松针褐斑病菌毒素LA-I的分离纯化及其化学结构  被引量:5

Separation and Purification, Structure of LA-I Toxin Produced by Brown Spot Needle Blight Fungus (Lecanosticta acicola)

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作  者:杨斌[1] 叶建仁[1] 包宏[2] 刘吉开[2] 董泽军[2] 

机构地区:[1]南京林业大学,南京210037 [2]中国科学院昆明植物研究所,昆明650204

出  处:《林业科学》2005年第2期86-90,共5页Scientia Silvae Sinicae

基  金:国家自然科学基金项目"松针褐斑病菌致病毒素的研究"(批准号 3 9870 62 7)

摘  要:采用柱层析和高效液相色谱分离相结合 ,从松针褐斑病菌的PD培养液中分离提纯到一种致毒活性物质LA -I,该物质为无色油状物。紫外扫描显示LA -I的最大吸收波长为 2 0 7nm。在 36 5nm和 2 5 4nm波长下LA -I无吸收。FAB- MS和HRFAB- MS分别显示该毒素物质的相对分子质量和分子式为 16 2和C6 H1 0 O5;氢谱中的 2个信号 (δ1 2 6 ,δ4 2 2 )表明该毒素物质存在—OCH(CH3)—基团。碳谱显示有 3个碳信号 (δ181 0 9,δ6 6 99,δ2 1 6 9) ,证明存在—COOH ,—CH ,—CH3基团。综合质谱、核磁共振谱分析确定LA -I为COOHCH(CH3)OCH(CH3)COOH(α ,α′ -二丙酸醚 ) 。Brown spot needle blight fungus (Lecanosticta acicola) could produce pathogenic toxin. A combination use of silica gel column chromatography, reversed phase silica gel column chromatography and HPLC led to the isolation of a phytotoxic compound, named LA-I, from the crude toxins produced by Lecanosticta acicola cultured in PD medium. LA-I was colorless oil. UV scanning results indicated the maximum absorptive wave length of LA-I was 207 nm. Under 365 nm and 254 nm, LA-I had no or little UV absorption. The MW and MF of this toxin was determined by FAB -MS and HRFAB -MS as 162 and {C 6H 10O 5. Two signals of H at δ1.26, δ 4.22 in 1HNMR spectrum showed —OCH(CH 3)— existed in the compound. 13CMNR spectrum indicated not only the —OCH(CH 3)— signals but also the signal of COOH (δ181.09). Synthesized FAB -MS, HRFAB -MS, 1HNMR, 13CNMR data, the structure of LA-I could be deduced as COOHCH(CH 3)OCH(CH 3)COOH. Such a structure could explain IR spectrum well.

关 键 词:松针褐斑病菌 化学结构 毒素 分离纯化 液相色谱分离 最大吸收波长 相对分子质量 活性物质 分离提纯 扫描显示 COOH 核磁共振 红外光谱 LA 柱层析 培养液 分子式 谱分析 信号 基团 

分 类 号:S763.712.4[农业科学—森林保护学] O631.61[农业科学—林学]

 

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