UPLC-MS/MS法检测禾谷镰刀菌中6-磷酸海藻糖和海藻糖的色谱柱选择  

Selection of chromatographic column for trehalose-6-phosphate and trehalose detection in Fusarium graminearum by UPLC-MS/MS

作　　者：吴琴燕[1] 梁红芳 张文文 温小林[1] 朱建飞[1] 徐超 庄义庆[1,3] WU Qin-yan;LIANG Hong-fang;ZHANG Wen-wen;WEN Xiao-lin;ZHU Jian-fei;XU Chao;ZHUANG Yi-qing(Central Laboratory of Zhenjiang Institute of Agricultural Sciences in Hill Area of Jiangsu Province,Jurong 212009,China;Zhenjiang Agricultural and Rural Bureau,Zhenjiang 212400,China;Central laboratory of Jiangsu Academy of Agricultural Sciences,Nanjing 210014,China)

机构地区：[1]江苏丘陵地区镇江农业科学研究所中心实验室,江苏句容212009 [2]镇江市农业农村局,江苏镇江212400 [3]江苏省农业科学院中心实验室,江苏南京210014

出　　处：《江苏农业学报》2021年第5期1299-1304,共6页Jiangsu Journal of Agricultural Sciences

基　　金：镇江市科技计划社会发展项目(SH2020019)。

摘　　要：选择6-磷酸海藻糖(T6P)和海藻糖(Tre)在超高效液相色谱UPLC分离中的最佳色谱柱。对T6P和Tre在C_(18)柱、Kinetex Hilic柱、T3柱、Luna■NH2柱、Cogent diamond Hydride柱和BEH Amide柱6种色谱柱中的色谱行为进行对比研究。结果表明,T6P和Tre在Luna■NH2柱和T3柱中分离效果较好,分别建立Luna■NH2柱和T3柱的UPLC-MS/MS检测方法,其检出限分别为1.25~5.10μg/L和12.75~15.62μg/L,定量限分别为3.75~15.60μg/L和38.25~52.03μg/L,回收率分别为71.5%~85.7%和82.8%~95.6%,相对标准差分别为3.8%~8.5%和2.7%~3.3%,Luna■NH2柱的灵敏度高,T3色谱柱的回收率高、稳定性好。2种色谱柱均满足禾谷镰刀菌中T6P和Tre同时检测的要求。The best chromatographic column of trehalose-6-phosphate(T6P)and trehalose(Tre)in ultra-high performonce liquid chromatography(UPLC)separation was selected.The chromatographic behaviors of T6P and Tre in six kinds of chromatographic columns(C_(18) column,Kinetex HILIC column,T3 column,Luna■NH2 column,Cogent diamond hydride column and BEH Amide column)were compared.The results showed that Amino column and T3 column were suitable for the detection of T6P and Tre according to the chromatographic retention effect.UPLC-MS/MS methods for T6P and Tre in Fusarium graminearum were established based on LunaNH2 column and T3 column,respectively.The detection limits of Luna■NH2 column and T3 column were 1.25-5.10μg/L and 12.75-15.62μg/L,the limits of quantification were 3.75-15.60μg/L and 38.25-52.03μg/L,the recoveries were 71.5%-85.7%and 82.8%-95.6%,the relative standard deviations(RSD)were 3.8%-8.5%and 2.7%-3.3%,respectively.The method established by Luna■NH2 column has high sensitivity,and the method established by T3 column has high recovery rate and good stability.Luna■NH2 column and T3 column can be used for the simultaneous detection of T6P and Tre in Fusarium graminearum.

关 键 词：超高效液相色谱-串联质谱 禾谷镰刀菌 6-磷酸海藻糖 海藻糖 色谱柱 

分 类 号：O657.63[理学—分析化学]