a solid phase extraction (SPE) and a novel on-column derivatization being employed for better efficiency and reproducibility. In spiking blanks, recoveries with SPE for the LOPs are between 77.84% and 99.57% with relative standard deviations (RSDs) ranging from 0.57% to 8.04% (n=3), while those with traditional liquid-liquid extraction (LLE) are from 44.52% to 86.16% with RSDs being from 0.53% to 13.14% (n=3). Moreover, the reproducibility is greatly improved with SPE, with less solvent consumption and shorter processing time. The average efficiency of on-column derivatization for LOPs is 100.8% ± 0.68%, which is significantly higher than those of in-vial or in-syringe derivatization, thus resulting in still less consumption of derivatizing reagents. Lignin in the surface sediments sampled from the south of Yangtze River estuary, China, was determined with the established method. Recoveries of 72.66% to 85.99% with standard deviation less than 0.01mg/10g dry weight are obtained except for p-hydroxyben-zaldehyde. The lignin content Σ8 (produced from 10 g dry sediment) in the research area is between 0.231 and 0.587 mg. S/V and C/V ratios (1.028 ± 0.433 and 0.192 ± 0.066, respectively) indicate that the TOMs in this region are originated from a mixture of woody and nonwoody angiosperm plants; the high values of (Ad/Al)vsuggest that the TOMs has been highly degraded.
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影响因子：
3
作者：
A. Miltner;K. Emeis
通讯作者：
A. Miltner;K. Emeis
影响因子：
2.8
作者：
C. Rezende;W. Pfeiffer;L. Martinelli;Elizabeth Tsamakis;J. Hedges;R. Keil
通讯作者：
C. Rezende;W. Pfeiffer;L. Martinelli;Elizabeth Tsamakis;J. Hedges;R. Keil
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作者：
R. B. H. Creighton;R. D. Gibbs;H. Hibbert
通讯作者：
R. B. H. Creighton;R. D. Gibbs;H. Hibbert
影响因子：
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作者：
T. Bianchi;S. Mitra;B. McKee
通讯作者：
T. Bianchi;S. Mitra;B. McKee
影响因子：
64.8
作者：
J. Tinsley
通讯作者：
J. Tinsley