中国农业科学2025，Vol.58Issue(8)：1630-1640,11.DOI:10.3864/j.issn.0578-1752.2025.08.013
利用大孔吸附树脂与高速逆流色谱纯化脱氧雪腐镰刀菌烯醇-3-葡萄糖苷
Purification of Deoxynivalenol-3-Glucoside by Using Macroporous Adsorption Resin Combined with High-Speed Counter-Current Chromatography
摘要
Abstract
[Objective]Deoxynivalenol-3-glucoside(DON-3G)is the most commonly found masked mycotoxin in cereals,however,the high cost of substrates hinders further studies on it.This study aimed to develop an efficient and affordable method for the large-scale purification of DON-3G from the enzymatic transformation product.[Method]Static adsorption experiments were utilized to screen various types of adsorption and ion-exchange resins,and a single-factor experimental design was employed to determine the optimal adsorption and desorption conditions.The adsorption thermodynamic model was established to fit the adsorption behavior.The pure material of DON-3G was then prepared using high-speed counter-current chromatography(HSCCC),and the biphasic systems were screened.The UV and NMR spectroscopy were used to confirm the product's structure,and high-performance liquid chromatography(HPLC)was used to assess its purity.[Result]With a maximal adsorption capacity of 269.23 μg·g-1 resin,the XAD-4 resin was determined to be the most effective macroporous resin for adsorbing DON-3G from the reaction system.The 40%methanol solution was used as the desorption solvent,because it could elute DON-3G within 5 bed volume.DON-3G and unreacted DON were separated using a biphasic system with n-butanol/trifluoroacetic acid/water(1:0.01:1)at a flow rate of 1 mL·min-1,a rotation speed of 1 000 r/min,and a column temperature of 35℃under the bidirectional elution mode.With optimal conditions,the HSCCC process produced DON-3G with a purity of 97.46%and the recovery rate was 79.7%.Unreacted DON could be recovered by reverse elution.[Conclusion]Over 100 mg of DON-3G might be separated and purified using this approach in a single run,paving the way for the subsequent research targeting DON-3G.关键词
脱氧雪腐镰刀菌烯醇-3-葡萄糖苷/隐蔽型毒素/分离纯化/大孔吸附树脂/高速逆流色谱Key words
deoxynivalenol-3-glucoside/masked mycotoxin/isolation and purification/macroporous adsorption resin/high-speed counter-current chromatography引用本文复制引用
陈龙云,胡俊强,何灿,史建荣,徐剑宏,王刚..利用大孔吸附树脂与高速逆流色谱纯化脱氧雪腐镰刀菌烯醇-3-葡萄糖苷[J].中国农业科学,2025,58(8):1630-1640,11.基金项目
国家重点研发计划(2023YFD1301003)、国家自然科学基金(32161143034)、江苏省科技计划专项资金(BE2022786)、江苏省农业科技自主创新资金(CX(23)3003) （2023YFD1301003）
