配位体交换色谱法测定槐米废渣水解液单糖成分

摘要

利用生物质转化成糖研究近年来备受关注,为给工业化高效利用槐米废渣提供检测技术,本文建立了槐米废渣水解转化糖液中4种主要单糖的铅(Pb2+)配位体交换高效液相色谱分析方法并采用离子色谱法验证了方法的可行性;实验比较了pb2和Ca2两种不同柱内抗衡离子对组分分离的影响,最终利用铅配体方法对实际样品进行了测试.方法分离柱采用Sepax Carbomix Pb-NP 5(300×7.8 mm ID,5μm,8％交联度)色谱柱,柱温75℃;流动相采用超纯水,流速0.50 mL/min;检测器采用示差折光检测器,检测器温度为30℃;样品采用活性炭固相萃取小柱脱除色素.结果表明,组分葡萄糖、木糖、半乳糖和阿拉伯糖在25 min内完成分离,在0.2～20.0 mg/mL浓度范围内呈现良好的线性关系,方法检测限在1.94 ～ 1.98 μg/mL之间;槐米废渣水解液中阿拉伯糖平均含量大于67％,具有较高回收价值.方法样品前处理简便,重现性好,结果准确,测试成本低.%In recent years,conversion of biomass materials to monosaccharides has attracted significant attention.In order to develop testing techniques for efficient usage of Flos Sophorae residue,the determination method of 4 monosaccharides in hydrolysate from Flos Sophorae residue was established with lead(Pb2+) ligand exchange high performance liquid chromatography(LEX-HPLC) and ion chromatography was used to verify the feasibility of this method.Influence of separation by different counterions(Pb2 + & Ca2+) in column was investigated.The lead (Pb2+) ligand exchange was applied in the actual samples detection finally.A Sepax Carbomix Pb-NP 5 (300 × 7.8 mm ID,5 μm,8％ crosslinkage)column was used for the separation with ultrapure water as mobile phase.The flow rate of mobile phase was 0.50 mL/minat a column temperature of 75 ℃.Temperature of refractive index detector(RID) was 30 ℃.Samples were pretreated by solid phase extraction (SPE) with activated carbon to remove colorings.The results showed that the separation was achieved within 25 min.The calibration curve was linear in the mass concentration range of 0.2-20.0 mg/mL,the limit of detection (LOD) of glucose,xylose,galactose and arabinose were 1.94-1.98 μg/mL,respectively.Content of arabinose in samples exceeded 67％ and it had a high usage value.The method was simple,accurate,economical and reproducible.