Mokochinski Joao Benhur, Bataglion Giovana Anceski, Kiyota Eduardo, de Souza Letícia Marrone, Mazzafera Paulo, Sawaya Alexandra Christine Helena Frankland
Department of Plant Biology, Institute of Biology, State University of Campinas, UNICAMP, 13083-970, Campinas, São Paulo, Brazil.
Anal Bioanal Chem. 2015 Sep;407(23):7221-7. doi: 10.1007/s00216-015-8886-9. Epub 2015 Jul 14.
A simple extraction protocol and an ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) method for the determination of the syringyl/guaiacyl (S/G) ratio in lignin is reported herein. The method was entirely developed using stems of three Eucalyptus species, which were hydrolyzed with NaOH and partitioned with ethyl ether; vanillin (from the G monomer) and syringaldehyde (from S monomer) were quantified. The S/G ratios obtained were comparable to those usually reported for eucalyptus. The data for one of the eucalyptus species were compared with those obtained with a widely accepted method using thioacidolysis and gas chromatography-mass spectrometry (GC-MS). The method was also applied to sugarcane and showed to be reliable. The yield of the NaOH hydrolysis of the monolignols ranged from 89.94 to 95.69%, with more than 77.12% of recuperation in the liquid-liquid extraction. The whole analytical procedure was validated, achieving results with less than 4.38% of variation. The lowest LOD and LOQ were 0.01 and 0.05 μg/mL, respectively. In addition, the method combines reliability and a fast and direct quantification.
本文报道了一种用于测定木质素中紫丁香基/愈创木基(S/G)比率的简单提取方案和超高效液相色谱-质谱联用(UHPLC-MS)方法。该方法完全是利用三种桉树的茎开发的,这些茎先用氢氧化钠水解,然后用乙醚分配;对香草醛(来自G单体)和紫丁香醛(来自S单体)进行定量。得到的S/G比率与通常报道的桉树的比率相当。将其中一种桉树的数据与使用硫代酸解和气相色谱-质谱联用(GC-MS)的广泛接受的方法所获得的数据进行了比较。该方法也应用于甘蔗,结果表明是可靠的。单木质醇的氢氧化钠水解产率在89.94%至95.69%之间,液-液萃取中的回收率超过77.12%。整个分析程序经过验证,变异小于4.38%。最低检测限和定量限分别为0.01和0.05μg/mL。此外,该方法兼具可靠性以及快速直接定量的特点。